uuu E 1,28: v.8/bk.1 BOOKSTACKS- POCUMENTS FE-1 734-41 (Vol.8)(Bk.l) RUN REPORTS: COj ACCEPTOR PROCESS GASIFICATION PILOT PLANT Final Report, Volume 8, Book 1 of 6, Runs 1-11, January 1972-July 1973 Work Performed Under Contract No. EX-76-C-01-1734 Research Division Conoco Coal Development Company Library, Pennsylvania and Stearns- Roger Incorporated Denver, Colorado €►1 U. S. DEPARTMENT OF ENERGY NOTICE This report was prepared as an account of work sponsored by the United States Government. Neither the United States nor the United States Department of Energy, nor any of their employees, nor any of their contractors, subcontractors, or their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness or usefulness of any information, apparatus, product or process disclosed, or represents that its use would not infringe privately owned rights. This report has been reproduced directly from the best available copy. Available from the National Technical Information Service, U. S. Department of Commerce, Springfield, Virginia 22161, Price: Paper Copy $11.75 Microfiche $3.00 UNIVERSITY OF ILLINOIS LIBRARY AT URBANA-CHAMPAIGN STACKS FE-1 734-41 (Vol.8)(Bk.l) Distribution Category UC-90c RUN REPORTS CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT FINAL REPORT, VOLUME 8 BOOK 1 OF 6, RUNS 1 - 11 PERIOD: JANUARY 1972 - JULY 1973 CONOCO COAL DEVELOPMENT COMPANY RESEARCH DIVISION LIBRARY, PENNSYLVANIA 15129 AND STEARNS-ROGER INCORPORATED P.O. BOX 5888 DENVER, COLORADO 80217 PREPARED FOR UNITED STATES DEPARTMENT OF ENERGY AND AMERICAN GAS ASSOCIATION UNDER CONTRACT EX-76-C-01-1734 Digitized by the Internet Archive in 2013 http://archive.org/details/runreportsc0acce81cono FOREWORD The reports contained in this document were prepared jointly by Conoco Coal Development Company and Stearns-Roger, Incorporated, as partial fulfillment of the Department of Energy contract (EX-76-C-01-1734) for the development of C0_ Acceptor Gasification Process. Each report normally covers the operation of the CO^ Acceptor Process Pilot Plant for a single run. Some runs, however, nave several parts (A, B, C, etc.) and occasionally two or more runs have been grouped together in a single report. The reports are informal data reports which were written shortly after the completion of the respective runs. The reports serve the purpose of recording the objectives, accomplishments, and problems encountered during the pilot plant operations. Operating data are also often pre- sented. However, these data are, for the most part, presented as a matter of record since the inclusion of heat and material balances and the analysis of the data was not part of the scope of the run reports. Prior to Run 16, no periods of truly steady-state integrated plant operation were obtained for which heat and material balances can be cal- culated. The development of a reliable, standardized startup procedure, the solving of process and especially mechanical equipment problems, were the primary concerns during these early runs. Much needed process data at steady- state conditions were gathered during the later runs. Detailed heat and material balances for selected runs are presented in Volume 12 of the Final Report. Some discrepancies will be found between the data presented in the run reports and the heat and material balance results. For example, the acceptor circulation and gasifier vent rate presented in many of the run reports do not agree with the heat and material balance values. The run report acceptor circulation rates are based upon the acceptor lift line pressure drop and are considered to be only an approximation of the actual acceptor circulation rate. The pressure drop derived cir- culation rate served as a guide to the plant operators and provided trend information. Because of the severe temperature and pressure conditions in the process, the acceptor circulation and also the fuel char rates cannot be directly measured. These rates can only be ac- curately determined via detailed heat and material balance calculations. A mathematical model of the process, which is embodied in the form of a computer program was therefore developed. The model values for the acceptor circulation and the fuel char rates are presented in the de- tailed heat and material balances. These rates arc considered to be correct. m The measured gasifier vent rates (product gas rates) contained in the run reports are generally lower, and often much lower, than the mathe- matical model values. There are several reasons for this. First, pro- cess flow measuring instrumentation was often fouled by the small amounts of char fines and liquid water contained in the vent gases. Secondly, undetected process leaks from valve packings and from vessel and piping flanges represent sizable losses in the available vent gas quantity to be measured. The actual vent gas from the gasifier is better repre- sented by the mathematical model value than by the measured value. The above examples point out that consideration must be given and judge- ments made concerning the use of certain process data. The philosophy with respect to data analysis, has been to use the mathematical model to match as much as possible the measured process data. Differences be- tween the model results and the measured data are resolved by the re- examination of instrument records and the pilot plant logs or by mod- ifying the model where necessary. TV TABLE OF CONTENTS Abstract Page RUN 1 1 Run lA 2 1 . 1 Summary 2 1.2 Discussion 2 2 Run IB 4 2 . 1 Summary 4 2.2 Discussion 5 3 Acceptor Size Analyses 7 RUN 2 1 Summary 12 1.1 Major Modifications 12 1.2 Duration 12 1.3 Startup Steps Accomplished 12 1.4 Termination 12 1.5 Difficulties Encountered 12 2 Discussion 14 2.1 Sequence of Events 14 2.2 Dolomite Circulation 15 2.3 Bed Densities 15 3 Acceptor Size Analyses 16 RUN 3 1 Summary 21. 1.1 Major Modifications 21 1.2 Duration 21 1.3 Startup Steps Accomplished 21 1.4 Termination 21 1.5 Difficulties Encountered 21* 2 Discussion 22 2.1 Hot Acceptor Circulation 22 2.2 Char Addition to Gasifier 22 2.3 Bed Densities .22 2.4 Char Acceptor Interface 23 RUN 4 Foreword 27 1 Summary 28 2 Significant Events and Observations . .29 2.1 Major Modifications 29 2.2 Duration 29 2.3 Startup Steps Accomplished 29 2.4 Termination 29 2 . 5 Temporary Shutdowns 29 2.6 Milestones Achieved 29 2.7 Difficulties Encountered 30 RUN 4 (cont.) Page 3 Results and Discussion 31 3.1 First Startup and Shutdown--Run 4A 31 3.2 Second Startup and Shutdown- -Run 4B 32 3.3 Third Startup and Shutdown--Run 4C 33 4 Regenerator Water Jacket Steam Production Runs 1 to 4 35 5 Size Analyses Runs 3 and 4 36 5.1 Acceptor Size Analyses 36 5.2 Char Size Analyses 36 5.3 Gasifier Bed Size Analyses 36 RUN S Foreword 46 1 Summary 4y 2 Discussion 49 2.1 Dolomite and Char Analyses 50 2.2 Startup, Dolomite Addition, Dolomite Circulation 50 2.3 Char Feed To Gasifier 51 2.4 Char Burning 51 2.5 Fluidization Tests 52 RUN 6 Foreword gg 1 Summary * 81 2 Discussion gj 2.1 Glass Model Fluidization Experiment 83 2.2 Atmospheric Fluidization of Limestone in the 86 Gasifier 2.3 Plant Gasifier Tests Under Pressure and 88 Temperature RUN 7 Foreword ^ -125 1 Summary ' 126 2 Discussion • • . 2.1 System Changes From Previous Runs .'.'.' 127 Operating Sequence • • • -^^^ Acceptor and Char Data .'.*''* 130 Operating Conditions .*.'*' 130 2.5 Natural Gas Combustion in the Regenerator *.*.'.'.' 130 2.6 Calcination ,_, 2.7 Material Balance \ ,,, 2.8 Gasification 3 Startup Procedure for Run 7 '.'.'. 177 4 Detailed Operating Instructions .'.'.*.*.'.'.*.'.'. 136 4.1 Preliminary Conditions and Information 17^ 4.2 Procedure ... ^^^ 136 vi 2.2 2.3 2.4 RUN 8 Page Foreword 151 1 Summary 152 2 Discussion 153 2.1 Introduction 153 2.2 Operating Sequence 153 2.3 Operating Conditions 155 2.4 Char and Acceptor Data 155 2.5 Acceptor Circulation 156 2.6 Gasification Data 156 3 Startup Procedure for Run 8 157 4 Detailed Operating Instructions for Run 8 158 4.1 Preliminary Conditions and Information 158 4.2 Procedure 159 5 Modification to Run 8 Procedure to Maintain a 166 Reducing Atmosphere in the Regenerator RUN 9 Foreword 175 1 Summary 176 2 Discussion 177 2.1 Operating Sequence 177 2.2 Operating Conditions 177 2.3 Char and Acceptor Data 178 2.4 Acceptor Circulation 178 2.5 Gasification Data 178 3 Detailed Operating Instructions for Run 9 179 3.1 Preliminary Conditions and Information 179 3.2 Procedure 181 RUN 10 Foreword 196 1 Summary 197 2 Discussion 199 2.1 Operating Sequence 199 2.2 Operating Conditions and Results 202 2.3 Systems Performance 202 3 Startup Procedure for Run 10 208 4 Detailed Operating Instructions for Run 10 211 4.1 Preliminary Conditions and Information 211 4.2 Procedure 212 4.3 Some Shutdown Notes 220 5 Shutdown Program for Run 10 222 6 Chronology of Operations for Run 10 224 vn RUN 11 Page 1 Summary 253 2 Run 11 Test Data 256 3 Chronology of Operations 257 3.1 General 257 3.2 Run llA 257 3.3 Run 1 IB 258 4 Discussion and Analysis 261 4.1 Solids Feed Preparation for Run 11 (100 area) 261 4.2 Process Section (200 area) 264 4.3 HPC and Quench Systems (300 area) 267 5 Future Plans 269 vm LIST OF FIGURES AND TABLES Page RUN 1 Table 1-1. Conditions and Results for Run 1 (2 sheets) 8 Table 1-2. Acceptor Size Analysis for Run 1 10 RUN 2 Table 2-1. Conditions and Results for Run 2 (2 sheets) 17 Table 2-2. Acceptor Size Analysis for Run 2 19 RUN 3 Table 3-1. Conditions and Results for Run 3 (2 sheets) 24 RUN 4 Table 4-1. Gas Rates for Gasifier-Regenerator System--Run 4A 37 Table 4-2. Gas Rates for Gasifier-Regenerator System--Run 4B 38 Table 4-3. Gas Rates for Gasifier-Regenerator System--Run 48 38 Table 4-4. Gas Rates for Gasifier-Regenerator System--Run 4C 39 Table 4-5. Gasifier and Regenerator Overhead Gas Compositions 40 Table 4-6. Regenerator Conditions and Water Jacket Steam Evolution . . 41 Table 4-7. Acceptor Size Analyses for Runs 3 and 4 42 Table 4-8. Char Size Analyses for Runs 3 and 4 43 Table 4-9 Gasifier Bed Size Analyses for Runs 3 and 4 44 RUN 5 Figure 5-1. Gasifier Boot Density During First Char Addition 59 Figure 5-2. Char Burning, October 27, 1972 60 Figure 5-3. Char Burning, October 28, 1972 ! .* .61 Figure 5-4. Gasifier Boot Pressure Drop Record for First 62 Fluidization Test Figure 5-5. Bed Pressure Due to Solids (First Gasifier Bed 63 Expansion Test) Figure 5-6. Gasifier Flow Test: Side Flow Constant at 20 MSCFH, Boot . .64 Flow Variable at 20 to 45 MSCFH Figure 5-7. Gasifier Flow Test: Boot Flow Constant at 20 MSCFH, Side . .65 Flow Variable at 20 to 40 MSCFH Figure 5-8. Predicted Bed Densities for Char and Half-Calcined 66 Dolomite Figure 5-9. Regenerator Flow Test 67 Figure 5-10. Gasifier dPT and TE Locations .....'.'.*.* .* .' .* ,* .' .* * 68 Table 5-1. Dolomite Analytical Summary .*.'.'.' 69 Table 5-2. Char Analytical Summary .* i !.'.*.*.*.*.'.* 70 IX RUN 5(cont.) Page Table 5-3. Results of First Char Feed to Gasifier (2 sheets) ... 71 Table 5-4. Char Combustion Data, October 27,1972 73 Table 5-5. Char Combustion Data, October 28, 1972 74 Table 5-6. Results of Gasifier Bed Expansion--Test 1 75 Table 5-7. Results of Gasifier Bed Expansion- -Test 2 76 Table 5-8. Results of Regenerator Bed Expansion--Test 1 77 Table 5-9. Regenerator Flow Test 2, October 26, 1972 78 RUN 6 Figure 6-1. Steam Addition--Gasifier Fluidization Test 93 Figure 6-2. Glass Model Char and Limestone Fluidization Apparatus . 94 Figure 6-3. Equipment for Testing Showering of Acceptor 95 Figure 6-4. Bed Density vs. Fluidizing Velocity for 6x9 Mesh . . .96 Limestone in Air, 12- inch Glass Model Figure 6-5. Bed Density vs. Fluidizing Velocity for 6 x 16 97 Mesh Limestone in Air, 12-inch Glass Model Figure 6-6. Bed AP vs. Fluidizing Velocity for 6x9 and 98 6 x 16 Mesh Limestone in Air, 12-inch Glass Model Figure 6-7. Bed Density vs. Fluidizing Velocity for 20 x 65 Char . .99 in Inert Gas, 12- inch Glass Model Figure 6-8. Bed AP vs. Fluidizing Velocity for 20 x 65 Mesh . . . .100 Char in Inert Gas, 12- inch Glass Model Figure 6-9. System Setup for Atmospheric Boot Fluidization Tests . .101 Figure 6-10. Bed Pressure Drop as a Function of Velocity for .... 102 6x9 Mesh Limestone Figure 6-11. Bed Pressure Drop as a Function of Velocity for .... 103 6 X 16 Mesh Limestone Table 6-1. Glass Model Circulation Tests--Run 6-IIC 104 Table 6-2. Material Size Analyses, Glass Model Fluidization . . . .105 Tests- -Run 6-IIA, 6- I IB and 6-IIC Table 6-3. Limestone Fluidization Tests--Run 6-IIA (5 sheets) . . .106 Table 6-4. Limestone Fluidization Tests--Run 6-IIA (2 sheets) . . .111 Table 6-5. Char Fluidization Tests--Run 6-IIB (4 sheets) 113 Table 6-6. Atmospheric Gasifier Fluidization Test With 6x9. . . 117 Mesh Limestone (2 sheets) Table 6-7. Atmospheric Gasifier Fluidization Test with 6 x 16 . . .119 Mesh Limestone (2 sheets) Table 6-8. Side Flow Test, January 25, 1973 121 Table 6-9. Special Boot Flow Test, January 26, 1973 122 Table 6-10. Typical Data During Showering Tests at Various 123 Temperatures and Flows RUN 7 Figure 7-1. Regenerator Temperature, Actual CO^ Partial 144 Pressure, and Equilibrium CO, Partial Pressure as a Function of Time Figure 7-2. Gasifier Operation- -Run 7 I45 RUN 7 (cont.) Table 7-1. Table 7-2. Table 7-3. Table 7-4. Figure 8-1. Figure 8-2. Table 8-1. Table 8-2. Table 8-3. Table 8-4. Figure 9-1, Figure 9-2, Table 9-1. Table 9-2. Table 9-3. Table 9-4. Figure 10-1, Figure 10-2, Figure 10-3, Figure 10-4. Figure 10-5, Figure 10-6. Figure 10-7. Table 10-1. Table 10-2. Table 10-3. Acceptor Data for Run 7 Average Char Feed Data for Run 7 Typical Gas Flows, Temperatures, and Compositions for Run 7, February 22, 1973 Typical Gas Flows, Temperatures, and Compositions for Run 7, March 5, 1973 RUN 8 CO2 Partial Pressure and Temperature Profiles . . vs. Time for Run 8 Gasifier Operation- -Run 8 Gas Flows, Compositions, Indicated Bed Densities , and Temperatures for Run 8, April 2, 1973 Typical Gas Flows, Composition and Temperatures . for Run 8, April 3, 1973 Char Data for Run 8 Acceptor Data for Run 8 Page .146 .147 148 149 168 169 .170 171 172 173 RUN 9 Regenerator Temperature, Air Flow, and Actual .... 189 and Equilibrium CO2 Partial Pressure as a Function of Time for Run 9 Gasifier Operation- -Run 9 190 Gas Flows, Compositions, Indicated Bed Densities, . . 191 and Temperatures for Run 9, April 16, 1973 Typical Gas Flows, Compositions, and Temperatures . . 192 for Run 9, April 18, 1973 Char Data for Run 9 193 Acceptor Data for Run 9 194 RUN 10 Gasifier Conditions for Run 10 228 Gasifier Conditions for Run 10 229 Regenerator Conditions for Run 10 230 Regenerator Conditions for Run 10 231 Calcination of Acceptor for Run 10, May 23, 1973 . . 232 Calcination of Acceptor for Run 10, May 30 233 and 31, 1973 E-302 Venturi Modification 234 Conditions and Results for Run 10, May 31, 1973 . . . 235 1730 Hours (3 sheets) Conditions and Results for Run 10, June 1, 1973, . . .238 2130 Hours (3 sheets) Conditions and Results for Run 10, June 2, 1973 ... 241 1630 Hours (3 sheets) XT RUN 10 (cont.) Page Table 10-4. Conditions and Results for Run 10, June 3, 244 1973, 0930 Hours (3 sheets) Table 10-5. Typical Operating Conditions of Gasifier and 247 Regenerator for Run 10 Table 10-6. Overall Material Balances for Run 10, Second 248 Part of Run (3 sheets) Table 10-7. Elemental Balances for Run 10, Second Part of Run . . 251 RUN 11 Figure 11-1. Ring Type Gas Distributor 270 Figure 11-2. Acceptor Calcination Curve- -Run llA 271 Figure 11-3. Acceptor Calcination Curve--Run IIB 272 Figure 11-4. Regenerator CO Concentration and Bed Temperature . . .273 During Calcination, Run llA Figure 11-5. Regenerator CO Concentration and Bed Temperature . . .274 During Calcination, Run IIB Figure 11-6. Regenerator Bed Gas Velocity During Calcination ... 275 Run IIB Figure 11-7. Solids Deposits at Venturi After Run IIB 276 Table 11-1. Preheater Test--Char 277 Table 11-2. Preheater Test (4 sheets) 278 Table 11-3. Gasifier-Regenerator Data, Run llA (2 sheets) .... 282 Table 11-4. Gasifier-Regenerator Data, Run IIB (2 sheets) 284 Table 11-5. Solids Analyses (Average) 286 Table 11-6. Solids Analyses (Average) 287 LIST OF APPENDICES Appendix 11-A-l. Program for Run 11-Plant Startup and 288 Gasification (11 pages) Appendix ll-A-2. Program for Run IIB-Plant Startup and 299 Gasification (3 pages) Appendix 11-B. Runs llA and IIB-Daily Operations Chronology . . 302 (2 pages) Appendix 11-C-l. Shutdown List-Repairs and Revisions Between . . .304 Runs 10 and 11 (5 pages) Appendix ll-C-2. Shutdown List-Repairs and Revisions Between . . .309 Runs llA and IIB (2 pages) xn ABSTRACT For the purpose of demonstrating the feasibility of the CO2 Acceptor Gasification Process, a pilot plant was constructed and oper- ated in Rapid City, South Dakota. This report presents the objectives, mechanical and process problems, solutions to problems, operational details, and plant data for each of the 47 runs which were completed in the 6 years of operation. The pilot plant operations conclusively demonstrated the operational feasibility of the CO2 Acceptor Process to gasify lignites and subbituminous coals. The demonstrated scale-up factor for the pilot plant over previous bench-scale operations was approximately 280 based upon dry coal feed rate. Demonstration of synthesis gas conversion to SNG was also in- cluded in the pilot plant program. For this purpose, a methanation unit which featured the use of a catalyst- in-tube, externally cooled reactor design was constructed and successfully operated. Methanated gas with a heating value of over 900 BTU/SCF was produced. xm RUN 1 RUN lA APRIL 5 to APRIL 11, 1972 RUN IB APRIL 15 to APRIL 25, 1972 CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 1 RUN lA 1 . 1 SUMMARY 1.1.1 Duration (1) Start: April 5, 1972 (2) End : April 11, 1972 1.1.2 Startup Steps Accomplished (1) System pressure test and heat up (2) Establishment of dolomite inventory and MgCOj calcination 1.1.3 Termination (1) Step : Establishment of dolomite inventory (2) Cause: Pressure taps in the gasifier boot were lost. There- fore, the dolomite bed level in the gasifier could not be determined nor could dolomite circulation be attempted. 1.1.4 Difficulties Encountered No major problems other than the loss of pressure taps occurred during the operation. 1.2 DISCUSSION The first startup attempt ended two days after dolomite was fed to the gasifier. The boot pressure recorder, DPR-2034 and DPR-2035, did not indicate any bed level even after the addition of 2500 pounds of dolomite. A test was devised to determine if leaks existed between the pressure impulse lines and the metal sheath which contains the lines. When the purge gas to the probe sheath was increased, the pressure drop readings across the gasifier upper boot and across the gasifier cyclone increased. This indicated that leaks existed between the sheath and the impulse lines. Since the circulation of dolomite between the regener- ator and the gasifier was impossible without the knowledge of the gasifier bed levels, the plant was shut down. Dolomite was then removed from the gasifier. Inspection of the gasifier probe revealed that thermal expansion had caused the protective sheath to pull away from some of the impulse lines. Side pressure taps were installed in both the gasifier and re- generator. * This first run demostrated that: (1) dolomite could be fed into the system through the lignite lockhoppers and (2) calcination of the magnesium portion of the dolomite could be carried out in the gasifier prior to the establishment of a dolomite bed in the regenerator. In a dolomite sample from the gasifier, all the MgCO_ and 15 percent of the CaCO_ was calcined. Table 1-1 (first column) shows the system conditions before the first dolomite addition and gives the screen analysis for a sample of half calcined dolomite. These data indicate only that the proper condi- tions existed for dolomite feeding. Since bed pressure drops could not be measured, no additional meaningful data could be obtained. 2 RUN IB 2 . 1 SUMMARY 2.1.1 Major Modifications (1) Installed side pressure taps in gasifier and regenerator (2) Removed vertical pressure probe from gasifier 2.1.2 Duration (1) Start: April 15, 1972 (2) End : April 25, 1972 2.1.3 Startup Steps Accomplished (1) System pressure test and heat up (2) Establishment of dolomite inventory and MgCO^ calcination (3) Establishment of dolomite circulation 2.1.4 Terminat ion (1) Step : Establishment of dolomite circulation (2) Cause: Relief valve broke on inert gas holder. This caused the gasifier and regenerator beds to slump. Solids filled and plugged off the dolomite lift line to the regenerator. The pressure taps were also lost in the regenerator and gasifier. Finally, the packing on valve, LCV-2003, blew out and system pressure could not be maintained. 2.1.5 Difficulties Encountered (1) Level control valve, LCV-2003, occasionally stuck in the open or closed positions. (2) Pressure taps for the spent dolomite transfer line balance gas controller, dPRC-2037, continually plugged. (3) Water accumulated in flare stack and caused pilot to be extinguished. (The cause of this was not discovered until June. A blind in the 10-inch line from the knock-out drum to the flare had never been removed after construction. All gases entered flare through the 2 inch drain line.) (4) Due to high solids loadings, the suction strainers on the regenerator quench tower pumps, J-203 A and B, continually plugged. (5) Nitrogen supply was not always reliable. Periodically the nitrogen supply to various users was reduced until a nitrogen supply truck could replenish the inventory. 2.2 DISCUSSION 2.2.1 Sequence of Events After installing side pressure taps in the gasifier and regen- erator, the plant was again started up. The first dolomite was charged to the gasifier from lignite lockhoppers on April 17. The prevailing system conditions prior to dolomite feeding are shown in Column 2 of Table 1-1. Also shown are the size consists for the second batch trans- ferred to the regenerator. Before the first dolomite batch could be transferred to the regenerator, workmen had to force LCV-2003 open. Subsequent transfers went smoothly. Later in the run when attempts were made to circulate dolomite, LCV-2003 tended to stick open. On April 22 a flame-out in the lift gas heater, B-205, reduced the recycle gas to the engager pot. This caused the regenerator bed to slump. After many attempts to keep the furnace lit, the low flow switch was jumpered. The furnace ceased to kick out. For a short time the main air compressor, J-202, was used to help lift and refluidize the regenerator bed. When the bed was fluid- ized, the air addition was stopped. An inert gas holder relief valve broke on April 24. The valve was replaced, but both beds slumped and the side pressure taps were lost. In addition, solids filled the dolomite lift line between the engager pot and the regenerator. Since the plug could not be cleared, the plant was shut down. 2.2.2 Dolomite Circulation Dolomite circulation was attempted on April 21 and 23. Smooth circulation was not obtained because transfer line controllers never operated properly and the balance gas purges continually plugged. The operation did demonstrate that the gasifier level control, LCV-2003, operated properly. 2.2.3 Bed Densities The determination of bed densities during the run was difficult. Usually the pressure taps were either not completely covered or they were plugged. Only on two occasions could bed densities be determined with any confidence. On April 18, the gasifier dolomite bed density was calculated from pressure tap measurements to be 59,8 LB/CU FT. This compares with the Consolidation Coal Company (Consol) density correla- tion value of 51.7 LB/CU FT. Good agreement was obtained for the two methods. Small errors in the gas flow measurements, in the calculated particle diameter or an enlargement of the boot diameter by 1 inch, due to refractory shrinkage, would account for the difference. The regen- erator bed density could not be determined at this time because the pressure taps were not fully covered. The bed density for the regenerator was calculated to be 74.0 LB/CU FT from pressure tap measurements (April 21) . An identical value was determined by extrapolating the results obtained from the Consol bed density computer program. Since the bulk bed density for half calcined dolomite is normally about 65 LB/CU FT, the calculated values indicate that the bed was not fluidized. More fluidizing gas than was available was required for the regenerator. The bed density in the gasifier could not be determined because dolomite level in the boot had been lowered below the DPT-2034 top pressure tap. 3 ACCEPTOR SIZE ANALYSES Table 1-2 shows typical size analysis for the Tymochtee dolomite, This material was obtained from C. E. Duff and Son, Hunt svi lie, Ohio. Analyses are given for the as received stone, the sized acceptor (raw charge), and for half calcined acceptor. These data indicate that fluidization, half calcination, transfer and circulation had little effect on the size distribution of the dolomite. rvi B 1-^ • ^■v a. 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'-I ^x CN CO ■^ CN -J e' • • E a. • 01 4-) CO !J t— ( CO O o •p q; tD x: CO 3 a; o CO ►J ::3 00 U4 Di Q z < CO 2 O I—! 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Since a blind had never been removed from the flare line, all waste gases entered the flare through the water drain line. Closing a valve on the drain line caused the gasifier and regenerator pressures to increase. Because the gasifier and regenerator back pressure controllers were unable to react quickly on manual control, reopening the drain valve shocked the system and caused the plant to shut down. 1.5 DIFFICULTIES ENCOUNTERED (1) Pressure taps on the gasifier and regenerator continually plugged. (2) Control valve, LCV-2003, in the dolomite transfer line from the gasifier to the engager pot periodically stuck in either an open or closed position. (3) The gas inlets to the gasifier and regenerator quench towers periodically plugged. (4) Water accumulated in the flare stack and caused a high back pressure to exist on the flare system. 12 (5) Shear pins in the ash lockhopper rotary feeders, L-209 A and B, and the fresh dolomite feeder, L-204, had to be continually replaced. 13 2 DISCUSSION 2.1 SEQUENCE OF EVENTS Prior to the second startup attempt, all solids had been removed from both the gasifier and regenerator. The purge gas system had been cleaned out, and the inert gas generator had been repaired. The inert gas system was repaired because operation of the nitrogen system was both expensive and unreliable. System heat up commenced on June 3, 1972. Dolomite feeding from the lignite lockhoppers to the gasifier was initiated the following day. A bridge apparently formed in the gasifier boot after the first dolomite addition. Surging the system by increasing the recycle flow through FIC-2019 and back blowing into the gasifier boot from the engager pot through LCV-2003 with XCV-2010 closed failed to eliminate the bridge. Finally, the dolomite dump hopper, F-213, was pressurized to 200 PSIG and allowed to blow back into the gasifier. This collapsed the bridge. The dolomite was then transferred to F-213. Subsequent dolomite feeding failed to produce any bridging in the gasifier. During the run solids accumulated in the gas inlets to both the gasifier and regenerator quench towers. These accumulations were caused by water entering into inlet nozzles. Once the nozzle outlets were wetted, dolomite solids adhered to the pipe. Capillary forces caused the water to migrate further inside the nozzle and thus trap more solids. Gradually, solid plugs formed in the nozzle outlets and restricted the gas flows to the towers. Periodic hammering on the nozzle flanges was used to knock loose the deposits. Most dolomite was charged to the system via the lignite lock- hoppers, F-204A and B. Column 1 of Table 2-1 shows the system con- ditions before the first dolomite was fed to the gasifier. After en- tering the gasifier, the dolomite was fluidized in the boot section and allowed to remain long enough to calcine the MgCO portion. The ma- terial was then transferred to the regenerator. Dolomite was also fed to the system through the dolomite lockhopper, F-206. By June 8 a sufficient inventory of dolomite had accumulated in the regenerator to allow for dolomite circulation. Circulation was maintained for 14 hours until the plant was shut down. As the run progressed, a high back pressure developed in the flare system. When the drain line from the flare was valved off, the gasifier and regenerator pressures began to increase. A blind, which had not been removed after construction, was discovered in the 10-inch line leading from the flare knockout drum to the flare. This blind forced all the waste gases to vent to the flare through the two-inch water drain line. When the drain line was valved off and then reopened, the back pressure controllers on the regenerator and gasifier were on manual. This provided no control for the pressure surge which occurred when the drain valve was reopened. The plant was shut down. 14 2.2 DOLOMITE CIRCULATION The 14 hours of continuous dolomite circulation proved that the system was stable and that the proper pressure balances could be main- tained. Frequent pressure surges which were caused by dislodging the solid plugs which formed in the quench tower inlets failed to upset the system. 2.3 BED DENSITIES The second column of Table 2-1 shows the system conditions at a time when sufficient bed level was present in the gasifier boot so that a bed density could be determined. A bed density of 55.6 LB/CU FT was determined from the pressure tap measurements. The bed density deter- mined by the Consol bed expansion correlation is 46.5 LB/CU FT. The agreement is not good. However, the figures do indicate that the bed was fluidized. Since the bed pressure taps continually plugged, deter- mining when the taps were registering correctly was difficult. Column 3 of Table 2-1 shows the system condition at a time when the regenerator bed density could be determined. The pressure tap measurements indicated a density of 68.9 LB/CU FT while the Consol correlation gives a value of 44.5 LB/CU FT. The pressure tap value indicates a non-fluidized condition. However, during the run the re- generator bed appeared to be fluidized. Again, the difference in den- sities can probably be explained by partially plugged pressure taps. 15 3 ACCEPTOR SIZE ANALYSES The raw dolomite material was obtained from C. E. Duff and Son, of Huntsville, Ohio. Analyses are given in Table 2-2 for the raw feed and for the half calcined dolomite. These data indicate that particle degradation occurred once the dolomite entered the system. This is contrary to the results obtained during the first run. That run showed little degradation for the circulated dolomite. Because the data are limited, conclusions concerning the attrition should not be made based on the results of the two runs. 16 CM 00 o r c CO ro in 00 >J m t^ '^ r^ 0) >3- - E CO CM O CO • • e (0 o CO E O •— I o Q (U Oi u X o o i CM CM CM >* • • • • o CM 00 00 ^ Z 3- 00 CM in m vO m r- • • • • • • ■— 1 ^^ •J- 00 CO •—1 m ■— 1 >3- f-i sO m o o o »n •n o r-* CM CO vO •1-t £ >-. a ^-4 CO ■u o o • 3 CO 4J CO c o 0) (1> rt o 3 >-• « CO CO E- •1-1 CO CQ 0) CQ 17 ^OOOt^OO.— lO^ ro ^-^000,— I Z ^ 'H CO (« w ^ (0 CO O Sn^ Z -^ -H CO CO vO O cNi fn CXD 00 .—1 f^ ^ m m cr tvl vO o^ in u-i ^ ^-4 z )— 4 • r^ flJ CO c > <: < o o ^^ CM CM t u w t-l a* «^ CM cmX O O cm cm m X o u a z o < u o C3 ft*. OS 0) M X ^^ "^ 0) CO *J •-4 -H O •-) >N U l-i CN O a oo 00 CM z o - < (0 3 o O "^ 4J < a N -U U *4-l ec -J u CO u (U >» l-l o a; 4-1 4-1 C C O (U -r^ Q 4J w o E ^^ o cioa •^ CQ aa M CO O CM (U O O CN CM ^ U O Z O o >N u O CM CM CM f^ r~- co t^ O^ c e E (U . . ^ (0 CO CO 4J O O • O CO "O CO •• •• q; oj ^ -J- jr .—I V) CU 4-> 4-) -H e CO CO -^ CO Xi CO C C CO dJ 01 4-1 >4-l ^ ^ (/) o CO CO o; ■U 4-1 gj 4-1 Qfi 01 01 O CO -^ — I C u a. Ci. 0) e E 13 > CO CO 0< < CO CO oa w G > o E o u o e CO C OJ 3 O T3 CO 01 (J 6C 00 O 3 4J 1—4 fX 0) •—4 a CO CO C o 0> 13 Qi Oi O U. CO E- j ::: CO u Di a z < CO z o o u I (NI XI CTJ --^ CM on -J in vO 18 c o o t— t «4-l O -I o « X h o 4J cx-o (U 0) o 0) o a. < 5 •o (0 lU a: N w I vO ^s Or-lLTl'^OOlOLnirir^^l^— 1 — ' ro rsi . — . OOOvDoooOr^iomrocxDfMCO OOrsj3-fN0^C0»i-sOm>j00Q000 OOvOr~~nr- <-^n>j.-( oo3'.-<.— lOOO'^ cN en r-< m m CM c O Qi Di O tu CO I— I CO >< < < M l-H CO Di O a, pj CJ u < 4J zs 4= (A V X « 0) •> .-4 4J a U) E 1-« (0 w 1-4 CO c < rsi I 19 RUN 3 JULY 10 to JULY 19, 1972 CO ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 20 1 SUMMARY 1.1 MAJOR MODIFICATIONS (1) Revised side pressure taps to 1/2-inch pipe with rod-out assemblies . (2) Reinstalled gasifier pressure probe using 1/2-inch rather than 1/4-inch tubing for sensing lines. (3) Revised balance gas and balanceAP taps to eliminate coils of 1/4-inch tubing. (4) Repaired line from gasifier to engager pot. 1.2 DURATION (1) Start: July 10, 1972 (2) End : July 19, 1972 1.3 STARTUP STEPS ACCOMPLISHED (1) Pressure test and heat up (2) Establishment of acceptor inventory and MgCO_ calcination (3) Hot acceptor circulation 1.4 TERMINATION (1) Step : Char addition to gasifier (2) Cause: Acceptor lift line ruptured when char dolomite mix- ture was transferred to the regenerator using recycle gas which contained about 18 percent oxygen. Failure of the line was due to a local hot spot caused by the combustion of char by the oxygen-rich recycle gas. 1.5 DIFFICULTIES ENCOUNTERED (1) Gasifier char-acceptor interface was not maintained when char was added to the system while circulating acceptor. (2) Plugs were experienced in the char introduction line from the lignite lockhoppers into the bottom of the gasifier. (3) Gasifier bed pressure differentials were distorted by leaks in the impulse lines. 21 2 DISCUSSION Conditions and results from Run 3 are shown in Table 3-1. The conditions shown are those corresponding to hot acceptor circulation and those prior to the termination of the run when the gasifier char bed height was at its maximum. 2.1 HOT ACCEPTOR CIRCULATION Hot acceptor circulation with the plant in pressure balance was successfully demonstrated during Run 3. Although the char standleg m the gasifier was not sealed, the content in the gasifier recycle gas was reduced to 1.4 MOL percent while the regenerator recycle gas was essentially air. The standleg pressure droos were effectively controlled so that the pressure drops across the butterfly valves in the acceptor loop were zero. A series of circulation tests were performed over a wide range of acceptor circulation rates with no loss of pressure bal- ance. The system was also shown to be stable during plant upsets. 2.2 CHAR ADDITION TO GASIFIER Char feed was begun on July 16. The prevailing plant con- ditions were those shown in the first column on Table 3-1. An attempt was made to feed char while maintaining acceptor circulation. However, a char acceptor mixture was formed in the gasifier boot as indicated by a sharp rise in the regenerator bed temperature and the acceptor lift line temperature. Circulation was continued to the point where all of the incoming 0^ in the air was consumed and the regenerator recycle gas contained -13 percent CO. Attempts to circulate were terminated when it became obvious that despite 2000 LB/HR char feed, the solids level in the gasifier was not increasing. The interface level controller had been set to control the same differential pressure (22 inches H^O) as used previously for acceptor circulation. After ceasing circulation, an attempt was made to fill the gas- ifier with char feed from the lignite lockhoppers. After the fluid- ized bed covered the char inlet in the gasifier, frequent plugs occurred in the inlet line. These plugs were due to having no positive flow from the lockhoppers into the gasifier. The purges to the lignite lockhoppers were ineffective because of leaks in the system. A maximum gasifier char bed height of about 10 feet was achieved. The data in Column 2 of Table 3-1 correspond to this condition. Raw dolomite was injected into the gasifier via a "shot pot." Although the differential pressure drop across the upper portion of the boot increased, the gasifier char acceptor interface was not established. This was shown when acceptor circulation was resumed and combustion occurred in the lift line and regenerator bed. This combustion resulted in the line rupture. 2.3 BED DENSITIES The bed density measurements obtained during Run 3 were distorted by mechanical difficulties. Leaks in the impulse lines were a major 22 source of errors. The regenerator bed density measurement was affected by a collapsed heat shield in the air inlet line (which is included in the densityAP) . A correction of 90 inches H„0 was used for the pre- sence of the collapsed heat shield. This was the AP reading before solids were added to the regenerator. The bottom tap of the boot den- sity AP became plugged when char was added to the gasifier. The regenerator bed densities calculated using the density pres- sure taps are in the range of 61 LB/CU FT, whereas the correlation pre- dicts densities in the range of 54 to 59 LB/CU FT. These differences may be related to errors caused by the collapsed heat shield. The character of fluidization was such that there was no evidence of bed temperature gradients or solids handling problems. The bed density in the boot prior to char introduction calculated using the density AP taps was 60.2 LB/CU FT as opposed to density of 66 LB/CU FT calculated via the correlation. Further measurements were not possible as the tap became plugged. The char bed density could not be calculated because the top density tap was not covered. However, the AP reading was such that the bed density was greater than 42.7 LB/CU FT. The correlation would predict a highly expanded bed at these conditions. The presence of acceptor in the char bed and the possibility of gas bypassing through the gasifier refractory could have contributed to the high bed density. 2.4 CHAR ACCEPTOR INTERFACE During Run 3, a char acceptor mixture formed in the boot immed- iately after the addition of char to the gasifier. Several factors may have contributed to the failure to form an interface. First, cir- culation was continued while char was added. Since there is evidence to suggest that the pressure of the char bed stabilizes the interface, acceptor circulation should be discontinued until the char bed is es- tablished. Second, the presence of fines in the acceptor in the boot could cause unstable fluidization behavior in the boot. Third, the condition of the refractory in the boot could have contributed to un- stable fluidization. According to both the fluidization correlation and the measure boot density, the fluidizing velocity was favorable to the formation of a stable interface. The presence of a clean char acceptor interface, although desir- able, is not essential to the success of the process since the char transferred with dolomite can be compensated for by reducing the amount of char transferred to the regenerator by the char lift line. To insure safety, the acceptor lift gas must be free of oxygen. This can be ac- complished by delaying acceptor circulation until combustion of char is begun in the regenerator and the recycle gas is no longer oxidizing. 23 Run No. : ^ i r Date : July 16, 1972 July 18, 1972 Time : i- 6:00 p.m Ty n mochtee :30 p.m. Acceptor r Size, mesh/wt. 'L 6x8 16.1 14.8 8 X 14 58.6 47.9 14 X 20 15.5 13.8 -20 9.8 23.5 Circulation Yes No TCV-203U loading, psi 7 3 (No Feed) LIC-2003, auto or man Auto Manual Char 4- — Husky - ► Size, mesh/wt. °L (1) +14 4.6 0.4 14 X 100 67.2 45.4 -100 28.2 54.2 Gasif ier Pressure, psig A. 1 Sf> k. V ij\j — 9- Temp. , " F 1315 1200 Flows, MSCFH Boot 40.5 36.7 Bed 19.7 32.9 Total 60.2 69.6 Velocity, ft. /sec » Boot 1.60 1.36 Bed ./ft.3 0.59 0.64 Bed Densities, lb Boot 60.2 dP tap plugged Bed 40.6 Char Bed, ht. , ft • 10 Recycle Gas Composition, Mol. 7« H2 0.9 CH4 CO 2.7 CO- N2 7.6 9.3 90.5 87.0 O2 1.9 Regenerator Pressure, psig 141.5 145 Temp., " F 1210 1280 Flows, MSCFH Air Inlet Air 47.0 51.0 Recycle 8.7 8.7 Acceptor Lift Air Recycle 58.0 62.3 Table 3-1. CONDITIONS AND RESULTS FOR RUN 3 (Sheet 1 of 2) 24 Char Lift Recycle Inert (887, N^ , 127, CO^ ) Total Fluidizing Velocity, ft. /sec. Bed Density, lb. /ft. 3(2) Bed Height, ft. Recycle Gas Composition, Mol. 'k CO CO2 O2 ^ ^ 20.4 (1) As stored in Preheater (2) Correction of 90" H2O allowed on density aP for collapsed heat shield in air inlet line. 5.8 4.3 119.5 126.3 1.71 1.84 67.6 61.1 24.3 24.2 No Analyses ) 0.6 Avail abb e 87.0 Table 3-1. CONDITIONS AND RESULTS FOR RUN 3 (Sheet 2 of 2) 25 RUN 4 RUN 4A AUGUST 10 to AUGUST 12, 1972 RUN 4B AUGUST 13 to AUGUST 14, 1972 RUN 4C AUGUST IS to AUGUST 20, 1972 CO ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 26 FOREWORD The gasification plant was started up and shutdown three times during August. These startup attempts are denoted as Runs 4 A. B and C. Since steady-state conditions were never obtained during the runs, meaningful heat and material balances cannot be made for the sys tern. All data presented in the report are point values and are tran- sient in nature. 27 SUMMARY During the plant startup for Run 4, three major shutdowns occurred. All three resulted from blockages in either vessels or transfer lines. The first shutdown was due to a solids plug in the gasifier boot. Dolomite plugs in the dolomite lift line, CD-208, and in the char lift line, CO-204, were responsible for the second and third shutdowns respectively. 28 2 SIGNIFICANT EVENTS AND OBSERVATIONS 2.1 MAJOR MODIFICATIONS (1) Revised all line AP taps to eliminate coils of 1/4-inch tubing. (2) Revised startup procedure to inert regenerator recycle gas before circulating acceptor in the presence of char. (3) Temporarily abandoned use of the preheater to give better control on the size consist of the char fed to the gasifier 2.2 DURATION (1) Start: August 10, 1972 (2) End : August 20, 1972 2.3 STARTUP STEPS ACCOMPLISHED (1) Pressure test and heat up (2) Establishment of acceptor inventory and calcination of the MgCO (3) Feeding char to the gasifier 2.4 TERMINATION (1) Step : Char combustion and CaCO_ calcination (2) Cause: Disengager pot in char lift line to regenerator became plugged with dolomite that had at sometime agglomerated in the pot. 2.5 TEMPORARY SHUTDOWNS (1) A shutdown occurred on August 12, when the gasifier boot became plugged while attempting to establish the acceptor inventory. (2) A second shutdown occurred while attempting to circulate acceptor. The standleg seal between the gasifier and engager pot was lost, causing the regenerator bed to slump and the acceptor lift line to plug. Although the regenerator bed was refluidized and the lift line was nearly cleared of solids, a persistent plug remained. 2.6 MILESTONES ACHIEVED (1) Successful filling of the gasifier char bed was achieved 29 after properly maintaining the purges in the lockhopper system. (2) Char combustion was initiated in the regenerator for the first time. 2.7 DIFFICULTIES ENCOUNTERED 2.7.1 Gas bypassing through the gasifier refractory caused several problems: (1) Inability to circulate acceptor (see shutdowns above) (2) An unusually high char bed density (3) Irrational behavior of the gasifier boot AP measurements 2.7.2 Difficulties associated with char combustion: (1) Char feed rate control was not adequate to control 3 per- cent CO in the regenerator recycle with 20,000 SCFH air. A more sensitive control device will be installed in the char butterfly valve control loop. (2) A deposit consisting of acceptor cemented together by fused char ash was found in the cone of the regenerator. Apparently the local temperature in the cone was higher than the maximum measured temperature of 1700 F. Better control of the char feed rate (see above) and reduced pre- heat on the regenerator air should reduce the potential for local hot spots. (3) A deposit formed in the gasifier boot gas inlet line consisting of iron, nickel, and sulfur. This deposit, caused by H_S attack of the pipe in the heater coils, will be avoided by operating the heaters at 1450 F (150 F lower than in Run 4) . 30 3 RESULTS AND DISCUSSION 3.1 FIRST STARTUP AND SHUTDOWN - RUN 4 A Plant startup was initiated on August 10. The gas flows es- tablished around the regenerator and gasifier before dolomite was charged to the system are shown in Table 4-1. Dolomite was charged to the gasifier via the lignite lockhopper F-204B. The first batch (1200 pounds) entered the gasifier at 6:00 PM August 11. After the dolomite addition, high differential pressure drop readings of 55 inches H2O and 100 inches H2O were registered by DPR-2002 and DPR-2003 respectively. Additionally, the boot tempera- ture and differential pressure readings indicated that the bed was not fluidized. The high differential pressures obtained are typical of packed bed operation. The temperature readings indicated that the temperature probe was surrounded by a cold, stationary bed of dolomite, which insulated the probe from the hot fluidizing gases. However, dolo- mite transfer to the regenerator was accomplished several times with- out a fluidized bed. A dolomite purge of 470 pounds was removed from the gasifier through the dolomite out hopper, F-213. The material consisted mainly of dolomite and char fines. The fine material had remained in the system since the July shutdown. At that time we believed that the fines were hampering the dolomite fluidization. An experiment with the glass gasifier model had shown that a mixture of fine char and dolomite would increase the chances of plug formation in the gasifier boot. We now believe that gas bypassing through the gasifier boot refractory is the probable cause of the non-fluid bed. After the third shutdown, the gasifier boot was inspected and holes were found in the refractory which allowed the gas to bypass the solids bed. At 7:00 AM August 12, a plug formed in the gasifier boot. The plug was indicated by the inability of the operators to transfer dolo- mite to the regenerator or to dump dolomite to F-213, Plug removal was attempted by pressuring F-213 to 350 PSI and then back blowing into the gasifier. The purge line, UAD-206, was plugged too solidly to allow the pressure to relieve. The gas flow to the gasifier boot was decreased stepwise from 36,700 SCFH to 31,200 SCFH. This was done to allow any gas supported plug in the boot to collapse. No effect was noted. This again indi- cated that the boot was packed with solids. By 12:00 noon August 12, the plant had been shut down. After depressuring the plant, most of the dolomite inventory in the gasifier was removed through the gasifier dump hopper, F-216. The gasifier and regenerator were then pressurized with inert gas to 31 45 PSIG and allowed to^relieve into the engager pot. This emptied the vessels. Both the 180 bend below the engager pot and the tee below the gasifier were removed to facilitate cleanup. Workmen next attempted to disconnect the dolomite purge line, UAD-206, above the block valve, but found that the line was pressurized. Apparently, a plug had formed between the control valve, XCV-2073, and the block valve. After relieving the internal pressure, the line was disconnected. Visual inspection of the line revealed that the plug had collapsed during depressurization. Air was blown through the line to insure that a plug was not located in the 45° bend. Some of the material removed from F-213 was wet. This indicated that water had entered UAD-206 and caused the dolomite to bind together. A week later, following the third shutdown, a crack was discovered in the upper flange on UAD-206. This crack probably allowed water from the water jacket to enter the line. After the cleanout the system was again put back together and heated up. 3.2 SECOND STARTUP AND SHUTDOWN - RUN 4 B By 5:30 AM August 13, the system was ready for dolomite addition. The gas flow rates around the gasifier and regenerator are shown in Table 4-2. The first batch of 500 pounds of dolomite charged to the gasifier caused the boot temperature to drop from 1440° F to 670° P. Again a fluidized bed was not obtained. The flow reading on FIC-2019 was in- creased by about 15,000 SCFH in order to get the dolomite fluidized. Future dolomite additions to the gasifier were made by periodically operating of the lignite feeder, F-207B. The feeder was operated for 2 out of every 20 minutes. This provided an average dolomite feed rate of 300 LB/HR. The boot temperature remained above 1150° F. Dolomite was also continuously fed to the regenerator through the dolomite lockhopper F-206 and the engager pot at a rate of approximately 700 LB/HR. The first transfer of dolomite to the regenerator from the gasifier occurred at 9:35 AM August 13. The gas flow rates around the system at that time are shown in Table 4-3. At 2:15 AM August 14, the regenerator bed almost slumped when F-206 was depressurized for dolomite refilling. The bottom block valve above the dolomite feeder, L-204, leaked through and caused the lift line, CD-208, to be starved for gas. The air flow to the regenerator was increased by 14,000 SCFH and the block valve below L-204 was closed. Prompt action by the operator kept the regenerator bed fluidized and averted a shutdown. 32 After the system recovered, more dolomite was transferred to the regenerator. The bed level in the regenerator reached the dolomite transfer line to the gasifier by 3:00 AM August 14. By 6:10 AM the regenerator inventory was sufficient so that dolomite could be circu- lated between the regenerator and gasifier. Dolomite was circulated several times between the two vessels Difficulties were observed with gasifier to engager pot transfer. The seal m this transfer line was lost at 1:20 PM August 14. The lift gas vented into the gasifier, causing the regenerator bed to slump The bed was refluidized by increasing the air rate to the regenerator. Dolomite was drained from the lift line into the engager pot. After closing XCV- ^010 the engager pot was back blown into the gasifier. This did not ^■^rv^v^on!^^^ ^^"^ completely, a plug remained between the regenerator and XCV-2010. The plant operators were unable to clear the plug Raising the engager pot pressure to 265 PSI to blow the plug into the regenerator failed to have any effect. The plant was shut down. After degressurizing, XCV-2010 was opened and the regenerator dumped. The 180 bend below the engager pot and the tee below the gas- ifier were both removed to aid in draining the solids from the reactors Inspection of the gasifier boot with a mirror revealed what appeared to' be a large horizontal crack in the refractory near the bottom of the boot. Discovery of this crack lent further support to the theory that gas was bypassing the solids in the gasifier boot. 3.3 THIRD STARTUP AND SHUTDOWN - RUN 4C The system was again started up on August 15. The first dolomite was charged to the gasifier by 8:15 AM August 16. The continuous feed- ing of dolomite from F-206 was resumed. After the regenerator upper bed DPR (DPR-2020) read 45 to 50 inches H^O and the flow of FRC-2015 was changed from recycle gas to inert gas, char was fed to the gasifier. Char feeding started at 8-00 AM August 17. The gas flow rates around the gasifier-regenerator system are given m Table 4-4. Column 1 gives the rates before char was added to the gasifier. Column 2 shows the rates during the times char was added to the gasifier, and Column 3 shows the gas rates just before char was transferred to the regenerator. Compositions for the overhead gases from the gasifier and regen- erator are given m Table 4-5. These data were obtained for the time period during which char was fed to and burned in the regenerator The hT.h hlTnl f ^^^j:egeneTatOT overhead gas oxygen concentration 'was high before char addition to the regenerator (lo.U percent), that it declined to 0.0 percent during the time char was burning and that it IT. .T^"^^^^'^ T °^'^'^^' ^^'"^ ^^^^^ ^^^ ^^^^ ^^^ consumed. These pr^duc^efin'^he ^^ ^^^^°^^"' ^^^^°^ -"-^^^' -^ "^-^-e wer\" 33 Char feeding to the regenerator via the char lift line and LCV- 2002 started at 11:55 AM August 18. The seal in the char lift line was soon lost but was reestablished by 2:00 PM. More char was transferred to the regenerator. The regenerator bed temperature increased to a maximum of 1700°F at 4:50 PM. Again the seal in the char lift line was lost (5:15 PM) . Attempts were made to reestablish the seal. At 9:30 PM the char lift line plugged between the disengager pot, F-224, and the regen- erator. This was indicated by the lack of a pressure drop measurement on the char lift line and the high reading for DPR-2004. The char lift line was back blown from the regenerator to the gasifier. This caused dolomite to flow into the char line from the regenerator. The char lift line then oecaroe plugged. All attempts to back blow the plug into the gasifier or to move the plug into the regenerator failed. Even pres- surizing the line with the 500 PSI discharge of the CO^ compressor failed to dislodge the plug. At 8:20 PM August 20 the plant was shut down. Following the third shutdown, the solids were removed from the gasifier and regenerator. No evidence of char was found in the dolomite from the regenerator. The 600 pounds (approximate) of char which had been transferred to the regenerator was completely consumed. A hard buildup of dolomite was found on the bottom walls of the regenerator. From seven to nine cubic feet of material was chipped off the refractory. The material was found to be mainly compacted dolomite. Some ash-fused dolomite clinkers were also found. A dolomite ball was found in the disengager pot. This ball obstructed the pot exit. However, the ball quickly disintegrated from a gentle prodding. The char lift line was found to be plugged with char and dolomite. The lower head was removed from the gasifier. Inspection of the head showed that the crack in the gasifier boot, which was discovered during the second shutdown, was actually a separation of refractory along the seam between the head and the gasifier shell. The separation allowed gas to penetrate and erode passageways into the soft outer refractory liner. The holes in the refractory prove that considerable quantities of gas bypassed the solids bed in the gasifier. This gas bypass explains the loss of pressure taps in the booi and the high bed densities obtained in the gasifier upper bed. The tee below the gasifier was removed and inspected. Several pounds of iron-nickel sulfide was found in the line. This material apparently came from se^' ons lA and IIA of the gasifier recycle heater B-201. Hydrogen sulfide from the coal char had attacked the furnace tubes and removed some metal. Since ultrasonic testing of the tube wall thicknesses did not reveal any substantial metal losses, the losses were probably evenly distributed over a large area. Steps are being taken to eliminate the problem during future runs. 34 4 REGENERATOR WATER JACKET STEAM PRODUCTION RUNS 1 to 4 The steam evolution from the regenerator water jacket is pro- portional to the system heat loss and is indicative of the condition of the vessel refractory. The results of an investigation of the regen- erator jacket steam production over the first four runs are reported herein. Table 4-6 gives the regenerator conditions and jacket steam evolution at two different bed heights for each of the runs. The bed heights correspond to the level of the acceptor withdrawal line (20 feet) and the maximum bed height achieved (about 25 feet) . The data show an appreciable increase in steam production with time. This increase may indicate gas bypassing through the regenerator refractory. The level steam production rose dramatically during Run 3 after the first occurrance of char combustion and the related elevated temperatures (1680 F maximum) . Despite this evidence, no large cracks in the refractory have been observed by visual examination through a 10-inch hole in thf^ top of the regenerator. Also, in Run 4, the regenerator bed temperature was PTumn!'^ u^^'^u^ responsive to relatively small heat releases (1 million BTU/HR) while burning char. Prior to char combustion in Run 4 the bed temperature gradient was less than 25° F, indicating a well fluidized Ded. The evidence of gas bypassing indicated by the water jacket steam evolution is not supported by other indications. This suggests that the problem is not yet severe. However, corrective action will be required If the trend toward higher heat loss continues. 35 5 SIZE ANALYSES RUNS 3 and 4 The size analyses of samples obtained during Runs 3 and 4 are reported herein. The following Tables are attached: Table 4-7. Acceptor Size Analyses - Runs 3^4 Table 4-8. Char Size Analyses - Runs 3^4 Table 4-9. Gasifier Bed Analyses - Runs 3 § 4 5.1 ACCEPTOR SIZE ANALYSES In Table 4-7, a typical size analysis of the Tymochtee dolomite as received is shown. This material is designated no. 7 grind. The supplier is C. E. Duff and Son, Huntsville, Ohio. Also shown are the average size analyses of the acceptor charged to the plant via the lignite lockhoppers and the acceptor lockhopper during Runs 3 and 4. The charged material was prepared by screening the NO. 7 stone at 6 X 16 mesh. The range of maximum and minimum weight percentage observed for each size fraction is reported. The final regenerator inventory size analyses are given to show the effects of fluidization and circulation on the size consist. 5.2 CHAR SIZE ANALYSES Analyses of char from the grinding system in Runs 3 and 4 and the preheater in Run 3 are reported in Table 4-8. The preheater was not used in Run 4 due to apparent size degradation occuring in Run 3. During Run 3, char grinding was completed on July 15. The preheater size analyses for July 16, 17, and 18 show a definite trend towards a smaller size consist. In Run 4, the ground char was stored in tote bins before being charged via the lignite lockhopper. 5.3 GASIFIER BED SIZE ANALYSES The gasifier bed size analyses are reported in Table 4-9. These materials are listed separately since they contain both char and accep- tor. The weight percentage acceptor in the bed was determined in the lab on the basis of the ratio of calcium and magnesium in the sample as compared the Ca-to-Mg ratio in the char ash and acceptor. The reported number is, at best, a rough estimate. 36 Date: 8/11/72 Time: 4:30 AM Location Gasifier Upper Bed Gasifier Boot Char Lift Line Air Introduction Line Engager Pot Gasifier Charge Gas Gas Flow Element Rate, SCFH Recycle ( ~5% 0^) FR-2260 16,300 Recycle ( -5% 0^) FIC-2019 45,500 Recycle (Air) FRC-2015 5,000 Recycle (Air) FRC-2032 24,400 Air Charge FRC-2113 36,000 Air Charge FRC-2C13 Recycle (Air) FRC-2014 59,300 Inert Gas Make !-Up FIC-2028 5,110 Table 4-1. GAS RATES FOR GASIFIER-REGENERATOR SYSTEM -RUN 4A 37 Date: 8/13/72 Time: 5:30 AM Location Gas Flow Element Rate, SCFH Gasifier Upper Bed Recycle (-5% O2) FR-2260 14,300 Gasifier Boot Recycle (—5% O2) FIC-2019 41,200 Char Lift Line Recycle (Air) FRC-2015 5,900 Air Introduction Line < jRecycle (Air) FRC-2032 24,400 - Air Charge FRC-2113 29,700 Engager Pot < r Air Charge / Recycle (Air) FRC-2013 FRC-2014 54,300 Gasifier Charge Gas Inert Gas Make-up FIC-2028 5,030 Table 4-2. GAS RATES FOR GASIFIER-REGENERATOR SYSTEM - RUN 4B Date: 8/13/72 Time: 9:35 AM Location Gas Gasifier Upper Bed Recycle (~5% Oj) Gasifier Boot Recycle (-'5% O2) Char Lift Line Recycle (Air) Recycle (Air) Air Introduction Line' Air Charge J Air Charge Engager Pot Gasifier Charge gas Inert Gas Make-up 1 Recycle (Air) Flow Element Rate, SCFH FR-2260 18,500 FIC-2019 55,600 FRC-201S 5,700 FRC-2032 24,400 FRC-2113 35,900 FRC-2013 FRC-2014 58,400 FIC-2028 5,300 Table 4-3. GAS RATES FOR GASIFIER-REGENERATOR SYSTEM - RUN 4B 38 Date: August Time: 17 17 18 5:30 AM 11:30 AM 11:30 AM Location Gasifier Upper Bed Gasifier Boot Char Lift Line Air Introduction Line Engager Pot Recycle Recycle Recycle (Inert Gas) Flow Element FR-2260 FIC-2019 FRC-2015 Recycle FRC-2032 Air Charge FRC-2113 Air Charge FRC-2013 Recycle FRC-2014 V. (Air) Gasifier Charge Gas Inert Gas FIC-2028 Make-up Rate, SCFH 12 3 13,800 17,400 44,800 48,700 45,300 24,200 5,500 5,500 5,500 24,400 25,200 24,400 33,800 33,800 11,300 59,000 59,000 60,900 5,000 5,000 6,900 Table 4-4. GAS RATES FOR GASIFIER-REGENERATOR SYSTEM - RUN 4C 39 Gasifier Date Time Composition, VOL % 0^ CO CO2 N2+A^ H2 CH^ .4 4.7 9.7 85.2 8.2 6.6 81.5 2.9 1.1 7.8 5.1 S3. 9 2.7 0.5 7.3 6.5 82.5 3.0 0.7 6.9 6.2 85.4 1.5 Composition, VOL % 0^ CO CO^ N_+A H- CH. 8/18 5:00 AM 16.8 -- 2.4 80.8 8/18 12:15 PM 0.5 1.8 18.7 79.0 8/18 2:15 PM 0.3 6.0 13.4 80.3 8/18 6:10 PM 12.6 -- 4.7 82.7 8/18 8:00 PM 12.7 -- 3.8 83.5 8/19 8:00 AM 15.7 — 3.7 80.6 Table 4-5. GASIFIER AND REGENERATOR OVERHEAD GAS COMPOSITIONS 8/18 5:00 AM 8/18 3:00 PM 8/18 6:30 PM 8/18 8:00 PM 8/19 8:0D AM Regenerator Date Time 40 00 e o o o CO o in o • . — 1 in vO ro cn in CN CNI r— 1 (N . — I CO B CO O o in ^0 r^ in CNI * O O — 1 O in in in CM v£) -3- ^ ON —I in Csj o r~ m in • r^ O CN -l 0^ VM •1-t X (0 OJ o > E CO a> 4-1 CO 41 o 1-1 4-) o c **-( ■U 0) o a > M c -o c (U t-^ C 3 c w ci &0 O 4J •HI CO (Ul < o 0C\ I CO 1 00 e; < C 00 o < mo~*cNinoooooo— I rO CO «N 2 oo o o o o • • • • • • • • < o r— 1 — 1 in CO o • 1—1 o o o o • • • • • • • • • • <: o ■—1 CO u-l o r-4 r-l 1—1 m I— 1 o CO CO • ^^ o t— < OO O a> r— 1 O o • • • • • • • • • • • <: o o <: i-^vOCNtNCOOOCO^fOvOvOvO OOosivoocooOvtin.— 10000 m o 1 oo^invj-^QOvOco •— i^ocov£>coococNi>a"\o<}- OOcsimOi— icovor^incMoo i-< OJ fS 1— I ^^ ^^ r^ •-j,-ir^ 1— •r^mr^O-4'ino OOi— ivOcvJr^OcOvOcoOtN 1— I ,_( CSI 1— < ^^ i-^ ,^ * in o CN O - •J < M 00 I o i-H 43 v> (0 (U 4J c B N 3 OT •H o 43 00'-^— l^<-)^i>■— 'i^r~-oor^PO>* .— I .—I r-l csi t— < r-l o a- Q 00 OOOOOOO^CXDfSvOii-lO^OrO--* to Z Di Oi o CO CO >- < in I— iirimOfMo^r--mro\0<— I 00 vO CO o x: w 0) S ^-v •« CN ■u ^^ W) u •H o OT 4-1 c • a- o o 0) o z o o JcNPO>3'\00 • o •1-1 M lO l-l 60 iTl o s CM 4J o Q- 1 • 0) O «j O o « >M •o o c « •H >-l m CO CO « V £ JD J= o o C C J= o t— 1 ^ o T3 «> X3 (U i-i JJ Q) c CO ■U •p-l t— 1 (U ,—1 CM < ^^ ^— ' UJ M I— I CO a UJ cc a: u tu (-H C/) < I 43 44 RUN 5 OCTOBER 9 to NOVEMBER 1, 1972 CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 45 FOREWORD Run 5 was initiated on October 9, 1972, after a prolonged turn- around, and terminated on November 1, 1972. During the seven-week shut- down, some 152 items of maintenance and plant revision had been ac- complished in an attempt to correct the numerous problems encountered in previous runs. The principle objectives of Run 5 were: (1) To achieve total calcination of dolomite, and (2) to produce gas by reaction of char and steam. This report reviews the events of Run 5, presents the significant data obtained, attempts to interpret the data, and reviews briefly the major problems encountered. 46 1 SUMMARY The plant was started up, and desired levels of dolomite were established in the gasifier and regenerator in routine fashion. Circulation of hot dolomite between the gasifier and regenerator was conducted at various transfer rates and with various flows of fluid- izing gas. Circulation was smooth and relatively trouble-free. Leaks in the feeding equipment presented some problems in feeding char to the gasifier, but these leaks were corrected. When feeding at the lowest possible rates, the gasifier bed cooled, and, therefore, feed was interrupted periodically to avoid cooling the bed below 1100° F. Char was successfully transferred from the gasifier to the re- generator and burned. Combustion was definitely achieved and a reducing atmosphere attained, with oxygen depleted and carbon monoxide in the off-gas in the one-to-three-percent range. Although samples for direct analytical proof of calcination were not obtained, equilibrium condi- tions were achieved to reduce calcium carbonate to calcium oxide. Fluidization tests were conducted throughout the run. These included tests on the gasifier with dolomite only and with both dolomite and char, and tests on the regenerator. Results of the fluidization tests were not conclusive and did not follow predictions based on ear- lier pilot plant work at Library. Dolomite fines probably affected the results. About 25 percent of the material removed from the system after the run passed through a Tyler NO. 20 screen. A dolomite-char interface apparently was not maintained in the gasifier, and bed densities throughout the gasifier were quite uniform. Low bed densities predicted from the experimental work at Library were never observed. Additional studies are needed to better understand the fluid- ization characteristics of the equipment at Rapid City. Simple atmos- pheric temperature and pressure tests, both in the gasifier and the glass model, have been planned, based on the information garnered in Run 1972?^^^ ^^^^^ ^^^^ ^^^" started at the time of this writing (December Shutdown was initiated because of increasingly frequent and difficult upsets, mainly in the quench system, external to the gasifier- regenerator equipment. During shutdown, char was burned in the regen- erator, but this was stopped when excessive jacket steam generation was 47 After the regenerator was cooled and opened, the dolomite bed was found to be agglomerated. Since there was no evidence of ash fusion, the agglomeration probably resulted from the inability to maintain reducing conditions in the regenerator. This allowed the formation of the transient liquid (calcium sulfide-calcium sulfate) which cemented the acceptor particles together. Also the regenerator refractory had a large hole opposite the air introduction line, and there was severe deterioration of the soft insulation between the vessel wall and the hard interior insulation. The basic plan for the run was carried through, but was stopped just short of gasification. 48 2 DISCUSSION Run 5 was initiated on October 9 and completed on November 1, 1972. The plan was to proceed stepwise from startup through char gas- ification, pausing at each step to establish steady operating conditions and record operating data. Planned steps were to: bring the plant up to operating pressure and temperature with hot gas circulation; add dolomite to the system; circulate hot dolomite between the gasifier and regenerator; add char to the gasifier; transfer char from the gasifier to the regenerator, burning the char in the regenerator to completely calcine the dolomite; add steam to the gasifier to produce gas. At various steps, fluidization data were to be taken. All steps except gasification were accomplished to some degree. The first few days of operation were used in pressure testing, and m correcting leaks, obstructions, and malfunctioning valves. By October 16, the system had been heated and filled with dolo- mite, and hot dolomite circulation was established. Tests were per- formed to show the effects of varying gas flows. On October 22, addition of char to the gasifier was initiated and, by October 25, the level in the gasifier was 26 feet. Flow tests were conducted, the level raised to 30 feet, and additional flow tests conducted. Transfer of char from the gasifier to the regenerator was started October 27, and was continued intermittently for three days. During and after each transfer of char to the regenerator, it was burned under con- trolled conditions. Since regenerator solids samples could not be taken, direct analytical proof of calcination was not attained. However the regenerator temperature records indicate that total calcination was ' at one time achieved. During the above operations there were numerous upsets to the plant, mainly in the quench systems and other equipment external to the gasifier and regenerator. The mounting frequency and seriousness of these upsets led to the decision to shut down. The shutdown was com- pleted on November 1. Although the objectives of the run were not fully accomplished both the quality and the quantity of technical data obtained were sub- stantially greater than in previous runs. Through training and exper- ience, the operating staff succeeded in bringing the plant through numerous upsets that, in earlier months, would have caused immediate snutdown. 49 2.1 DOLOMITE AND CHAR ANALYSES Numerous chemical and size analyses were made of dolomite and char, both of feedstock and of material removed from the system during and after the run. Relatively few in-process samples were analyzed, because several sample systems were plugged. Dolomite analyses, mostly averages, are shown in Table 5-1. The dolomite feedstock early in the run, as represented by average analyses for October 14, 15, and 16, was quite high in fines, 9 to 16 percent passing through a Tyler NO. 20 screen. Subsequent to October 16, all dolomite fef^dstock was doublescreened and any batches showing more than 5 percent fines were rescreened. The average feedstock after October 16 showed 4 percent fines. Thus, high-fines material was charged to the system through October 16, the day on which hot dolomite circulation was started, but better material was charged thereafter. The excessive fines in the initial feedstock account, in part, for the high fines in material removed from the system. The average analyses shown in Table 5-1 for October 16, 17, 21, and 22, have 26 to 35 percent fines. These were higher than any feedstock material, how- ever, so there was some attrition in the system. The sample taken at 0200 October 22 is the last ssimple before char addition. The chemical analyses in Table 5-1 show an increase in sulfate and miscellaneous metal oxides between the feedstock and material removed from the system, indicating the presence of char ash. There was no evidence, however, of fused ash. As shown in Table 5-2, char removed from the gasifier after the run has a slightly lower heating value and a slightly higher ash con- tent than the feedstock. This indicates a small (and expected) amount of devolatilization in the gasifier by the hot fluidizing gas. The smaller amount of fines in material removed from the bed, compared to feedstock, indicates rejection of fines through the gasifier cyclone. 2.2 STARTUP, DOLOMITE ADDITION, DOLOMITE CIRCULATION Startup for Run 5 was relatively uneventful. There were some flange and valve leaks and other minor problems with the equipment, such as are normally encountered after a prolonged shutdown. It was necessary to depressure the system once to correct these problems. Startup required six days. Dolomite addition was smooth. It was fed directly both to the gasifier and to the regenerator, and some was added to the regenerator by transfer from the gasifier. Dolomite was circulated in a loop from the regenerator to the gasifier and back at various rates. Stable circulation was maintained for about 2-1/2 days. The only upsets were from problems external to the circulation system itself. For example, when a downstream vent valve stuck, the system depressured partially and blew out dolomite; it was necessary to recharge the system with fresh dolomite. 50 2.3 CHAR FEED TO GASIFIER After the dolomite circulation tests had been completed, circu- lation was discontinued and char was added to the gasifier. Feed was continuous at a rate about as low as the rotary feeders could be oper- ated, until the bed temperature dropped to near 1100° F, when feed was discontinued until bed temperatures recovered; then continuous char feed was resumed until bed temperature dropped again. Char feed was smooth so long as there were no leaks in the hopper and feed system. Feed had to be discontinued occasionally while leaks were repaired. Data for the first char addition are recorded in Table 5-3. Boot bed density data, as calculated from differential pressure measurements are plotted in Figure 5-1 as a function of time. Also shown are the periods during which char was being added. Bed density rose smoothly from 65 to 75 LB/CU FT during the first two to three hours, dropped sharply to about 60 LB/CU FT, then continued to drop slowly over a 14 hour period to about 45 LB/CU FT. The behavior of boot bed density during char addition, as shown in Figure 5-1, has no definite explanation. Additional tests and ob- servations (now planned for Run 6) are required to obtain a better understanding of bed behavior during char addition. 2.4 CHAR BURNING On the afternoon of October 27, and again on October 28, char was transferred from the gasifier to the regenerator to establish combustion of char and calcination of calcium carbonate to calcium oxide. Oper- ating data for the two combustion runs are tabulated in Tables 5-4 and 5-5. On October 27, char was transferred continuously from 1235 to 1310 hours and from 1345 to 1700 hours. (The short interruption re- sulted from solids hangup above the butterfly feed control valve.) As shown in Figure 5-2, the temperature of the regenerator fluid bed in- creased rather steadily, except for a drop during the interruption of char transfer. The bed density decreased, which would be expected because of the increased gas velocity resulting from higher temperature. Carbon dioixde content of the overhead gas rose immediately. After about two hours, char feed was adjusted so that oxygen in the overhead gas fell to zero and stayed there; carbon monoxide concentration rose from zero and stayed in the range of 0.5 to 1.5 percent. During the run, steam generation in the vessel jacket was low and steady. The data for the October 27 char burning run definitely show that combustion took place, that oxygen in the system was depleted, and that a reducing atmosphere was established. Equilibrium temperatures were obtained for calcining calcium carbonate to calcium oxide, but solid 51 samples were not obtained for analytical confirmation. Significantly/, the temperature gradient across the regenerator bed was 27 at 1700 F, indicating a well fluidized bed with good dispersion of the combustion heat release. The above run was terminated because of major upsets with severe plugging in the quench systems. Another run was attempted the next day, October 28; the data are recorded and displayed in Table 5-5 and Figure 5-3. The thermocouple probe had failed earlier in the day and one temp- orary thermocouple had been inserted through a side tap. The results were similar to the October 27 run. Char transfer was intermittent during the middle of the run due to solid hangups aoove the butterfly valve; this is shown in Figure 5-3 by fall -off in temperature, by drop in both carbon dioxide and monoxide concentration, and by return of oxygen to the system between 1400 and 1800 hours. Again the run was terminated because of upsets from plugging in the quench systems. Char combustion continued on October 29 and 30. However, con- tinuing upsets in the quench systems made control of the CO concentra- tion in the flue gas impossible. By October 29, the regenerator bed P's indicated that the bed was no longer fluidized. Because of inad- equate temperature indication, bed gradient confirmation was not pos- sible. On the 30th, char combustion was discontinued when the steam generation from the regenerator jacket increased markedly. Subsequent inspection of the reactor revealed that: (1) The regenerator bed was totally agglomerated. (2) The regenerator refractory had been pierced directly opposite the air introduction line. The physical appearance of the bed material suggested that the transient liquid experienced in the bench scale work might be respon- sible for the agglomeration. The frequent periods of combustion at oxidizing and neutral conditions could be responsible for its occur- rence. Apparently the refractory damage resulted when the inlet air flow channeled through the agglomerated bed. Significantly, there was absolutely no evidence of fused ash in the bed. 2.5 FLUIDIZATION TESTS During Run 5, fluidization tests were conducted for both the gasifier and the regenerator. The tests were made to determine the effect of gas rate on bed expansion. Results are shown in Tables 5-6 through 5-9 and in Figures 5-4 through 5-9. 2.5.1 Tests Description The first gasifier fluidization test was conducted with half- calcined dolomite in the gasifier boot (char had not been added to the system) . At all times, the circulation of dolomite between the gasifier and regenerator was maintained throughout the test. This test demon- strated that bed level could be controlled smoothly by boot level 52 controller LIC-2003. During the test, the boot gas flow was varied between 30,000 and 51,000 SCFH, while the side flow (at the transition section) remained relatively constant at 18,000 to 19,000 SCFH. After the above test with dolomite only, a 26-foot-high char bed was established in the gasifier, and the second set of fluidization tests were conducted. Unfortunately, soon after the char addition to the gasifier, the solids interface in the boot was lost; the dolomite and char became mixed. Despite the loss of interface, tests were made to determine what effect gas velocity had on char bed expansion. Init- ially, only the boot gas flow was varied; the side flow remained con- stant at 20,000 SCFH. Then the boot flow was held constant at 20,000 SCFH and the side flow varied. This provided some data on flow dis- tribution and how it affects bed fluidization. Two regenerator bed expansion tests were also conducted. The lift line gas rate was maintained constant throughout the first test, while the air rate to the air interduction line was varied. The total gas rate varied from 130,000 to 190,000 SCFH. These data are considered to be qualitative since continued bed calcination may have occurred. Effects of both total gas rate and place of entry were studied in the second regenerator test. Each of the four gas flows to the regen- erator was varied at least once. In one case, the same total flow was obtained while two of the four flows were different. The data for this test are more complete than those taken during the first fluidization test. 2.5.2 Factors Affecting Fluidization and Differential Pressure Measurement In addition to gas flow, the main factors affecting fluidizafion are: (1) particle size, (2) L/D ratio (bed height to bed diameter), (3) DP/D (ratio of particle diameter to bed diameter) , and (4) place of gas entry. Of the above, only place of entry was studied in any detail. This was studied by varying the gas flows to the side and bottom of each reactor. In analyzing the data, particular attention should be given to the high amount of fines contained in the dolomite beds (see Table 5-1). The presence of fines may help explain some unusual bed conditions. Pressure tap configuration may also have some affect on the test results. Three configurations were used in the system: (1) side taps, (2) probe taps, and (3) hybrids. The side taps enter through the reactor walls and extend to the refractory inner surface. These taps are located either directly under each other (inline) or are rotated some degree apart (opposed). The inline taps are dPR-2002 in the gas- ifier and dPR-2020 in the regenerator. Opposed taps are dPR-2070 with taps rotated 135 degrees apart, and dPR-2001, with taps rotated 90 degrees; both are in the gasifier. The probe taps extend down what is approximately the center of the gasifier and are contained in a common pipe sheath. The recorders attached to this probe are: dPR-2031, dPR- 53 2032, dPR-2033, dPR-2034, and dPR-2035. Hybrids are crosses between the probe and side taps such as dPR-2005 in the gasifier, or are taps with one tap in a gas line and the other in the fluid bed; dPR-2003 in the gasifier and dPR-2018 in the regenerator are examples. The location of pressure taps and thermocouples on the gasifier are shown in Figure 5-10, 2.5.3 Results of First Gasifier Test Much confusion exists concerning the interpretation of the data represented by the differential pressure recorders. To aid in analyzing these data, the differential pressure record charts for the first gas- ifier fluid! zation test are shown in Figure 5-4. This figure is a composite of three pressure-recorder strip charts; since the pressures fluctuate rapidly, the pressure records have been outlined to define more clearly the spans of pen movements. The test duration shown is divided into six time intervals, as shown at the left margin of Figure 5-4. Interval 1. Gas flows of 40,000 SCFH to the boot and 10,000 SCFH to the side (at the transition section) were established. Level control LIC-2003 was operated at a setting of 17 inches HO. Interval 2. The level setting for LIC-2003 was increased to 23- to-25 inches HO to insure complete coverage of dPR-2002 pressure taps. All gas rates were held constant. Comparison of the low density (57.8 LB/CU FT) calculated from dPR-2002 reading, with the density (66.7 LB/CU FT) calculated from the dPR-2034 reading, indicated incomplete coverage of the low side pressure tap for dPR-2002. Assuming no density gradient in the fluid bed, both densities should have been identical. Therefore, raising the bed level should have, and did, greatly improve the density agreement (see Table 5-6) . Interval 3. After making the change in level control setting, the system was allowed to line out before the second set of data was taken. The continuous width and straightness of the dPR-2035 record demonstrates good level control. Interval 4. The boot flow was increased to 51,000 SCFH in an effort to increase bed expansion. Interval 5. In this interval the gas rate was decreased from 51,000 to 34,000 SCFH. Level control was also reset to 20-to-22 inches HO, Interval 6. The gas flow to the boot was further decreased to 30,000 SCFH and the level control, LIC-2003, was reset to 25 inches H-0. The system then lined out. Presently, no correlation exists between fluid bed dynamics and differential pressure recorder activity. However, the following inter- pretations for recorder activity are suggested, since they appear to be consistent with what would be expected for a fluid bed operation. 54 Figure 5-4 shows that bed density decreased with increased gas flow and that larger bubbles formed with increased bed activity. When the boot gas flow was increased from 40,000 to 51,000 SCFH, all dif- ferential pressure recorders acted as expected; the reading for dPR-2002 and dPR-2034 decreased while the readings for dPR-2001 and dPR-2003 increased. (See Figure 5-10 for dPR locations.) The pen span for dPR- 2035 increased with the increased gas flow. This was probably due to a more active bed in which large bubbles have continually formed and collapsed. The shape of the record for dPR-2001 adds credence to this supposition. The continual return of the recorder pen to the zero position (10 lines) indicates that solids only periodically covered the upper (low pressure) tap of dPR-2001 . In a homogeneously fluidized bed, no density gradients should exist. All points on a pressure-head plot, such as shown in Figure 5-5, should fall along straight lines. (The vertical axis of Figure 5-5 is the pressure difference between the gas space over the bed and a point in the bed. The horizontal axis is the elevation of that point above the top of the bottom cone in the gasifier.) As shown in Figure 5-5, the data contained in Table 5-4 all fall along nearly parallel straight lines except point 5, the pressure head at the bottom of the boot. The high boot pressure is due to the lack of consideration given to the solids in the cone section. In constructing Figure 5-5, thermal expansion of the pressure probe and the gasifier was neglected. The data correlated well. Had expansion been considered, points 2 and 4 would have moved closer to the ordinate. During the fluidization tests, the bed expansion was much less than expected. Figure 5-8 shows the predicted bed densities for half- calcined dolomite as a function of particle diameter and gas superficial velocity. The average particle diameter for material circulated during the first tests was 0.055 inch. Plotting the density obtained for the 30,000 SCFH case on Figure 5-9 indicates a particle diameter of 0.057 inch. Here, agreement is good between predicted and observed bed den- sities. However, the bed density should have dropped to 36.5 LB/CU FT at a superficial gas velocity of 2.51 FT/SEC. The actual calculated density was 63.0 LB/CU FT. The discrepancy may be due to the manner in which the fluid bed expansion was measured. In developing the Consol bed density correla- tion, visual averaging of the maximum bed heights observed in a glass model was used to determine bed expansion. By using this bed height to calculate volume, and the known weight of solids, the bed density was calculated. In a smoothly fluidized bed, with no bubble formation or slugging, this calculated density should be correct. If bubble form- ation occurs, the amount of material (both gas and solids) in a given volume will vary. Because of localized differences in density, the average pressure "seen" by the pressure recorders may be equivalent to the pressure head due to solids alone. Therefore, the density calcu- lated by differential pressure measurement may be higher than the ex- panded bed density. 55 2.5.4 Results of Second Gasifier Test Because of the loss of the char-dolomite interface, only char bed expansion was studied in the second gasifier tests. The results of these tests are shown in Table 5-7 and Figures 5-6 and 5-7. The data show that all gasifier temperatures increased with gas rate regardless of the gas entry point (at transition section or at boot) . The increase in boot temperature with increased side flow may be attributed to good back mixing. The change in bed density for the gas flows considered was less than expected. As shown in Figure 5-8, the predicted char bed densities for several of the gas rates are: Gas Velocity, FT/SEC Bed Density, LB/CU FT 0.360 33 0.615 27 2.069 10 However, the actual measured density remained near the char bulk density, No positive conclusions can be drawn concerning gas flow distri- bution via side or boot flow. For the cases in which point of entry was varied while the total flow remained constant, the density change is random. The increase in boot density with fluidizing gas rate may have resulted from a stripping action. At the high gas rates, the fine material in the boot was probably carried up into the gasifier char bed.. This might have allowed denser material to again segregate and collect in the boot section. The high transition section pressure drop, (often exceeding the range of dPR-2001) , indicates that the material in that section was not fluidized. After the tests were completed, the 50-inch range for dPR- 2001 was reset to 100 inches. This allowed measurement of the pressure drop. A 77 LB/CU FT bed density was calculated for the material in the transition section. Apparently, the dolomite which the char had dis- placed during the first char addition had collected and formed a plug. As the transition section pressure drop increased, the reading for dPR-2070 decreased. Since no leak was found in the common tap of dPR-2001 and dPR-2070, this may indicate (1) that channeling was occurr- ing or (2) that dPR-2070 was actually measuring the expanded density. The disparity between dPR-2031 and dPR-2070, which cover a common bed section, might be due to the difference in tap configuration (inline versus opposed) . 56 2.5.5 Regenerator Tests Two regenerator fluidization tests were conducted. The first one provided information on the maximum bed expansion at the highest gas rates available. During these tests, the regenerator actually shook, indicating a violently fluidized bed. The second tests were conducted to define the bed operation at gas rates that were to be used during the first char burning attempt. The data and results for these tests are shown in Tables 5-8 and 5-9 and in Figure 5-9. The following information was obtained from the tests: (1) The general trend was to lower bed densities with increased gas rate. However, the reduction in density was much less than expected. (2) For the same gas rates, the regenerator-dolomite bed den- sities were always higher than those obtained in the gas- ifier. This has not been explained, but may be due to the tap configuration of dPR-2018 or to gas bypassing into the refractory. (3) The recorder swing expanded with increased gas rate. Again, large bubble collapse is probably related to the recorder operation. 2.5.6 Proposed Future Tests The results of Run 5 clearly demonstrate that additional fluid- ization tests are needed to interpret the differential pressure recorder readings. Until this is done, any further operation of the gasifier- regenerator system would be pointless. Atmospheric fluidization tests for both the gasifier and a 12-inch glass model, followed by tests at pressure in the gasifier, have been proposed. These tests should help explain such questions as: (1) How does recorder activity relate to incipient fluidization, bubbling bed fluidization, slugging, and spouting? (2) Do the differential pressure recorders always indicate densities higher than the expanded bed density? (3) Should the average differential pressure reading be used to determine density or should a lower reading based on recorder swing be used? (4) Does pressure tap configuration make a difference in density measurement? (5) Did spouting, slugging, or large bubble formation cause the loss of the char-dolomite interface? 57 (6) What conditions are necessary to achieve interface oper- tion? (7) Why were the gasifier and the regenerator lower bed pres- sures always higher than expected? 58 o o 00 o o o so o o o o CN o r^ o 1 CN en o CM o ■«!r- o o CM CM - H l-H CO 2: w Q H O O CQ Di W HH (i, KH < C3 I LO 3 •H a. o o vO o o St e'i/*n-AxisNaa aaa 59 1800r Char Transfer Started 1235 Char Transfer Interrrupted 1310-13A5 12001 ^e o u CO o 1200 1400 1600 TIME October 27, 1972 1800 2000 Figure 5-2. CHAR BURNING, OCTOBER 27, 1972 60 1800 1200 80 M OT P70 M PQ M PQ 60 3.0 2.0 jmo TIME October 28, 1972 Figure 5-3. CHAR BURNING, OCTOBER 28, 1972 61 lL/\l/^\ o O o o CM o X to M X a fd g cn CO H Z u Ed Cm W u z o I— ( < 3 E- OS a: O u< Q cc o u w u a. o Q PJ Di CO CO w Oi a, o o 03 w I— I tu I— I CO < I LO u •H 000 'oc ooo'^e 000' ig HiOS *M01J SVO 000*0^ 62 — fMlllffffiltlllfll^ H - - + " - - - - ; - ; _- - $ - - - ill 1 1 m tli f Ttt - ++-H- tt-rt i-ti-* -H^ -n+*- +m- ■t-i-t-<- tt+t 1-M-r - ^i^M^^^^i;:;±|:±±!!i$±!;i!!;|;;|!i:!;^^ \\\ T\ T' tn i ' 1 n^^ iMii 1 [i ''1 1 ^::: + ;::r:4::::+::;T:::t:::::;::x: :::-::■ --'J r -irS ' ± t ^.--± X-.t ■.t:::::*: :i\iMzz::z±i:::::\\z:::it-:::::::t:: ::::::::::£::::::: ::::::|:-4:::|: ::::: t::: :;:::::::::::::::::::::i::::::::::|:::x::::;l^::-l: : ;[ t ; || ::|::::i ::g:±::±::;:;;;: MMI||lnl|| -X --X — — X-- -XX-f. 4--1- --L j_, , _x I. ■ ::;::;::::::::::"■ ^--- j^-^_ _ _. liMiiiMiW |[|lilllll[flllilllilllllll!llilllll 1 J^^i^l^^^^^^^^^^^^ lll{}}|{ill^ll^lllf{ltilli{||||i 1 nl - ~- — 1 .. -gK. _. , - - IP 1 Ml i iiiliiiM + ■< — f -- ■ 1 ■ -H — r»--r +'-r + Mf ' 1 IP^*^^ 1 1 11 '1 11 ti flttti N rtiW4l IBli|!iii[i|l :|::::i:::|::|:::::::|::::|i :::::::::-:::::-:::::::::::::::::::;:::::::::::::::::: :::::"■" :::5::::-;::E: ::::::: + :::::::::::::::::: ills:::: ;;:?!;:::-::::::::":::::::::::: ::::::::::::: ICTiMiiWipliii M :;;;;;;;|;;;;;Sji;:;:;|l;;::;|;;;|;;;3|;= ;;::;;|;;|;i:-;:|;|-|::::rHp;f :::::::|:::::::::::::::::|::::::::::::::::::::::.::: iB^H^WffiiliWMMIM liiiiHlBii^^ MgiiiiiiiiiiiiiiiiiiiijIBMillBMii ■*::::|;:::::::::::::::;-::;!:;;::!: ::::::!:::;: :::::::g::::::::::|::::j::t:::-::: |>. :;::::::: 4tl flm 1 Ml Btf Wa^^^^^^^ w^ fttfflflffllM 1 IIIIII nTiim lillff 1 Pi^^^^B^H^^^^^w :;;;::::::::::::-:::|:::::::|::-|;i-:::::-::- lll!illiillMrLUjJ4ti-lillliilllili|llillt4>ffl fiflff Figure 5-5. BED PRESSURE DUE TO SOLIDS (First Gasifier Bed Expansion Test) 63 C3 o en M Q 50 45 40 35 30 -«uir K" Top-Boot torn Boot Middle Ma n Bed Main Broader Span Bed o H 1300 120 1100 1000 u CO H I H M U s CO 2.0 1.5 1.0 0.5 0.0 TOTAL GAS FLOW MSCFH Figure 5-6. GASIFIER FLOW TEST: SIDE FLOW CONSTANT AT 20 MSCFH BOOT FLOW VARIABLE AT 20 TO 45 MSCFH 64 O I C3 H 50 45 40 35 30 1300 12001 1100 TOP-BOOT E ottom Boo : -^-^iddle Mainbed Main Bed r Span Broadei 1000 Bottom M linbed i 1 ^ Boot Jed __ J Bed Middl Top-Abo /e Bed u M CO H r H M O U u CO 1.5 1.0 0.5 0.0 — tiain Bed 4 5 60 7C TOTAL GAS FLOW MSCFH Figure 5-7. GASIFIER FLOW TEST: BOOT FLOW CONSTANT AT 20 MSCFH, SIDE FLOW VARIABLE AT 20 TO 40 MSCFH 65 66 H o PQ I I:: M CO o I H 80 75 70 65 60 1300 •v. 1200 1100 100(> o M CO H fa I >^ H M s M M CO 2.0 1.5 1.0 0.5 O.Ql 90 100 110 121 130 140 TCTAL GAS FLOW MSCFH 67 150 TE PROBL O TE-2033 CALCINED OOLOM\TE IW '^rU fypTy. L- UX StDt U mcu SIDE. MAX. CHAR BE.C5 MElGWr KIM. CU&R BED UEiGUT CMAR OUT TE-2032»K -TL-2035 -Tt-2D3T ^TEl- 2039 ^^— TD eOTTOM OF TE. PROe>t DOU3MITE TO A DOLOMITE TO UDOLMOPPER EM&A6ER POT GAS IKi Figure 5-10. GASIFIER dPT AND TE LOCATIONS 68 en CQ -V a c <0 u o z > •■-I , H c o c a »-( z o a o r-. CtO ^ 00 CO o O (0 • o 00 ^ (N CO CM CO CM CM vO O r^ O • (Nl .—1 O r^ o in in o ■X) • in r-l 00 1 ■4- lO 1 r^ 00 , (V) —t cr- m ■•O sO m vO O vO <3- O • • • • • • • • • • 1 (N ro .—1 tv) o . '-i TJ uu r- O r^ u-1 0^ O o- • • • • • • <1- • . • • f^ o r-» o I— 1 o CO fO - 00 00 • ■ • • • • • • « • CO 4^ c OJ r-l f-l >^N o a ^-N to CO 01 •r^ o- b o <0 O ^ 0) o CO o o •r^ u. to u O CM P •M • • J3 '^-^ CM g o U j^ 3 ^— ' 1 Q > r— 1 ^-•N o o CO OJ > M c; o QQ m o 4-1 Ki •H IM hJ Q > a (/) e (U • •T3 -o 01 r^ 01 f— 1 .—1 CM CM CM •H .o 4J o ^^ QJ 1 1 1 1 o J 1 1 1 1 1 g CO •H CM a fc o o o o a (0 O O o O o c5 V4 Fl -H .—1 f— 1 »— 1 f— 1 r— 1 •—1 ^^ >, > > •H 1 > > > > > 4J Q + ^ o <: < < ■< O Q < <: <: < ■< c C3 U-l o a <0 a U Q. CO ^ (0 < N^ U w o o o CM T Oi to + )-! •d CO CO O CO 4J CM • 1 c t— 1 r-l o < II ^ O 00 r-l X • • 1 cc CO en f— 1 .-4 CM o • « • CO o CM CO CM o o \0 1^ • CO in in CO ■—1 o — 1 o o in CO • a O H 4J a Oi •H M TJ Od ^3 Q (U o 0^ f-4 4J to 01 O •r-l u b Q ^ o 4J 0) T3 4-1 (i3 4J Q^ •— ( >i c o T3 QJ c ■u -l o • 1—1 f— 1 • • eg 1— t o in • • 00 <3- • 1— 1 00 • .—1 • vO .-4 in 2 • 00 —1 00 CO f— ( • CM 1—4 • in 1— 1 o in • • 00 • ,—1 o • in o • in 00 • o * • 00 in • o CM CO • 1-4 vO O O a; -d- • 1 1 CM 1— 1 • (M o o o CM O tn o CM 03 Z o 2 O a .O 0) ■-] 4-) 3 V. CO -4 3 01 CO •U X > W to o w a a E bC M^J g^ OSCN Ct,C cv I C C a m ►J < u I— I H < LO <-{ H 70 O O o o o lO in CO vO v£> O ,—t o r^ in 1— 1 CM o o o a- r-4 o 1—1 r-l CN O CM O o in in in r— 1 1—1 1—1 r-l o o O o O CO CM 00 00 o in o r~~ in CN • 9 • o^ 1—1 r— 1 o 00 0^ O o o^ •— 1 v£> r— 1 CM 1—1 1—1 .-4 CNI O CN o m o in vO in .— 1 1-4 1— 1 r^ m O o o o CO >* ^A o CM CSI r-l r-l 1—1 O CM O in O r- r^ vO r-l 1—1 r-l 1—1 o O O O >* CM .-1 00 CO >3- >J o 00 O 00 • • • 00 in fN CN r-4 1—1 f— 1 CO o CN o in o r^ r~ \£> 1—4 1-4 1-4 1—1 o o o o c^ a> CM CM O CN O o o CO CO • • • ■J- -3- CN CN li-l o f— 1 1— 1 o c^ CO CN CM 1—1 1—1 ^^ CO o CN O m o r^ vO vO 1—1 ^^ 1—1 1—1 CO bO C ir> o O o a^ <»• r^ OS CN 00 CO •o 1— 1 o CO CO • • • o in -J- o CO <3- o -^ i-< ^^ ' — ' CO (A 1 1 1 •H O 1 OQ 1 1 4J B TJ •H U* O T3 H O o Q G Q CO o o CO a O •o Q. 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O CM to lo in in o in CM in in in in 00 t^ in CM to Tt Tl- ^ o in in o i^ in i-t \o in to CM to to to to O to O O CM Tf ■<* in to i-H CM CM ■'^ ^ Tj- o o to in in LO rt to (TV t-- CM CM tT to to o CN in r-» CM in to in rr to CM CM CM CM CM a: X PU u. u. u. o o o o o o in o in in 00 O O 00 LO to • • CM vO i-H ^ '* 1-t CM •> •« •> r^ •> I — ^ (M O 04 i-i 00 r-~ to CN to o o in o LO CM o o o 00 in to • • CM \D i-H ^ •^ o to « ,> « t^ •> r^ CM O O^ <-i 00 r^ to CM to O O LO O LO o> ■^ O O 00 LO to • • CM vO i-H Tt rt 00 CM •»•*•» t^ * >0 CM O O) rH 00 h>- to CN to o o LO o in *o 00 O O 00 LO to • • CN \0 i-H • i-H 00 r>» to CN to o o in o in LO t^ O O 00 LO to • • CN vO i-H Tt Tj- ^ CN * " •> r^ •> t*» CN O Oi ft 00 r^ to CN to O O LO O LO to to o o 00 in to • • CN »0 i-l Tf Tj- 00 CN • •> •> t^ •> \0 CN a o^ I-t 00 r- to CN to to X X X ac X H •p u. u. cju u. UL u. a> u u u u u -"^ 0) CO en CO en to *: u- LO o o CM o r^ LO A i-t O CN I in re o CN o in LO A ft LO LO CT> LO r^ t^ LO + 'in • ^ r-t CN 00 I— • O i-H rH • rf SO CN LO o o CN h^ r- in + in LO so ^ •-• •-• LO CM O CN O C7i LO A LO CN A SO O O to to O CM I o CN + CN LO o I LO r»« in in + LO I • ^ • o i-H I O i-l 00 so i-H CM in LO + • 00 in o so ^ i-H in CM LO CN LO CM O LO • A ft <<* LO CN in CN O ^ • A rt CN CNO O O U U "-I en f> o. o a» CN i^ r>. o LO LO LO so ^ ft f* + ft ft ft ft ft CN 00 LO O + m I CN t^ I so Tj- • o C CN t-i X o o e) cj »— t t— I (— t t-H HH CO cn cn CO cn pL, Ol, Ol. Ol, Cl in ^0 00 • cu KJ CO t-t — en H a. tL. CN CM w CQ O H U O Q 2 O M tn CQ g U u I LO CD ft •S H B "M a, en s (U ♦J H o c a o 0) 0) M u 3 3 •*-> +J u u (U "O O -H 4> u CTJ Hi Oi o ♦-> CO / — 1 « f( c o 0) CM u to E O di 4-> (1> c •H O Cd -H H U J CN to o CN I CJ OC tU CN ^—^ I u ft n. O ^-' X C» ^1 « -H OS < c c •H .H •-} >-] >-i u •H ^H LO I-H O CM I U c o •H ft 4-> t/) <4-l C« •H C3 •-H CO 4-> X o X 4-) 4-> •H X (/) bO C -H a> 4) Q X 4) O CQ CO 0) 0) C C 00 bo V 4) o: a: 10 o o u trt CO (0 ft CN o o o o CN bOfi C rt •H > CO (h '-N O cO O -3 X O U o a> to > I ft ^S3 o > CNO o o u s V) V) o (-1 u u < CM CO O X Ou u u < so to trt o ^ CM O I (/) q: 4> Ou > ^ c 4> CN OJ O » O 4-) CN 0) I CQ 3 (/) to 0) >-l o 4-> CO iH 4> c o bO a: u 4> bO CO ^ bO CO C X 4J +J -H « o o ft 3 O c en f-" t-t 0) . > 4) 6 ^ * O ctt O U -H H O 4) -H X f< ^t^ O O ^t C X « 3 tu 3 cyoc en 73 o to OO i/> OOOOOrsiKi t^cg ^ oor^LOfN'. tot^ r^ (Ntoi— tTttor^o o vo to r^ t^ t-H to CM to o LO o LO r^ lO to lO to ->r^«LO(N a \D <-t r- 1^ rH to (N 00 C7» lO o LO r-- CT> ^^ LO to i—t vO . (N * rsi o to 00 Ort t^ OOOOOi-HI^ T^Tr-l lO OOtOLOOO-' to\o r- cMLoorri-irHO O VO i-t LO r>* i-H to , (N LO (N LO O LO r^ LO c^ r-- tf) o> 1^ LO h- to r^ LO • VO £> + T}- LO LO Tt CM rg CM tM o o o LO o o LO to LO to to O to en to CN (N O lO (N to o en O (N OQ 00 rt CM (N OJ CM to LO 00 to o o 1-H OQ O •-• o O 00 >* 00 to to a. O LO w \0 CM 1-3 CM (N CL, O U O o to a CM o vO (N OJ to ^^ CM CM I CM CM 1-H f-i •— ' •— • Lu 3 tu (L, o o o o O LO O O LO f-H O O CM to LO O • • (N 1— I to »* 1-H '^ CM • •> •» r~- •> r-» (N o o^ o r~- h~ to CM to O lO LO O O vO to o r^ 00 LO r-t • . CN 1-H 1-H TJ- O r^ 1-H * •> « t^ * vO (N O O^ 1-H 00 1^ to CM to O LO lO O O (N rj- o r^ 00 lo 1-H • • CN 1-H 1-H ^ O O 1-H n • • r^ * r>. (N o o^ 1-H 00 r^ to a> o o 00 LO to • • CN \0 1-H rf Tj- 00 o O O 1-H 00 r^ to CM to 1— t to X X X a: 3C H +-> u. tu u. (ju u. b a> U U U U U -^ Oi CO CO to C/5 to ^ u. LO vO vO to o • \0 • • C7^ CM O 1-H LO Tt . O • LO A O rsi I lO ^ (N • O ' \0 + CN f-H A 1-H LO r^ o^ CT> LO to 00 + rt LO LO • CM O 1-H f-H f-H LO 1-H • rt CM to r^ o^ LO LO to o + TT LO • • • f-H r-t rH r^ LO 1-H lO Tt CM (N CM TJ- CM 'i- t^ o lo r^ LO CM O • (N LO + + Tt LO • Tt • rH 1-H 1-H »— 1 O r-l ^ \0 CM CN LO Tf CN o LO h- cn O^ LO vO o O e>P Q- t-H X ^ r^ LO LO r^ LO t^ + Ti- . . •«a- • o^ •-H r^ o 1-H r^ LO vO CM 1-H u w cj cj c:) o tj CO t-H l-H l-H hH I— 1 hH ^v^ CO CO CO CO CO CO H a. CL (X a. a. a, u. •H CO 00 CN Oi w CO o E- u o i o 1-H CO CQ o u < X u LO I LO cc CO a> o ctJ a, &, u E OQ CQ (U H c o O i-H ■M -O _ O -iH u 00 3: u o Rj /— 0) 1-H c o a> (N O "^ to O 4-* t- 9i 5 C T3 O -H 4) rH J CQ U. Oi Ifl «4H O Cd -H H U J CM to o — ' O M «) -H OS < c c •H -H •H -H < < lO 1-H O (N I u OS u. c o ■H 1-H .-} U. •M to «+H (« •H C5 1-H M Rj n) 4-> fC o U H +-» 4-» •H jr (/) bO Q X 73 "O 0) (U OQ OQ U U O O *J ♦-• rt rt 0) 0) C C a> t»0 bo a> a; OS OS w o a. £ o u t/> / — \ / — > rt 1-1 CM C3 O O O O TJ CM CM <:i I I 0) OS OS fC <: 5 > CMO o o u bO c •H T3 (A O > 05 rt «5 > V ' (1 CMrt X u u a; > 1-H > u a fC u V) o o < a. < v> > / — ' C O I 0) tf) fH ^H (fl 0. a. o a; 4J ex _ o 4-> a. 0) rt c >H ^ -H 0) a; i-j C bo 0) rt ^ bo bo rt OCX OS cu u &, 3 X • +-» E +-•+-> -H M ii U S u a Qi 0) g 1-H 2 sort « U -H E- -H X -< <4H fH C X 4) 0) fX 5 3 O-OS CO 74 tNI r-- O O O in o lo \o ^<^ m O O O t^ CO CO o CM CM ^ O O O O CO vO 00 00 3- «N CM •« 0^ ff^ • • • • • • • •^ v^ w^ •> • \ O O 00 CO CM O CO — 1 CO 00 00 r-4 r-l f— t r-4 .— 1 O CO — 1 ^ <» CO CO CM NO vO OI - . o o o O in o "o •^m o o o — ^ ^a- UO .— 1 CM CM ^ o o o O »n O CO O CO »-^ CO CM .— t i-* xO CM ^ «^ A A • • • • • • • •^ Vk »k «t • ^^ o >3- CO CM CM r^ CO ^^ — < r- ^ ^^ F-l f-< 1— 1 •— 1 o CO r-i «n CO CO CO CM vO sO P3 - o o o o o o m "V. 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X o O 1 o ^-> CM » • £ B 4J 4J 4-> 0) ^ y •M CM 1 o Ol, o s . • H -. 5 QC to u —4 s E- H u* (/) 0) -H 4> U. D o oc u. 0) E c; •H I-l .-J 1-H * — ' I-H CM tu H B 0) a> 4) a> U 1 ^—^ 1-H (4 o o 4-) 1-H H Q X E O <4H 0) -H a: -J o c (U -H OS r-t a; OS V ' u •H < 4-> o c o u 4-» o CO •H ft o 73 a; OQ 73 0) 03 0) •M CO to to u CO C3k I LO .CI E- OQ cd o X •H 4J «4H -H ^ U (U O U,r-t 3 78 RUN 6 DECEMBER 1972 AND JANUARY 1973 FLUIDIZATION TESTS GLASS MODEL AND PLANT GASIFIER CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 79 FOREWORD In previous runs, the principal process (as opposed to mechani- cal) problem was the establishment of suitable fluidized beds, in par- ticular the establishment and maintenance of separate acceptor and char beds in the gasifier with an identifiable interface. There was almost certainly a discrepancy between actual fluid bed conditions and apparent fluid bed conditions determined by relating measured variables, especially differential pressures, to measurements and observations made earlier in the Library pilot facility. Run 6 was designed specifically to obtain data such that actual fluidization conditions in an operating plant could be predicted, ob- tained, and maintained through nonvisual measurement and observation. The fluidization tests were in three major sections: (1) tests in a glass model, at atmospheric conditions, with visual observation; (2) tests in the plant gasifier, with limited visual observation, also at atmospheric conditions; and (3) tests in the plant gasifier at normal operating pressure with temperatures and other variables approaching normal operating conditions. This run did not interfere in any major way with other programs, because the plant was shut down for a prolonged period for replacement of the regenerator insulation that failed toward the end of Run 5. 80 1 SUMMARY In December, 1972, an extensive series of atmospheric-condition fluidization tests was run in the 12- inch-diameter glass model and in the plant gasifier. Acceptor fluidization, using 6X9 mesh and 6 X 16 mesh South Dakota Minnekahta limestone, was tested in both vessels. Fluidization of 20 X 65 Husky char in the 12-inch glass model was test- ed. Fluidization of stone in a 4-inch-diameter boot on the glass model, with a 12- inch-diameter char bed of 20 X 65 mesh Husky char above the stone bed, followed by showering various sizes of stone down through the char bed into the boot, was tested in the model only. Pour gas-inlet configurations were tested on the model, two on the plant gasifier. Several bed depths were tested. Differential pressures between differ- ent bed elevations were measured at the center of the bed, the peri- phery, and intermediate points. Actual bed densities in the model were determined by volumetric measurement. Experiments in the glass model demonstrated that: (1) Differential pressure measurements between elevations in either stone or char beds do not accurately measure bed density. (2) The point of incipient fluidization of a bed can be recog- nized by careful observation of differential pressure measurements. (3) For moderately to highly expanded beds, the correlation of Library pilot data that relate gas and solids properties, superficial gas velocity, and bed density, provides reason- ably accurate predictions of bed densities with the equip- ment and broader range particle-size distribution used at Rapid City. The correlation does not predict the incipient fluidization point. (4) Acceptor, in size ranges from 6X9 mesh to 20 X 35 mesh, will readily shower through 20 X 65 char if: (a) The char bed is moderately expanded, and (b) The acceptor bed in the boot is near the incipient fluidization point. (5) Pressure gradients across the bed, horizontally, do not ■ normally exist. 81 (6) Qualitatively, a vertical gas sparger pipe protruding into the bottom of the boot, dead-ended at the top with hori- zontal outlet holes near the top, gives better fluidization and IS easier to control than a simple connection, with or without an inlet screen. Atmospheric tests with limestone only in the plant gasifier Z^^y^'A''" \^fS^^ '''^^^> conclusions reached in the glass model. When 6 X 16 mesh limestone was fluidized, the differential pressure increased, peaked at incipient fluidization, then decreased, with in- creasing gas velocity. For these tests, direct visual observation was precluded by clouds of dust over the bed surface; video pictures were ulTt M^'"^'\\' I i^ '""^ '^''" ^°^"^^^' by 1°^^^^"^ ^ ^a">era and light close to the bed surface. A tape of these pictures, with approp- v.t?nn f ° ^™e"tary is available at Rapid City. One vital obser- vation from this test is that the "swing- or "oscillation" of differ- of bed ?nnH ';'''" recorded by the instrument pen is an excellent indicator of bed condition A wide swing indicates a moderate to highly fluidized bed a narrow swing indicates an incipiently fluidized bed Previously a narrow swing had been interpreted as a slumped bed. viousiy, t>,. 1 During January 1973, additional fluidization tests were run in the plant gasifier. The vessel was isolated from other systems and 7aZoI ^^ """^^^ pressure of 150 PSIG at temperatures in the 1000 to 1450OF range using inert gas as the fluidizing medium. Limestone was charged to the boot and fluidized. A bed of char was establisherover tatnL ?"''/'''/" identifiable interface. An interface was main! T.l.r. fr P^°l°"?^d periods. With experience, it was possible to detect the beginnings of interface dissolution and, by adjusting flows and exercising patience, to recover a clearly defined interface In the recovered °" '""^' ' '°''''^ disrupted interface could not be the char'bef °rLovL'f^''^'l'\'^" '°P °^ '^" gasifier, showered through the char bed, removed from the bottom of the boot, and recharged to the top of the gasifier. This cycle was repeated several times. During the last two days of the run, steam was added to the till ' JV''^''^^^ ""^ ^""^ ^^^ "^^^"^ addition system and technique Methane, hydrogen, and carbon monoxide were produced briefly during'this experiment. Non-steady- state data on gas flows, bed temperatures fnd overhead_gas compositions during the steam-addition perLdf are ^hown in Extremely valuable fluidization data, much of it aualitativp were obtained during Run 6. This has led t^ high confidencein achiev ing a successful gasification run in the near future. Many of the tests in Run 6 were repeated several time^ ti..-c done in part to test reproducibility of result. Zt ti ^^ • " ""^^ four operating shifts an opportunity to obs'^rve'the re uUrand"' "'' practical experience with cause-and^effect dyn^^r^r^oiL^Tf ItT 82 2 DISCUSSION Fluidization tests were conducted in several parts. Some mod- ifications were made, based on experience gained, and a final experiment involving addition of steam to a hot, pressurized gasifier was added at the end of the run. 2.1 GLASS MODEL FLUIDIZATION EXPERIMENTS 2.1.1 Equipment and Materials The existing glass model in the lignite preparation structure was modified for these experiments. The equipment is shown in Figures 6-2 and 6-3. It consisted basically of a 12-inch-diameter pyrex glass vessel. A four- inch-diameter glass "boot" on the bottom of the vessel was used for tests involving both char and limestone. A vertical probe of two concentric tubes provided pressure sensing points spaced 12 inches apart vertically; the probe could be raised and lowered vert- ically and could also be moved horizontally from one side of the vessel to the other. These pressure taps, together with taps below and above the equipment, provided for measurement of differential pressure over the bottom section of the bed up to the bottom probe, over a 12-inch section in the bed, and over the top section of bed above the upper probe. Mercury- and oil-filled manometers were used for measuring differential pressure. Air, with a supply pressure of 150 PSIG, was used as fluidizing gas. Four gas inlets were used, three conical inlets with 1-, 2-, and 3-inch inlet pipes, and a 2-inch inlet sparger. The conical inlet with 3-inch inlet pipe has a support screen. Details of inlets are shown in Figure 6-2. Two sizes of Minnekahta limestone were used for fluidization tests, 6X9 mesh and 6 X 16 mesh. Finer material was used in some showering tests. Husky char, 20 X 65 mesh, was used. Typical screen analyses are given in Tables 6-1 and 6-2. 2.1.2 Limestone Fluidization Tests The tests were conducted in the 12-inch glass model with no boot section. Weighed amounts of limestone giving settled bed heights of approximately 12, 24, and 36 inches were tested. The four gas inlets shown in Figure 6-2 were used. Two sizes of limestone were tested. 83 .t.. ■ atmospheric temperature and pressure, air flow was increased stepwise and data taken at each step. Major data recorded were: bed heights (inches) gas rates and temperature, ambient pressure and differ- ential pressures (probe at wall, center, and intermediate points) mesh size m bed, gas inlet in use, qualitative description of bed condiUon Quantitative Results h.A A ^^!"''^^ ^~i ^"^ ^"^ ^""^ P^°t^ °^ ^^^^ ^^ Tables 6-3 and 6-4 showing bed density as a function of superficial velocity; for comparison p!o?s are shown of predicted densities based on correlation of earl e^da^a in the Libraiy facility. At higher velocities, with moderate to high fluiSi zation, there is good agreement between actual and predicted densities Data entiafpre's'ure ri^elT '' T'' ^^-tuations i^ bed height a^d differ-'' ential pressure. The wider scatter of 6 X 9 mesh data, compared to 6 X 16 data, may be because several observers recorded 6 X 9 iata knd a single observer recorded most of the 6 X 16 data. single nf A-J^^^'l^ ^^ ^^^^ ^^^^^' ^-^ ^"^ ^-4 ^°^ dat^) shows the insensitivitv ?n.fi r^i'^^P'"'""''" measurements to gas velocity above the point of ^ incipient fluidization. This is due to the nature of the fluidization be- havior for the system under study. The fluidized acceptor and char beds maintained m the Rapid City pilot plant vessels can be visualized as blin. and a dense phase which consists of solids particles held slightly apa^t by the passage of small gas streams between particles. As thf superficial 'ZJ'l'T^A^' increased, additional gas bubbles are formed wh I p^h through the dense phase and cause the fluidized bed of solids to ei^d and surge. Under these conditions the pressure drop per unit engS of bed IS nearly constant over a wide range of superficial gas velocities The indicated bed density measured by highly damped pneumatic differential pressure measuring instruments as used in the pilot plant closely corres ponds to the bed density at incipient fluidization. ^ A hump or peak in the differential pressure versus velocity curve TttleTbe^r^ TnZ' ^!;\" a""' r '''''''' ^^ ^-"^ increL'ffroT: p^i^ Xt\i^rcaL^rd ^;tairt:^:t^:f^?tVcie?-A\.p ?;i?tuidiz:rb:dirrsitt?:s iT''^ - ^-- --^- -- -- ' ' tally ac?os^^?h/h^^ TJ" l^'"^^ °"^ ^^ow some pressure gradient horizon- tally across the bed; data for 6 X 16 mesh stone do not show this gradient Differences detected were not significant. gradient. Qualitative Results The sparger was the best gas inlet dpvir^ tk« • ,. mlet was the worst. device. The cone with a 1-inch 84 Differential pressure fluctuations are considerably greater above the point of incipient fluidization than below. A change in degree of fluctuation of differential pressure is the best detector of the point of incipient fluidization (barring visual observation of the bed itself) . Spouting (the formation of a high velocity stream of solids and gas through the fluidized bed) is accelerated by: (1) low ratio of bed height to diameter, (2) high local velocity, such as was caused by the use of the 1-inch-diameter gas inlet, and (3) narrow particle-size distribution. Surging of the fluidized bed is accelerated by: (1) high gas rates, and (2) wide particle-size distribution. 2.1.3 Char Fluidization Tests The char fluidization tests in the glass model were essentially the same as the limestone tests. Figure 6-7 shows bed density as a function of superficial velocity (see Table 6-5 for data) . Again, predictions based on analysis of Library experimental data are shown for comparison. Figure 6-8 shows differential pressure as a function of si^erficial velocity. Incipient fluidization is clearly shown by a peak in the curve. As in the acceptor tests, the differential pressures do not indicate the bed density that would be obtained by dividing the weight of solids in the bed by the bed volume. The conclusions from the char fluidization tests are the same as those for the limestone tests. 2.1.4 Showering and Circulation Tests The 4-inch diameter boot was added to the bottom of the glass model as shown in Figure 6-3. An inventory of limestone was established in the boot and gas flow was established to obtain incipient fluidization. Char was added from the top to fill the top of the boot and a portion of the 12-inch-diameter tube. An interface between the limestone and char beds was established. Limestone of four different sizes (6 X 9, 6 X 16, 9 X 20, and 20 X 35 mesh) was showered down through the char bed into the boot. Limestone was removed from the boot periodically to maintain inter- face level. All four sizes of limestone showered successfully, but with differ- ent degrees of ease. The 20 X 35 mesh material was most difficult to shower. Test repeatability was poor; at a given gas velocity, a particular size 85 stone would shower easily one time, with difficulty another time. In par- ticular, if boot velocity is lowered to allow for the smaller size stone, side gas flow must be increased to compensate and provide sufficient flui- dization in the upper bed. The composition and condition of the material m the transition section between the 4-inch boot and the 12-inch main sec- tion seemed to be the key factor affecting the showering. On occasion the interface between the limestone and char beds was lost. However, recovery of the interface was easily accomplished The key to recovery was reducing the boot velocity until tlie material in the boot was barely mobile. Acceptor would then gradually separate from the char- acceptor mixture reforming the interface. Additional showering tests were conducted using inert gas as the fluidizmg medium. The gas was introduced both in the bottom of the boot and at the transition between the 4-inch and 12-inch sections. Gas velocity m the boot was varied, but gas flow to the transition was varied in the opposite direction to maintain a 0.45 FT/SEC superficial velocity in the 12-inch section. A mixture of 25 percent 20 X 35 mesh and 75 percent 6 X 16 mesh limestone was showered from the top, removed simultaneously from the boot, and carried to the top to maintain a constant circulation ot limestone through the char bed. (See data in Table 6-2.) All acceptor showered. The acceptor showered most readily when boot gas velocity was at the point of incipient fluidization and side flow was sufficient to maintain good fluidization in the upper bed. At higher boot gas velocities, the limestone traveled more slowly through the char bed- less limestone of -28 mesh size was withdrawn from the boot, indicating' a retention of fine limestone in the bed. 2.2 ATNDSPHERIC FLUIDIZATION OF LIMESTONE IN THE PLANT GASIFIER Atmospheric fluidization tests of limestone were conducted in the boot of the plant gasifier (which had been isolated from other parts of the plant) m the latter part of December. The tests were similar to the limestone fluidization tests in the glass model, but at a larger scale and using plant instrumentation. Visual observation of the bed surface from the open top of the gasifier was impossible, even with lights and binoculars, because of the dust of fines over the bed surface A tele vision_ camera and lights were lowered near the surface. This provided a good picture of the bed surface during the tests. A video tape of the pictures, including an audio description of the fluidization conditions has been preserved for the tests with 6 X 16 mesh limestone. 86 2.2.1 Equipment and Material Tests were conducted in the boot of the plant gasifier. Figure 6-9 is a schematic which shows the essential equipment setup. The regular gas inlet was used, and also a vertical dead-end sparger with six 5/8-inch hori- zontal holes near the top. The regenerator air compressor was piped to the gasifier and air was used as the fluidizing medium. Regular plant instru- ments (dPT-2001, 2002, and 2003) were used for differential pressure mea- surements, and manometers were installed to provide backup checking of the plant instruments. The high and low side pressure taps for dPT-2002 were modified to allow movement across the boot cross section. This was done to allow measurement of possible horizontal pressure gradients in the boot. Limestone used was 6X9 Tyler mesh and 6 X 16 Tyler mesh. 2.2.2 Test Procedure Pressure taps in the boot were set at the center of the vessel. Air flow was set for minimum incipient fluidization. Approximately 400 pounds of limestone was charged. Air flow was raised to a maximum for the parti- cular size of limestone, then more stone was added to reach a set bed level. Air flow was reduced stepwise, and at each step more stone was added to maintain the desired level. After the minimum flow for incipient fluidi- zation had been reached, air flow was again raised to the maximum and more limestone added to reach a higher set bed level. Again, flow was reduced stepwise, with addition of stone at each step to maintain the level. At minimum flows, pressure taps were moved to obtain a traverse of differential pressure measurements across the bed. The above procedure was followed for both sizes of limestone and with both air inlet configurations. Data recorded were: differential pressures (both instruments and manometers) , air flow rate (direct instrument reading plus air pressure and temperature) , temperature of overhead air from the gasifier, and limestone weights. 2.2.3 Results Figures 6-10 and 6-11 show bed pressure drops calculated from differ- ential pressure as a function of superficial velocity for the cases in which the bed level was held just above the low side pressure tap of dPT-2002 (see Tables 6-6 and 6-7 for data). Since both the high and low side pressure taps of dPT-2002 were submerged in the boot acceptor bed, the pressure drop per unit length of bed was easily calculated from the dPT-2002 and the middle manometer readings. Comparison of Figures 6-10 and 6-11 shows that 6 X 9 mesh limestone was never raised beyond the incipient fluidization point, while 6 X 16 mesh limestone reached incipient fluidization at a superficial velocity of about 3 to 3.5 feet per second. Remote video observation of the bed surface showed that incipient fluidization coincided with moderate oscil- lation of the differential pressure recorder pens. As in the glass model tests, the bed expansion was independent of the differential pressure mea- surements . 87 Whereas, in the model tests, the sparger gas inlet gave clearly superior results compared to the cone inlets, any superiority of the sparger in the gasifier was hard to identify because of more difficult visual oservation of the bed surface. Quantitative differences between the two gas inlets are more pronounced for 6 X 16 mesh limestone, as seen by comparing Figures 6-10 and 6-11. Differential pressure readings made with the sensors at the middle, the two walls, and halfway between showed no significant differences. 2.3 PLANT GASIFIER TESTS UNDER PRESSURE AND TEMPERATURE From January 8 to 28, tests of fluidization of limestone and char, showering of limestone through a char bed to a limestone bed in the boot, and addition of steam to the beds were conducted in the plant gasifier at an operating pressure of 150 PSIG and at temperatures ranging as high as 1450OF. Figure 6-9 shows the location of the side entering differential pressure taps and instrumentation which were used to monitor the gasifier fluidized beds. Since the system was operated at pressure, the manometers that were connected in parallel with the booths pneumatic differential pres- sure cells were removed. Redundancy in differential pressure measurement was achieved through the use of a vertical pressure probe (not shown in Figure 6-9) . The probe which contained six spaced pressure taps entered the gasifier through the top head and extended axially through the gasifier into the boot section. By measuring differential pressures over the gasi- fier length, the char bed density, the acceptor bed density, and location of the char-acceptor interface were determined. 2.3.1 First Fluidization Test On January 9, with recycle gas heaters set at 1450°F, a limestone bed was established in the boot of the gasifier. On the following day a char bed was established over the limestone bed. A stable interface between the limestone and char beds was maintained for over two days. Showering tests were not possible at this time because a plug developed in the limestone outlet line from the gasifier boot. Back- pressuring the line eventually broke the plug, but, in the process, the interface was destroyed. The char and limestone were so intermixed that prolonged attempts to reestablish the interface by adjusting flows were of no avail. The gasifier was shut down and emptied. During the shutdown, the gas distributor in the boot, a vertical 4-inch deadend pipe with eight 88 5/8-inch holes in the wall near the top, was shortened to 6 inches, bringing the holes a few inches below, rather than above the limestone outlet. It was hoped that this would provide greater bed activity near the outlet, keeping it free, and avoiding plugging. Inspection of the gas inlet tee at the bottom of the gasifier revealed a broken heat shield (which was repaired) and a solid iron- nickel-sulfide deposit similar to deposits found in earlier runs. The heater outlet temperatures were kept lower in subsequent tests (until near the end of the run) in an effort to reduce or eliminate sulfur attack on the hot heater tube walls. 2.3.2 Showering Tests On January 19, with heater outlets set at 1250 F, a limestone bed was again established in the boot, and on the following day a char bed was established over it, with a clearly defined interface. Limestone was successfully showered through the char bed into the limestone bed in the boot from a "shot -pot" that had been installed over the gasifier. The showering test could not be continued because the limestone outlet line again plugged. During the shutdown to empty the gasifier a "rod- out" device was installed on the limestone outlet line, so that plugs could be mechanic- ally broken. This device was used successfully several times during sub- sequent operations. Operation was resumed on January 22, with heater outlets set at 1150°F. Again, a limestone bed was established in the boot, and a char bed established over it. This time (with occasional assistance from the "rod-out" device) , limestone was repeatedly showered through the char bed into the limestone bed in the boot, withdrawn from the boot and lock- hoppered out of the system, carried to the top of the gasifier, lockhoppered into the system, reshowered, and so forth. This demonstrated conclusively the ability to shower uncalcined limestone. All particle sizes showered. There was no evidence of significant attrition of the limestone. 2.3.3 Side Flow Test On January 25, the side flow to the gasifier was varied from approxi- mately 24,000 to 60,000 SCFH. Heater outlets were at 11500F, boot flow was steady at about 34,000 SCFH, and there was no acceptor showering. Conditions at various side flows are shown in Table 6-8. The variation had no significant effect on differential pressures across the beds (or pseudo- density calculated from differential pressure), or on the stability of the interface. 89 2.3.4 Boot Flow Test On January 26, gas flow to the boot was varied from about 35,000 to 40,000 SCFH. Side flow was zero, heater outlets were at llSOOp, and there was no acceptor showering. Conditions at various gas flows to the boot are shown in Table 6-9. Again, there was no appreciable variation in differential pressures, and the interface was stable. Some limestone had to be added to maintain interface level, indicating that a portion of the limestone migrated into the char bed at the higher flows. 2.3.5 Showering at Different Temperatures ^ Showering tests were conducted with heater outlet temperatures of 1150 F (no steam addition), 12500f (with and without steam addition), and at 1350 F and 1450°F with steam addition. At each temperature except 1450°F (when a time limit shortened the test), five batches of limestone were show- ered through and removed, then, after a pause, a sixth batch was showered through and removed. Table 6-10 shows operating conditions during the above tests. Also shown are three typical limestone screen analyses of material fed in, and screen analyses of the final material removed from the boot during the 1150 1250, and 1450°F tests. ' 2.3.6 Limestone Color Limestone removed from the gasifier boot during the 1150°F experiment was lightly colored. Material removed during the 12500F experiment with no steam addition was much darker (black in color). When steam was added at 1250OF the stone was much lighter in color, and at 1350°F even lighter in color. ^ 2.3.7 Steam Addition On the last three days of the fluidization tests, steam was added to the gasifier. This was done to test the mechanics of the steam feed system and toobserve the system response so that any problems or surprises might be anticipated and planned for in Run 7. r- & Figure 6-1 displays a chronological record of key data over a 52-hour period from 1200 hours January 26 to 1600 hours January 28. At the top of T.t fl^T' r^ ^T ^^°^%^^^ ^h^^ted: recycle gas to the boot, recycle gas to the side, and steam flow. At the bottom of the figure, three tempera- tures are charted: recycle gas heater outlet temperature! limestone bc7 temperature m the boot, and char bed temperature. In th; center of the figure, concentrations of various chemical components in the gasifier over head gas (dry basis) are charted on a logarithmic scale. ^^'''^^ °^^^ 90 At approximately 2200 hours (10:00 PM) on January 26, steam was added to the gasifier. Immediately, hydrogen concentration rose from a fraction of a percent to about 10 percent. Methane and carbon monoxide levels rose about 2 to 3 hours later. Because of an improper valve action on the steam supply system, the steam valve went full open for a brief period, destroying the limestone- char interface and otherwise upsetting the system. Steam addition was stopped and flows were adjusted to regain interface. Con- centrations of hydrogen, methane, and carbon monoxide in the cycling gas depleted over a period of several hours. About noon on January 2 7, the interface had been restored and the system was again in a steady condition. Steam was again added. As before, hydrogen concentration immediately rose. This time, however, methane and carbon monoxide concentrations did not rise. Whereas char bed temperature had been about 1150°F at the time of the first steam addition, the bed temp- erature was now only 950 to lOOO^F, which is too low a temperature for carbon monoxide and methane formation. Steam was again shut off between 2200 hours January 27 and 0400 hours January 28 because of an operating upset. As expected, hydrogen concentration fell off during this period. When steam was added again at 0400 hours, hydrogen concentration again rose. At this time, char bed temperature was about 1050 F. Methane concentration rose about two hours after steam addition, but carbon mono- xide concentration did not rise until the char bed temperature had reached about 1150OF. On the afternoon of January 28, shutdown was started and concentrations of hydrogen, methane, and carbon monoxide gradually fell off. Some speculative observations on the steam addition test may be in order. Methane and carbon monoxide concentrations were lower during the final steam addition than during the initial steam addition, despite the bed temperature being the same or higher; this is likely to be because no fresh char had been added and the char was less reactive in the final period. Whenever hydrogen level was high, fractional percentages of hydrogen sulfide appeared in the overhead gas; again, the concentration level was lower toward the end than initially, presumably because no fresh char had been added and available sulfur in the char was less. At 2200 hours on January 2 7, hydrogen level was high; when steam was cut off, there was a brief increase in carbon monoxide concentrations, presumably because of an equilibrium shift when steam was removed. 91 2.3.8 Interface Stability A stable interface was maintained during most of the 150-PSIG tests described above. In all, the interface was lost five times; in each case there was some sudden change in conditions such as back-blowing the lime- stone outlet line to the spent dolomite hopper or a step change in the boot gas flow. As mentioned earlier, the first time the interface was lost attempts to regain it were unsuccessful. On all other occasions the interface was regained in due time. Recovery was achieved by re- ducing boot velocity as low as possible, yet retaining incipient flui- dization, then waiting until the interface was reestablished. 2.3.9 Iron-Nickel -Sulfide Formation As mentioned earlier, after the first brief test with heater outlets at 1450 F, a deposit of iron-nickel-sulfide was found in the inlet gas line to the gasifier boot. Presumably this resulted from sulfur attack on the heater tubes. In subsequent tests, heater outlets were kept 1250°F for two days, then at 1150 F for several days, then during the last two days u ^^^ '''^' ''^^^^^ successively to 1250, 1350, and 1450°F. After final shutdown, no iron-nickel -sulfide deposit was found. During most of the last two days, when heater outlets were over 1250OF, steam was being added and hydrogen concentration was over one percent, for brief periods hydrogen concentration was as high as 10 to 19 percent. It is believed that the presence of steam and hydrogen in the gas inhibits sulfur attack on the hot metal tubes . 92 Figure 6-1. STEAM ADDITION - GASIFIER FLUIDIZATION TEST 93 TIME (UQURS') J^N. It. ms IZOO IWIO ItOO IbOO 0600 Figure 6-1. STEAM ADDITION - GASIFIER FLUIDIZATION TEST 93 cowctwraic DlFrtREWTIiiL 7t'U"CxD.. ,A'I.t>.. -W.* % % ; D TOP Pftoae T lVt"o.o. , STRie>uTog^ Figure 6-2. GLASS MODEL CHAR AND LIMESTONE FLUIDIZATION APPARATUS 94 l^A-ao. cowctMraic Pupae. 1ii"o.D. 1 4" ix:,. iViu" «r 2"S04. 4o «Pt "TOP PftOftE jJVk," ^' y scH. 40 ptpt bJVTRlftUTOR D f^' H 2' •>V Fw , MO€MtNT \ ■- »■ ROD rOQ. uoctiz. Ta^vi.Q.«>e.. x5 CZZ3X1 ^ Miit^PTEB. -■?. 4" 6 6LA*>^ l>4TtC^P^Ct ^ 4 tx ezylL v5,GATE VALVE ^CCtPn-OR OUT ^/ ^LAOCS&O, £: FLOOP. Figure 6-3. EQUIPMENT FOR TESTING SHOWERING OF ACCEPTOR 95 M E- M > o M M M a (-• I U GO ij riD/ai 'AiisNaa aaa 96 w Q O CO o a: u 2 I— < I I— I < W o C/D t: X o ^ > p PL, o z M >- I— t U o > I-H Nl HH Q 1— I PL, C/3 > H t-H C/D Z tu Q Q UJ CO LO 1 li no/ai *AiisNaa 97 -J c o < CJ3 U I a: I— I < O vO c o u o UJ > z I— t M 3 > a, < Q U CO vO s, •r-( 98 o u in H w Q O CO C/3 < ►J a: u z CO < E- Qi a: < u O o z O •-• s o •J '-^ > 2 I— I 3 > CO w Q Q UJ I •H li no/fli 'AiisNsa aaa 99 o g t/5 I CO < < X u CO o o H h-l u o >-] UJ > 2 I— I SJ I— I Q n ►J u. CO > Q QQ 00 I 100 CA^IFltf^ REACTOR TOP HEAP -_,.^_ (MOT TO *>CACE.) I^/^ CALCINE P ACCEPTOP. IhLEf ^ N024LE —>/^ «»uPPOf^T TV CAM£P.A U6NITE FEEP NOZZLE ACCEPTOR LEvet 51DE FLOW 5TtAM (MLET BOTTOM ME FLAN&e. &O0T GA5 IMLET (_me. (SPARGER, GA^ Pi^TRipuroft <7HourO eiPENT ACCEPTOPv ponp uNc 2.'53 1iP.GR- nANonET£P>9 r^;LPvCUP-V MAHOMtTiP, AIR-V* Figure 6-9. SYSTEM SETUP FOR ATMOSPHERIC BOOT FLUIDIZATION TESTS (NOT TO SCALE) 101 UJ z g C/D o tJJ 10 ^^ 1— ( J 00 T- «»• CO NO a> ^ X vO V ■^ o a. CM >- •^ 1— 1 U o o J . u U3 ^ 00 tZ o 2 O H-l 1— 1 ^0 U E- Ul > PS u. ^ M < CO < (N * cu lO O Qi Q o M s ^3 CO 00 CO . LU PM a: a. \o Q w rs CQ I vO (U ^-( 3 DO •H JJOIHH aaa do ni/"d*m ni 'dv aaa 102 o X vO 1— I X vO o u o o H i IX, o PC Q U CO CO w Di ex Q w CQ I — I to o vo r^ «o vo LO i-H CN to i-H LO LO C7> to 00 r-H 00 O to CN to en (Jl ■-« I— ( OtOOLOLOO'^O ■-H CNJ CN •— t I— I viJCN'^CN'-H'-H'— ltO ocNorxi^ooo I— t (N (N >— I CN r-t u o CO C3 U X oi o ti. >- U VO CO z O •J U a: I— I u (U Q VO LO i-H ro •-J < X X t-i H VO o t— 1 CN 2 t-i FT FT/SEC /SQ FT-HR (75% - 1 LO CN V ' Q UJ Z < OQ H •^ J U] CN U ^ r: C/3 Qi ^— '^-^ (— ) 1— < Q CO oVP oa u u UJ > 2 hJ O o OQ J H H-4 J kJ < •s^ ^ Pi 2 ^ PU X X <: X t-i c/j a en < C/3 D tu CO 1— ( f — ^ Q M CO r— ( K-t z U UJ ^ 5 c^ ^ w o. >^ 1 UJ UJ 03 ^ ^ X Q CJ3 O a: 5 •* X _ 2 CC E- tu o w UJ • H s 3 CO Q Q (-1 < O z Qt: z I-] §^ (^ .«:. UJ UJ M CO CQ 1— ( 5 O CO gss >■ H OJ CO Cx CO C/3 H Qa CO a: Qi Qi h-l g ^ CO § w < < < 3 [^[^ Cl, X u 55uf 1— ( 1— 1 ►J M tOOOOOOOOOtOLOLOLOCNLO r^L0"^0^O°000rJ-'^r-("5t- to rsi to Tt to 00 1— I --• CN CN --< .-H '*V0200'*OOOloOOOOOZ r-ti-lfvJCNtO^vOOO^ r— I fN CL, Q UJ z UJ a CO Q U Z ►J < < X u CO z UJ a ►J < z UJ D- X UJ cc o UJ o Uh I 104 < J in X o ^ OS u .^ n: LO to vOg X u. 2 V ' »— 1 o < CM H s H Z U u Di UJ a. w z H o 5 CO 1 — 1 pj 1— 1 nJ vO r-l X VO O CO X vO II II 1^1 rtrooocnoocMO -— < (N CM --H .-< Ln o OOLO"— Ir-tOOi— ICT( vOLOOor^CTiootOi— I >-< CNJ (N CM •^ '^ O CM — I -^ O 00 CM 1 1 r-( 00 LO LO >— I O \0 Q Csl O u OQ I VO Pi > CO H CO o < •-J Q CO l-J CO w CO I— I CO 1-4 a; U ►J < t— ( a: Qi tu tq H J >- S H ■^ vD 00 o^ O '* vooooldoooooz •-H(NrNtO';fvOOO< --( CM Cl, I VO I— I 105 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL, IN 6 6 6 6 6 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 1 (17 INCH INITIAL BED HEIGHT) 6X9 MESH LIMESTONE SPARGER FLUIDIZING VELOCITY FT/SEC 1.77 2.35 2.94 3.53 4.12 4.71 4.71 4.71 4.71 5.29 5.29 5.29 5.29 5.88 5.88 5.88 5.88 6.47 6.47 6.47 6.47 7.06 7.06 7.06 7.06 7.65 7.65 7.65 7.65 7.06 7.06 7.06 7.06 6.47 6.47 6.47 6.47 DENSITY BED AP* LB/CU FT IN/IN 83.7 0.263 83.7 0.641 83.7 0.904 83.7 1.255 79.3 1.224 73.0 1.313 73.0 1.224 73.0 1.167 73.0 1.209 64.6 1.401 64.6 1.284 64.6 1.196 64.6 1.341 58.0 1.370 58.0 1.255 58.0 1.284 58.0 1.313 55.2 1.341 55.2 1.196 55.2 1.166 55.2 1.255 52.6 1.370 52.6 1.166 52.6 1.138 52.6 1.196 50.3 1.370 50.3 1.224 50.3 1.138 50.3 1.255 52.6 1.458 52.6 1.166 52.6 1.138 52.6 1.282 55.2 1.341 55.2 1.224 55.2 1.138 55.2 1.313 ♦INCHES WATER COLUMN PER INCH OF BED HEIGHT Table 6-3. LIMESTONE FLUIDIZATION TESTS - Run 6 - IIA (Sheet 1 of 5) 106 TEST 1 (17 INCH INITIAL BED HEIGHT) MATERIAL FLUIDIZED 6 X 9 MESH LIMESTONE GAS DISTRIBin'OR SPARGER PROBE POSITION FLUIDIZING VELOCITY DENSITY BED AP* FROM WALL , IN FT /SEC LB/CU FT IN/IN 5.88 61.2 1.224 3 5.88 61.2 1.196 6 5.88 61.2 1.196 9 5.88 61.2 1.341 5.29 64.6 1.341 3 5.29 64.6 1.167 6 5.29 64.6 1.224 9 5.29 64.6 1.313 5.00 66.9 1.224 3 5.00 66.9 1.282 6 5.00 66.9 1.196 9 5.00 66.9 1.429 4.71 73.0 1.341 3 4.71 73.0 1.224 6 4.71 73.0 1.224 9 4.71 73.0 1.341 4.41 78.1 1.224 3 4.41 78.1 1.196 6 4.41 78.1 1.224 9 4.41 78.1 1.255 6 — • 4.12 83.8 1.109 6 3.53 87.1 1.109 6 2.94 88.7 0.918 6 2.35 90.5 0.817 6 1.76 90.5 0.495 *INCHES WATER COLUMN PER INCH OF BED HEIQIT Table 6-3. LIMESTONE FLUIDIZATION TESTS - RUN 6 - IIA (Sheet 2 of 5) 107 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL, IN 6 6 6 6 6 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 2 (24 INCH INITIAL BED HEIGHT) 6X9 MESH LIMESTONE SPARGER FLUIDIZING VELOCITY FT /SEC 1.77 2.35 94 53 12 71 71 71 4.71 00 00 00 00 30 30 30 30 59 5.59 59 59 88 88 88 88 47 47 6.47 6.47 06 06 7.06 06 65 65 65 65 DENSITY BED AP* .B/CU FT IN/IN 90.8 0.554 90.8 0.933 90.8 1.313 88.6 1.692 82.7 1.224 76.0 1.429 76.0 1.429 76.0 1.313 76.0 1.458 73.0 1.516 73.0 1.516 73.0 1.429 73.0 1.604 67.7 1.516 67.7 1.516 67.7 1.341 67.7 1.458 63.1 1.838 63.1 1.604 63.1 1.370 63.1 1.750 59.1 1.747 59.1 1.525 59.1 1.692 59.1 1.546 55.5 1.662 55.5 1.370 55.5 1.429 55.5 1.458 49.6 1.516 49.6 1.341 49.6 1.313 49.6 1.313 44.3 1.429 44.3 1.546 44.3 1.401 44.3 1.575 ♦INCHES WATER COLUMN PER INCH OF BED HEIGHT Table 6-3. LIMESTONE FLUIDIZATION TESTS - RUN 6 - IIA (Sheet 3 of 5) 108 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL, IN 3 6 9 3 6 9 3 6 9 3 6 9 6 6 6 6 6 2 (24 INCH INITIAL BED HEIGHT) 6X9 MESH LIMESTONE SPARGER FLUIDIZING VELOCITY FT/SEC 6.47 6.47 6.47 6.47 5.88 5.88 5.88 5.88 5.30 5.30 5.30 5.30 4.68 4.68 4.68 4.68 4.10 3.51 2.93 2.34 1.76 DENSITY BED AP* LB/CU FT IN/IN 57.2 1.458 57.2 1.370 57.2 1.575 57.2 1.662 59.1 1.575 59.1 1.429 59.1 1.487 59.1 1.604 65.3 1.633 65.3 1.444 65.3 1.429 65.3 1.516 70.2 1.575 70.2 1.487 70.2 1 . 862 70.2 1.487 76.0 1.255 84.6 1.138 86.6 1.021 86.6 0.861 86.6 0.686 *INfflES WATER COLUMN PER INCH OF BED HEIGHT Table 6-3. LIMESTONE FLUIDIZATION TESTS - RUN 6 - IIA (Sheet 4 of 5) 109 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL, IN 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 6 3 (36 INCH INITIAL BED HEIGHT) 6X9 MESH LIMESTONE SPARGER FLUIDIZING VELOCITY FT /SEC 1.76 2.34 2.93 3.51 4.10 4.68 4.98 5.27 5.56 5.86 6.44 5.86 5.27 4.68 4.09 3.51 2.93 2.34 1.76 1.17 DENSITY BED AP* LB/CU FT IN/IN 85.6 PRESSURE 85.6 TAP OUT 85.6 OF 85.6 SERVICE 80.7 74.2 68.7 65.5 65.5 55.1 49.3 55.1 65.5 72.3 78.4 83.7 85.6 86.9 87.7 87.7 ' r *INCHES WATER COLUMN PER INCHES OF BED HEIGHT Table 6-3. LIMESTONE FLUIDIZATION TESTS - RUN 6 - IIA (Sheet 5 of. 5) 110 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL, IN 6 6 6 6 6 6 6 6 6 6 6 4 (13 INQI INITIAL BED HEIGHT) 6 X 16 MESH LIMESTONE SPARGER FLUIDIZING VELOCITY FT/SEC 1.13 1.69 2.25 2.82 3.38 3.94 4. 51 5.07 5.63 6.19 6.76 DENSITY BED AP* .B/CU FT IN/IN 88.6 0.787 88.6 1.123 86.2 0.889 73.1 0.875 67.2 0.926 61.1 0.955 56.0 0.969 50.2 0.918 46.7 0.918 40.5 0.896 37.3 0.963 TEST MATERIAL FLUIDIZED PROBE POSITION FROM WALL, IN 5 (24 INCH INITIAL BED HEIGHT) 6 X 16 MESH LIMESTONE ZING VELOCITY FT/SEC 1.66 2.49 2.90 3.31 3.81 4.14 4.97 5.80 6.77 DENSITY LB/i CU FT 88 .8 82, .9 76, .3 69. ,9 64. ,0 58. 1 53. 2 47. 8 41. 9 BED AP* IN/IN 1.144 1.516 1.458 1.516 1.429 1.415 1.356 1.269 1.093 *INCHES WATER COLUMN PER INCH OF BED HEIGHT Table 6-4. LIMESTONE FLUIDIZATION TESTS - RUN 6 - IIA (Sheet 1 of 2) 111 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL, IN 3 6 9 3 6 9 3 6 9 3 6 9 3 6 9 6 (36 INCH INITIAL BED HEIGHT) 6 X 16 MESH LIMESTONE SPARGER FLUIDIZING VELOCITY E FT/SEC L 1.60 2.00 2.40 2.40 2.40 2.40 3.20 3.20 3.20 3.20 3.60 3.60 3.60 3. 4. 4. 4. 4. 4. 4. 60 00 00 00 00 40 40 4.40 4.40 3.20 2.40 2.00 1.60 0.80 DENSITY BED AP* .B/CU FT IN/IN 89.5 1.152 88.8 1.224 84.7 1.240 84.7 1.255 84.7 1.255 84.7 1.269 68.1 1.341 68.1 1.341 68.1 1.341 68.1 1.341 65.1 1.370 65.1 1.284 65.1 1.341 66.9 1.313 59.3 1.341 59.3 1.313 59.3 1.282 59.3 1.298 55.6 1.166 55.6 1.166 55.6 1.166 58.0 1.109 71.8 1.166 82.9 1.181 88.8 1.167 89.5 1.079 89.5 0.569 ♦INCHES WATER COLUMN PER INCH OF BED HEIGHT Table 6-4. LIMESTONE FLUIDIZATION TESTS - RUN 6 - IIA (Sheet 2 of 2) 112 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL FROM CONE IN IN 1(32 INCH INITIAL BED HEIGHT) 20 X 65 CHAR 3 INCH CONE WITH WIRE SCREEN FLUIDIZING VELOCITY DENSITY FT/SEC LB/CU FT BED AP* IN/IN 6 6 6 6 6 6 6 6 6 6 6 6 6 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 -1 11 23 23 11 11 11 11 11 23 23 23 11 11 11 11 11 5 5 11 0.0 76 0.153 0.229 0.259 0.30 7 0.381 0.454 0.525 0.525 0.525 0.595 0.595 0.664 0.664 0.664 0.664 0.664 0.664 0.79 8 0.79 8 0.917 0.917 0.917 1.040 1.040 1.040 1.241 1.041 1.041 0.919 0.919 0.799 0.799 42.1 0.627 41.2 0.992 40.4 1.296 39.5 1.006 38.3 0.700 37.3 0.772 36.6 0.846 36.1 0.864 36.1 0.715 36.1 0.641 34.9 0.627 34.9 0.656 33.4 0.627 33.4 0.976 33.4 0.671 33.4 0.655 33.4 0.627 33.4 0.715 31.3 0.715 31.3 0.700 30.0 0.686 30.0 0.686 30.0 0.612 28.0 0.627 28.0 0.612 28.0 0.686 26.7 0.671 29.4 0.700 29.4 0.686 30.9 0.686 30.9 0.715 33.0 0.758 33.0 0.744 *INCHES WATER COLUMN PER INCH OF BED HE I Q IT Table 6-5. CHAR FLUIDIZATION TESTS - RUN 6 - IIB (Sheet 1 of 4) 113 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL FROM CONE IN IN 1 (32 INCH INITIAL BED HEIGHT) 20 X 65 CHAR 3 INCH CONE WITH WIRE SCREEN FLUIDIZING VELOCITY DENSITY FT/SEC LB/CU FT BED AP* IN/IN 0.665 0.517 0.381 0.305 0.229 0.185 0.154 34.9 0.729 36.7 0.729 39.7 0.729 41.0 0.744 42.2 0.627 42.2 0.511 42.4 0.423 *INCHES WATER COLUMN PER INCH OF BED HEIGHT. Table 6-5. CHAR FLUIDIZATION TESTS - RUN 6 - IIB (Sheet 2 of 4) 114 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL FROM CONE IN IN 6 11 6 11 6 11 6 11 6 11 6 5 6 17 17 11 5 5 11 6 11 6 11 6 5 6 17 6 17 6 11 6 5 5 6 5 11 17 17 11 5 5 11 17 6 17 6 11 6 5 6 5 6 11 2 (32 INCH INITIAL BED HEIGHT) 20 X 65 CHAR 3 INCH CONE WITH WIRE SCREEN FLUIDIZING VELOCITY FT/SEC 0.076 0.151 0.227 0.303 0.376 0.376 0.376 0.376 0.376 0.376 0.522 0.522 0.522 0.658 0.658 0.658 0.793 0.79 3 0.793 0.79 3 0.793 0.793 0.793 0.926 0.926 0.926 1.0 36 1.036 1.036 1.036 1.036 1.036 1.153 1.153 y DENSITY BED AP* LB/CU FT IN/IN 42.4 0.103 42.4 0.394 42.2 0.567 40.2 0.802 39.4 0.729 39.4 0.744 39.4 0.729 39.4 0.715 39.4 0.729 39.4 0.686 36.9 0.655 36.9 0.686 36.9 0.715 35.4 0.729 35.4 0.787 35.4 0.686 32.8 0.672 32.8 0.729 32.8 0.772 32.3 0.656 32.3 0.700 32.3 0.686 32.3 0.686 30.0 0.686 30.0 0.672 30.0 0.672 28.0 0.686 28.0 0,686 28.0 0.672 28.0 0.671 28.0 0.686 28.0 0.686 27.0 0.686 27.0 0.672 *INCHES WATER COLUMN PER INCH OF BED HEIGHT Table 6-5. CHAR FLUIDIZATION TESTS - RUN 6 - IIB (Sheet 3 of 4) 115 TEST MATERIAL FLUIDIZED GAS DISTRIBUTOR PROBE POSITION FROM WALL FROM CONE IN IN 6 6 6 6 6 6 6 6 6 6 6 6 2 (32 INCH INITIAL BED HEIGHT) 20 X 65 CHAR 3 INCH CONE WITH WIRE SCREENS FLUIDIZING VELOCITY DENSITY BED AP* FT/SEC LB/CU FT IN/IN 1.1S3 27.0 0.641 1.141 27.0 0.672 1.141 27.0 0.700 1.141 27.0 0.700 1.242 26.2 0.686 1.147 27.2 0.672 0.982 30.0 0.672 0.858 32.3 0.672 0.734 33.8 0.700 0.597 36.7 0.700 0.455 38.9 0.729 0.306 41.1 0.744 0.229 42.4 0.627 0.153 42.4 0.409 0.000 43.0 0.000 ♦INCHES WATER COLUMN PER INCH OF BED HEIGHT Table 6-5. CHAR FLUIDIZATION TESTS - RUN 6 - IIB (Sheet 4 of 4) 116 o Tf Irt Csl LO •^ VO r^ \o at •»CM 1— 1 o ■^ in CM lO -^ vO r-t r- VO CTi •> CM i-H O "^ a> vo Lo "^ VO •^ vO a\ •« CM rH !5 ^ a> 00 Lo to VO t^ 00 o> o . •»CM VO 1— 1 S? ""ia- Oi '^ a> to VO 00 o Oi LO CM C7» to VO « to a> LO to rH lO to rH* 00 cr> CM to ri O — I to (vj to csl to to r^ . •. to 00 t^ CM O (N CNJ to f^ r-l 00 o LO . 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H O M CO CO pq E- ( o 00 o (M ^ vO to (N (71 O LO o LO to 00 •>»■ to —I r^ 00 Tj* o ^ vo I/) --I CM vo 01 '!■ O 'H to CM |-> LO l^ LO vD ':r ^-1 to to CM to r^ a» ^ f^ o t^ o en ■ o ^ f~^ 00 ^ 00 CM CM r^ 10 r-i -a- LO to (N 1 00 •» «» ^ rC 10 Lo" to r-( • VO 00' to' r^ r-- ^ to Nl CM 00 to '^ VO to t^ LO r^ 00 ,—1 to vr> c^ 1 10 CJi LO r-i rr 10 rvi CM ^ "^^ vO VO t rv4 ^, t^ '^ '-; VO —1 to rg o I t-^ LO vO to * 10 >-H Tf to 00 LO — 1 -^ C7) O) 00 (M ( -H ,-< ■^ E- .12 ! ° i a: u < O Q •UJ ^ ^ < w [U Q H t- S H UJ w 8Q UJ (/3 •-1 >-( UJ OS CQ to t- H >-< (- ajoQcQaooi-iHHoSoQcomS nT^ 8 8 s g CI. o UJ U _J < :§ I Ci r-i H 123 FEBRUARY 12 to MARCH 11, 1973 CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 124 FOREWORD Run 7 was initiated February 12 and terminated March 11, 1973, with several interruptions in operation to remove solid plugs or repair malfunctioning equipment. As in Run 5, the ultimate objective was to produce gas contin- uously at a preestablished set of conditions for a reasonable length of time. Most of the operations required for gasification were achieved, but only intermittently, and desired operating parameters were not achieved simultaneously. The knowlege gained in the Run 6 fluidization tests, together with the extended interval between full operation in Runs 5 and 7 (while the regenerator refractory was being replaced), allowed a thorough, extensive review and revision of operating procedures. The resulting general startup procedure and the detailed operating procedure are presented as Sections 3 and 4 of this report. This report reviews the events of Run 7, the accomplishments made and problems encountered. 125 1 SUMMARY Run 7 had many successes, including: (1) Steady circulation of acceptor on a continuous basis. (2) Full batch calcination of limestone acceptor; this was the first time limestone, rather than dolomite, was used as acceptor. (3) Combustion of natural gas in the regenerator for the first time; this was a new procedure to speed startup and to eliminate erratic regenerator temperatures that had resulted in earlier runs when initial char transfer from the gasifier to the regenerator had been erratic and hard to control. The run was plagued with equipment failures, line plugs, loss of interface in the gasifier, and so on. It was necessary to dump the solids and recharge the system several times. The temperature and pressure probes in the regenerator broke when they were heated to about 1950 F, leaving regenerator operating conditions partially unknown. Finally, when an agglomeration of solids in the gasifier could not be broken, and numerous line plugs occurred simultaneously, the run was terminated. 126 2 DISCUSSION Run 7 was the first full-scale operation since termination of Run 5 on November 1, 1972. At the termination of Run 5, the refractory lining in the regenerator was so extensively damaged that total replace- ment was necessary. During the three-month interval required for re- fractory replacement, Run 6, a fluidization testing program, was con- ducted, first in the glass model and then in the gasifier system, which was totally isolated from the regenerator and other systems. Run 6 provided much-needed information on interface stability, fluid bed activity, and gas distribution requirements. This information was used in revising the system itself and in revising the operating procedures for Run 7. 2.1 SYSTEM CHANGES FROM PREVIOUS RUNS Significant changes made to the system (in addition to refractory replacement) were: (1) Installation of a bypass on the hot potassium carbonate system so that troublesome pressure buildups in this system could be avoided. (2) Installation of a sparger-type gas distributor in the regenerator. (3) Revision of steam piping to the gasifier to allow separate steam feed to either the transition section, the bottom, or both was done during the run. (4) Installation of instrumentation to positively identify the acceptor-char interface. 2.2 OPERATING SEQUENCE Prior to startup, the system was pressure tested, final adjust- ments were made to all instruments, and the new refractory lining in the regenerator was "cured" in accordance with procedures recommended by Conoco 's insulation-refractory specialist. Run 7 started February 12. During initial startup, there was a high pressure drop in the regenerator recycle gas system; this was cured by reinstalling a bypass on the hot potassium carbonate system. A plug developed between the gasifier quench tower and separator; this was broken and the solids were cleared. A capacity test was run on four recycle compressors, including two devolatilizer compressors that had been connected in parallel with the regenerator recycle compressors. Total capacity of the four mach- ines was 131,000 SCFH. Limestone was charged to the gasifier boot February 15 but dumped because instruments indicated low density; apparently some char 127 residue from Run 6 mixed with the acceptor. It was recharged the next day, then limestone was fed to the regenerator both directly and by transfer from the gasifier. A plug developed in the acceptor lift line between the engager pot and the regenerator, so both vessels were dumped on the 17th. While in the vessels, the limestone had been subjected to very high velocities from the distributor gas jets; the dumped material had an excessive amount of fines. By shifting part of the flow to the acceptor lift line, the flow through any given inlet was reduced to a maximum port velocity of 160 feet per second. Total flow to the regen- erator was reduced from 175,000 SCFH to 138,000 SCFH. The system was again pressurized and heated on the 18th and limestone levels were established on the 19th. The gasifier was dumped and recharged because a differential pressure instrument indicated excessively low density. The regenerator lift gas heater (B-205) was providing insuf- ficient heat. After extensive tests, the problem was solved by re- placing the burner tip on the heater. The air lift heater (B-203) shut down intermittently; this problem was corrected by adjusting the low flow switch and the fire eye. By February 22, the proper limestone levels had been established in both vessels and a seal had been established in the regenerator-to- gasifier acceptor transfer line (above TCV-2030) . At this time lime- stone was circulated and natural gas combustion heated the regenerator. Circulation and natural gas burning were stopped while char was charged to the gasifier. This was char that had been removed from the gasifier after Run 6 -- it contained a considerable amount of limestone and the gasifier transition section became unstable because of the limestone contained in the char bed. As a result, the interface was lost. The gasifier was dumped. More "used" char (containing less limestone) was used in recharging the gasifier. A bridge developed in the boot but was broken. A char bed ten feet deep was established. On the 23rd, gas vented back from the acceptor lockhopper to the gasifier, again disrupting the interface. The gasifier was dumped again. Bed levels were reestablished and limestone was circulated. On the 24th, when steam was added to the gasifier, the steam feed valve opened fully because of a blocked-in instrument air line; again the interface was lost and gasifier was dumped. All levels were reestablished on the 25th and limestone circu- lation established, although circulation was not steady. In preparation for adding steam, apparently a slug of water went to the gasifier, disrupting the interfac Shortly afterward, in unplugging a drain line, there was a sudden system pressure drop causing backflow from the regenerator to the gasifier. The regenerator bed slumped and could not be refluidized. Both vessels were dumped. 128 On March 1, limestone was circulating between the vessels, steam was being fed to the gasifier, and addition of natural gas to the regen- erator for heat was started. The char was pregasified with steam to reduce its density. On March 2, the interface was lost, during a boot flow test, and the char lift line became plugged simultaneously. The char feed was material that had previously been dumped from the gasifier and it contained some limestone; this may have contributed to difficul- ties experienced in feeding char. The plug was cleared, but the inter- face could not be regained; therefore, the gasifier was dumped on March 3, Then recharging of the gasifier started. Bed levels were again established on March 4. Limestone circula- tion was lost, then reestablished March 5. Natural gas combustion in the regenerator was resumed, and steam addition to the gasifier was reestablished to reduce char density. On March 6, while experimenting with gas flow to the boot, the interface was lost and some char- stone mixture was transferred to the regenerator. Limestone was shot-potted to the gasifier; after trying to reestablish the interface unsuccessfully with constant boot gas flow, the flow was varied some, and the interface was reestablished on the 7th. Acceptor circulation and steam gasification were reestablished. On the 8th the char preheater was put in service to feed hot char to the gasifier. Limestone circulation from the regenerator to the gasifier was lost, then regained, by reducing regenerator temperature and in- creasing differential pressure between vessels. Char feeding was stop- ped during this upset. On March 9 through 11, there was a series of problems that re- sulted in the decision to terminate Run 7. First, there was bridging in the transition section of the gasifier, above the boot, preventing showering of limestone. Then, while calcining limestone, the lines to the ash lockhoppers plugged. The line from the gasifier boot to the spent dolomite lockhopper plugged, preventing dumping of the gasifier. The acceptor in the boot apparently agglomerated, forming a plug which could not be broken. A large amount of calcined limestone was lost overhead from the regenerator. Shutdown was initiated on March 11, ter- minating Run 7. Draining the system and opening the regenerator top head revealed: (1) That all of the temperature and pressure probe supports in the regenerator had failed. (2) That the regenerator temperature probe had separated at its welds. (3) That a thick (l/4-to-3/8-inch) hard glaze deposit (97 per- cent CaO) covered the regenerator walls. (4) That the glaze deposit was heaviest at the locations of cold projections into the reactor. All differential pressure probes and the transfer line outlets were covered with heavy deposits. 129 (5) That the hardface refractory near the air inlet line had been eroded by high-velocity gas jets from the air sparger Pit depth ranged to about 3 inches. 2.3 ACCEPTOR AND CHAR DATA Table 7-1 presents data on the limestone acceptor. A screen analysis and chemical analysis of fresh limestone acceptor feed are shown. Screen analyses of typical acceptor samples removed from two different sample points on February 22 and March 5 are shown These samples show that all sizes of acceptor showered freely through the char At the end of the run, samples were taken of the glaze deposit on the regenerator walls and the agglomerate balls in the regenerator bed- chemical analyses of these materials are shown. The agglomerate baUs' and glaze deposit have essentially the same composition as the fresh acceptor. j-icau ^nH ho l^^^^J-^ ^i^Wf ^he average size distribution, chemical analysis and heat content of the fresh char used in this run. 2.4 OPERATING CONDITIONS Operating conditions - flows, temperatures, and overhead gas 7-4!°?espec?i;;?y! "^""^ ^'' '"'^""""^ '' ""^ ^""^^ '' ^^ ^^^^^^ ^"^ and who. . J^^ conditions on February 22 are just prior to char addition when the system was fully charged with limestone acceptor and the accep- tor was being circulated continuously. Heat was being supplied to the regenerator by combustion of natural gas, but the tempera?ure had not been raised to the point of calcination. ^^ naa not with hoth^^''"^'^'°''' ^°'' ^^""^^ ^ ^""^ ^^^" ^^^ ^y^^^^ ^as fully charged W .h l^'^^stone acceptor and char. Acceptor was being circulate! suonlied Tn\T' '""' transferred to the regenerator. hL was being supplied to the regenerator by combustion of natural gas. Steam was being added to the gasifier to react with char and reduce its density to calcliled'' ""''" ''°"'''"^- "'^ '^^^^^°"^ ^-^P^- ^-d not yet been 2.5 NATURAL GAS COMBUSTION IN THE REGENERATOR in the regenerator'^'^^hr'' '" '"" ' ^"^ ''' combustion of natural gas possible conSon^H h h J"""^"'^ "^^ '° '^°^'^" ^'^^^"P ^i"'^ ^"d make Chilli ^°"5^°llfd high-temperature operation without burning char in the regenerator. In previous runs, transfer of char to the regenerator t^o f^' ^''? ''■^^'^"' "'^'^^"2 i^ impossible to achieve good controJof temperature. It was intended that when char was transferred to ?he 130 Natural gas was first introduced February 22 with no untoward results. Combustion was initiated at temperatures as low as 1100 F without difficulty. This procedure was thus established as a regular means for speeding startup and controlling temperature, 2.6 CALCINATION Full calcination of limestone was achieved in Run 7. This is graphically shown in Figure 7-1, a time chart of regenerator temper- ature, equilibrium partial pressure of carbon dioxide for the calcina- tion reaction at that temperature, and measured carbon dioxide partial pressure in the overhead gas from the regenerator. The time period is late March 9 and early March 10. At the start of the period, with a regenerator temperature slightly over 1700 F, the measured and equil- ibrium partial pressures match within practical limits of measurement. When the regenerator temperature rose early March 10, to a high of 1940° F, the actual carbon dioxide pressure did not rise to meet reac- tion equilibrium conditions. This indicates that full calcination was achieved. 2.7 MATERIAL BALANCE A solids material balance was attempted during Run 7. Results were: Solids Charged to System Pounds Limestone in from Lignite Lockhopper 6,010 Limestone in from shot-pot 150 Limestone in from Acceptor Feed Lockhopper 39,450 Char in from lockhoppers 25,270 Total in 68,880 Solids Removed Fines from ash hoppers 9,210 Material removed from gasifier acceptor dump 10,210 lockhopper Carbon dioxide vented in calcination 20,050 Solids to water holding pond 4,070 Char reacted (rough estimate) 6,800 Miscellaneous measured cleanup 2,100 Total out 52,440 Deficit 16,440 Thus, 25 percent of the material charged was not accounted for. Large quantities of solids were retained in the system after shutdown and the methods required for cleanout precluded measurement. None- theless, material balance techniques were shown to be inadequate. They have been revised in the light of experience gained in this attempt and, hopefully, will lead to better results in the future. 131 2.8 GASIFICATION Figure 7-2 shows temperatures, flows, and the composition of gasifier outlet gas during the reduction of char density with steam. Substantial reaction heat was provided from sensible heat of acceptor. The response of gas composition to steam addition and to bed temperatures is quite similar to that shown in Figure 6-11 of the report on Run 6. Fresh char was fed during this run, as shown in Figure 7-2, whereas no char was added during Run 6 gasification. A study of Figure 7-2 itself will be more fruitful than a detailed description here. 132 3 STARTUP PROCEDURE FOR RUN 7 (1) Pressure test at 150 pounds. (2) Establish recycle as follows: Gasifier Inert Gas Boot Total FRC-2126 5,000 SCFH FRC-2019 37,000 SCFH FRC-2020 57,000 SCFH Regenerator Char Lift Gas Air Lift Gas FRC-2015 7,000 SCFH FRC-2113 50,000 SCFH FRC-2014 50,000 SCFH (3) Heat up system. Bring quench systems on at 250° F (Compressor suction temperature) Regenerator heater at 1450° F. Gasifier heater at 1150° F. (4) Regenerator flow tests. Determine maximum recycle capacity. (5) Set maximum recycle capacity and air to give 175,000 SCFH. Maintain temperature at 1450° F and split flows between B-203 and B-205 to give maximum temperature with maximum control. (6) Feed 1200 pounds acceptor (6 X 16 limestone) to boot via F-204 A or B. Weigh in exact amount. Be sure all tote bins are sampled during filling and that fines criteria has been met. (7) Charge 2000 pounds limestone to F-206. Begin feeding to regenerator. Keep feed at level which allows regenerator temperatures to remain above 1000° F. Keep accurate records of feed RPM and feeding time. Include time and notation of RPM changes. (8) Note when the following regenerator bed differential pressure recorder pens lift: DPR-2018, 2074, 2019, 2075, and 2020. (9) Continue feeding until regenerator is full. DPR-2076 equals DPR-2075. (10) Set dPRC-2030 on 5 PSI. Adjust regenerator recycle rate to maintain discharge pressure. (11) Briefly circulate acceptor to prove integrity of system and test new controller, LIC-2003. 133 (12) Run gasifier flow tests to determine incipient fluidizing velocity. (13) Feed char bed (use both hoppers) . Feed continuously at minimum RPM. Use material from Run 6-1 II. Bring char bed level to 25 feet (lift pen on 2033). (14) Observe behavior of LIC-2003. If OK, resume circulation by opening TCV-2030. (15) Initiate combustion in regenerator by adding methane. Note temperatures in bed. If hot spot occurs, cease fuel addition. Char will then be used as heating fuel; revised operating instructions will be required. Decrease air 10,000 SCFH/100° F until 2 to 4 percent CO con- centration is obtained. (16) Bring temperature of regenerator to 1700° F and line out. Minimum amount of fluidizing gas, 135,000 SCFH at 1700° F. (17) When gasifier bed reaches 1250° F, add steam. Add 13,000 SCFH steam and reduce recycle gas by 10,000 SCFH (2.4 ATM steam pressure). (18) Adjust FIC-2019 downward to maintain constant boot velocity. Also correct setting for decreased temperature at orifice upon steam addition. As boot temperature increases, decrease flow on FIC-2019 according to following table: (Table may be revised depending upon results of Step 12) . SCFH 37,000 35,800 34,800 33,800 32,800 31,900 31,000 30,200 29,400 Also decrease the amount of recycle gas to maintain the same side flow (20,000 SCFH). (19) Increase acceptor circulation to keep temperature above 1200° F. Adjust air and fuel rate accordingly to keep regenerator temp- erature at 1700° F. (20) If hydrogen exceeds 10 mol percent, increase heater out- lets stepwise to 1500° F. 134 Temperature, °F 1100 1150 1200 1250 1300 1350 1400 1450 1500 (21) When gasifier bed density decreases to 25 LB/CU FT, increase regenerator temperature to calcine. (22) Line out regenerator temperature at 1850° F and adjust air and fuel rates to maintain reducing conditions (2 to 4 percent CO) , (23) Cut recycle flow to maintain total flow of 105,000 SCFH to regenerator. (24) When gasifier bed temperature reaches 1500° F, add 13,000 SCFH steam and reduce flow on FRC-2020 by 10,000 SCFH. Start preheater and bring temperature to 500° F. (25) Adjust acceptor circulation to obtain 1500° F in gasifier. (26) Open LCV-2002 to initiate char feed to regenerator and reduce methane to bring CO to 2 to 4 percent. (27) Continue above until methane is totally removed. (28) Charge preheater and begin feeding char to keep gasifier bed height at 20 to 25 feet. 135 4 DETAILED OPERATING INSTRUCTIONS On January 30, and February 7, 1973, meetings were held between Consol and Stearns -Roger concerning Run 7. The following procedure includes steps outlined in the meetings as well as previously estab- lished operations. 4.1 PRELIMINARY CONDITIONS AND INFORMATION (1) Regenerator refractory curing is complete. (2) Air flow from J-202 to regenerator shut off and B-203 shut down. (3) New data sheets available. (4) All dPT's and dPR's are to have been zeroed per SK-245. (5) All Moore regulators are to be bypassed. (6) All purges in service are to be at a reading of 2 during initial stages of pressurizations and be at a reading of 7 when up to operating pressure except the following: FI Setting FI Setting 2177 3.5 2176 3.5 2154 3.5 2153 3.5 2152 3.5 2278 20 2277 20 2276 20 2275 20 2069 20 2070 20 2072 20 2074 20 2280(2046 20 TEMP) 2041 20 2038 20 2036 20 2096 20 2098 20 2213 20 2100 20 2102 20 2104 20 During pressure testing and pressuring of system, bring all purges up slowly to values indicated above as system is brought to test or operating pressure. 4.2 PROCEDURE (1) Pressure test regenerator and gasifier systems to 175 PSIG with air in 25-PSI steps. Hold at each plateau and check for leaks. (2) After system has been successfully pressure tested with air, depressure system slowly in about 2 hours to atmospheric pressure. 136 (3) Unless already done, fill the revised regenerator quench tower, gasifier quench water separator and the foul water stripper water separator to operating levels with boiler feed water. Fill the piping, regenerator and gasifier jacket systems, if not already filled. Start circulation of jacket systems and begin chemical treatment of the water. Do not start steam to the regenerator and gasifier jacket systems at this time. Do not pressure the gasifier steam drum with inert gas. (4) Fill seal leg on steam line from gasifier steam drum. (5) Pressure the reactor system to 150 PSIG static pressure with inert gas through FIG -2 126 at 5,000 SCFH and through FRC-2015 from J-209 at 7,000 SCFH maximum or at the maximum output of J-309. J-309 may not be able to supply 7,000 SCFH, Do not line up the natural gas part of the system. The new double block and bleed station is to be blocked in and tagged closed with the bleed open. (6) Line up PCV-2022 (with PRC-2022 at 150 PSIG on automatic) PCV-3009 (with PRG-3009 at 100 PSIG on automatic) dPCV-2030-1 (dPRC-2030 at zero on manual) and PCV-2071 (with PRC-2071 at 80 PSIG on automatic) for normal operation. (7) Block in FCV-2032, FCV-2013, FCV-2014, and FCV-2113. (8) Close XCV-2024 on manual. (9) Block in regulators on A and B purge system from dryers. (10) Start one compressor of J-201. Set PRC-2052 at 250 PSIG. (11) Start J-207 A/B compressors. Set PRC-2041 at 250 PSIG. Be sure J-207 A/B are lined up in parallel with J-203 A/B. Observe operation of J-207 A/B for any unusual situations. (12) On A and B dryers, open the valves to vent a few turns to put some load on the dryers. Check out the performance of each dryer with respect to dewpoint at least through one cycle of each chamber. When the dewpoints can be maintained at least below -20 F, continue with this procedure. Be sure to record the results of this checkout. (13) The regulators on the A and B systems are set at 200 PSIG. Be sure these settings are maintained. Activate these regulators and close XCV-2070 and XCV-2072. Both dryers will then take over the supply to the purge systems. Report readings on PI -2167 and PI-2168. 137 (14) Recheck all rotameter settings. (15) Adjust all other rotameters to be in use in the structure. (16) Leave LCV-2003, LCV-2002, XCV-2073, XCV-2015, V-2048, and TCV-2030 open with valve kickers deactivated. (17) With dPRC's on manual, establish maximum flows through dPCV-2026 2036, and 2037. ' (18) Open XCV-2010 if it is not already open. (19) If J-207 A/B are operating satisfactorily, start J-203 A/B and the other compressor of J-201. We will men have six compressors running. Two of them will be on the gasifier recycle system and tour will be on the regenerator recycle system. (20) Set PIC-2047 at 200 PSIG on automatic. (21) Establish the following flows: (a) FRC-2126 5,000 SCFH (inert gas) to discharge of J-201 A/B. (b) FRC-2020 57,000 SCFH (recycle) to B-201 A/B from J-201 A/B. (c) FIC-2019 37,000 SCFH (recycle) to B-201-A, then FR-2260 will be 20,000 SCFH (recycle) to B-201-B. (d) FRC-2015 7,000 SCFH (inert gas) to B-204 from J-309. (see Step 5.) (e) FRC-2032 50,000 SCFH (recycle) to B-203 from J-203 A/B and J-207 A/B. (f) FRC-2014 50,000 SCFH (recycle) to B-205 from J-203 A/B and J-207 A/B. (g) FRC-2113 SCFH (air) to B-203 from J-202. (22) When the oxygen content of recycle gases is less than 2 per cent, start process heaters. B-203, B-204, and B-205 are brought to 1450 F final heater outlet temperatures B-201 IIA/IA and IIB/IB are to be brought to 1150° F final heater outlet temperatures. Raise all heater final outlet temp- eratures at an even rate of 100° F per hour until 1000° F IS reached. Then raise temperatures at the rate of 50° F per hour until the final outlet temperatures are reached Adjust dampers and registers for proper heater combustion by stack analyses. Monitor final furnace outlet tubes with optical pyrometer every four hours. Monitor new pencil 138 thermocouples in B-201 lA and IB outlet headers for un- equal readings which would indicate unequal gas flow through the heater tubes. (23) Close LCV-2003, LCV-2002, XCV-2073, XCV-2015, V-2048 and TCV- 2030 when the reactors have reached 1000° F. (24) Start quench system after inlet gas reaches 200° F. Bypass SO^ scrubber until quench towers are circulating. Then cir- culate SO2 scrubber and put on line. Start steam to regen- erator and gasifier Jacket water steam drums. Hold regen- erator steam drum at 200 F and the gasifier steam drum at 350 F. (25) The following should be kept drained and free of any condensed water during the heatup period: (a) F-207 A/B (b) F-216 (c) F-213 (d) Any other points where water might condense (sample points, etc.) (26) Hold at Step^22 final conditions until reactors are at a min- imum of 1000 F. Hold until further instructions are given. (27) Determine the regenerator recycle compressors rates at the following conditions: (a) 12 PSIG air loading on PRC-2041 . This is done by in- creasing the flows on FRC-2032 and FRC-2014 equally until PRC-2041 has an air loading of 12 PSIG. If at the con- ditions of Step 21, the air loading is already 12 PSIG or higher, reduce flows to give the 12 PSIG air loading. (b) 13 PSIG air loading on PRC-2041. (c) 14 PSIG air loading on PRC-2041. (d) Almost to 15 PSIG air loading on PRC-2041 but with instru- ment still on control. This will give the maximum recycle capacity of the four compressors. (28) With maximum regenerator recycle compressor capacity, bring gas from J-202, through FRC-2113, and through B-203 to give a total flow of 175,000 SCFH to the regenerator. Maintain regenerator heater outlets at 1450° F, have air and recycle to B-203, recycle to B-205, and inert gas to B-204. Adjust recycle between B-203 and B-205 to give the 1450° F outlets with best control. 139 (29) Determine the gasifier distributor differential pressure at varying boot flows. Keep the side flow at 20,000 SCFH. After the test, restore the boot flow to 37,000 SCFH. (30) Grind 1200 pounds of 6 X 16 limestone into a clean tote bin. Sample every 400 pounds for a composite sample to be sent to the lab for size consist. After lab results, confirm proper size consist (less than 5 percent through 20 mesh and less than 12 percent retained on 6 mesh), charge the 1200 pounds to one of the lignite lockhoppers. (31) Crack open LCV-2003 by manually setting 5 PSI output on LIC-2003. (32) Feed the 1200 pounds of Step 30 to the gasifier. (33) Set dPRC-2037 on automatic. (34) Charge the limestone in tote bin NO. 8 to F-206. Run through feeder L-204 to a clean empty tote bin until the low level alarm comes on. Close valve above feeder and empty feeder. Determine amount of limestone left in F-206. Have main- tenance replace swage under L-204. (35) Prepare tote bins with 2000 pounds of acceptable ground 6 X 16 limestone and charge F-206 with 2000-pound batches. Sample every 500 pounds for composite sample to lab. Feed each batch to the engager pot and thereby to the regenerator. Feed at a rate which allows the regenerator temperatures to stay above 1000° F. Feed only until the low level alarm comes on before recharging F-206. Keep accurate records of feeder RPM and the time of feeding. Note any RPM changes and record the time at each change. This is very important. Keep complete records of all materials in and out of the reactors. (36) When each of the following dPR's lift, note the time on the respective chart, read and record all dPR's. dPR-2018 dPR-2074 dPR-2019 dPR-2075 dPR-2076 dPR-2020 (37) Continue feeding until dPR-2077 equals dPR-2076. This will indicate about 25 feet of acceptor in the regenerator. (When dPR-2077 lifts, we will then have a seal above TCV-2030. Set dPRC-2026 on automatic.) 140 (38) When regenerator acceptor bed has been established set dPRC-2030 (using dPCV-2030-1) on 5 PSI. If necessary, adjust regenerator recycle rate to maintain compressor discharges at 250 PSIG. (39) Set dPRC-2036 on automatic. (40) Circulate acceptor for 2 to 3 hours to prove integrity of the system and to test and tune the revised controller LIC- 2003. Check all instruments and other equipment for proper operation or problems. Obtain solids samples from new sam- pling points in order to test the sample collection systems. (41) Run gasifier flow tests under Consol's direction to determine boot incipient fluidizing velocity. (42) Using char from the gasifier from Run 6- II I (currently tote bins 13, 14, and maybe 6) first and then ground char in tote bins 12, 16, 17, charge the lignite lockhoppers. Grind additional char as needed. (43) Feed char to the gasifier continuously at minimum RPM on the feeder, using one lockhopper at a time. (44) Bring char bed level to about 25 feet as indicated by dPR-2033 starting to show a pressure differential. Have lignite lock- hoppers empty when this bed level is reached. (45) Observe behavior of LIC-2003. If it is operating satisfac- torily, resume circulation of acceptor by first opening TCV-2030 slowly to an air loading of 8 PSI. When an indi- cation is obtained on dPR-2035 (and LIC-2003) of an increase in acceptor level, set LIC-2003 on automatic. (46) Continue circulation of acceptor unless system is upset, interface between char and acceptor deteriorates or other abnormal condition occurs. During circulation, the acceptor (near 1300° F) will heat the char (initially near 1050° F) and the acceptor will be cooled in the gasifier. (47) Initiate combustion in the regenerator by adding methane to the suction of J-309 at the rate of 1000 SCFH. (48) Monitor regenerator bed temperatures closely. If any hot spots occur, cease methane addition immediately. Char will then be used as fuel. If no hot spots occur, continue methane addition and decrease the air to the regenerator 10,000 SCFH per 100° F rise in regenerator temperature until 2 to 4 per- cent CO concentration is obtained. Then maintain air at this rate and reduce recycle 10,000 SCFH per 100° F rise. 141 (49) If char is used as fuel, feed to regenerator via LCV-2002. Rate of addition will be established by Consol . Air rate o will be decreased 10,000 SCFH per 100 F rise in regenerator temperature and a 2 to 4 percent CO concentration will be established. Then recycle gas will be reduced 10,000 SCFH per 100 F rise instead of air. (50) Bring temperature of regenerator to 1700 F and line out. The minimum required fluidizing gas at 1700 F is 135,000 SCFH. 1700 F is below calcining temperature, therefore, acceptor circulation is adding only sensible heat to the gasifier, not any chemical heat. (51) IVhen gasifier bed reaches 1250° F, slowly add 13,000 SCFH of steam while reducing recycle gas by 10,000 SCFH. (52) Adjust FIC-2019 downward to maintain the boot velocity as established in Step 41. Be sure to allow for the decreased gas temperature at the orifice because of steam addition in figuring meter factors. As boot temperature increases, decrease boot flow in FIC-2018 according to the following table: Temperature, °F SCFH 1100 37,000 1150 35,800 1200 34,800 1250 33,800 1300 32,800 1350 31,900 1400 31,000 1450 30,200 1500 29,400 NOTE: This table may be revised depending upon the results of Step 41, Maintain side flow at 20,000 SCFH unless otherwise directed. (53) Increase acceptor circulation to keep char temperature above 1200 F. Adjust air and fuel rate to keep regenerator tem- perature at 1700° F. (54) If hydrogen concentration in the gasifier overhead gas is above 10 percent or if the hydrogen to H^S ratio is above that supplied by Consol, increase gasifier heater final out- lets to 1500 F if possible. 1500 F is the target operating temperature in the gasifier but it may not be attainable this run. (55) When gasifier char bed density decreases to 25 LB/CU FT, increase regenerator temperature to calcine. A char bed height of 17 feet is minimum allowable. 142 (56) Line out regenerator at about 1850O F and adjust air and fuel rates to maintain 2 to 4 percent CO and calcine the acceptor. (57) As acceptor is calcined, cut recycle flow to regenerator to maintain a total flow of 105,000 SCFH to regenerator. (58) When gasifier bed temperature reaches 1500° F, slowly add 13,000 SCFH more steam and reduce recycle flow by an addi- tional 10,000 SCFH. (59) Using regenerator overhead gas, start preheater and bring temperature to 500° F. (60) Adjust acceptor circulation to obtain 1500° F in gasifier, if possible. Calcined acceptor will furnish chemical as well as sensible heat. (61) If methane has been used for fuel, initiate char feed to regenerator at this time through LCV-2002. As char is fed to regenerator, slowly reduce methane flow to keep CO in the 2 to 4 percent range. (62) Continue Step 61 until methane is totally removed. (63) When methane is totally removed, charge preheater and begin feeding char to gasifier via the lignite lockhopper to keep gasifier bed height at 20 to 25 feet. 143 2 < H < Cl. O u CQ :3 a a: W CO lU ' oi a. •-] < E- Di < Cl. o u _] < m E- M < -O DC Z :3 o S U UJ Z Q, 3 u H < OC (/) o < t- <; UJ UJ :d z to tU CO u UJ UJ a: a: a. I oo •H ^-^ ^[U73^Wai 2k?X7a^N-39aa 144 Figure 7-2. GASIFIER OPERATION - RUN 7 145 SIZE DATA DATE « • 2/22/73 2/22/73 3/5/73 3/5/73 AVERAGE TIME 1 1 1 5* l2 30Vf 1100--'Vf 1 1 OOVfVr ACCEPTOR SAMPLE LOCATION S-10 S-9 S-10 S-9 FEED AND LCV-2003 TCV-2030 LCV-2003 TCV-2030 MAKE-UP MESH SIZE 4 , 6 1.5 0.9 8 14.5 17.1 1^.9 14.3 20.1 9 18.7 20.2 19.0 20.0 19.2 10 18.2 20.7 16.4 16.5 15.0 12 14,7 15.1 12.8 12.7 12.5 14 13,7 13.5 13.1 12.1 12.7 16 7.7 7.4 9.5 8.8 9.6 20 3.1 3.4 8.1 7.3 7.7 24 0.7 0.8 3.8 3.4 2.2 28 0.4 0.3 2.5 2.2 0.5 PAN 6.6 0.5 2.0 2.4 0.5 BULK DENSITY, LB/CU FT 88 88 90 90 PARTICLE DENSITY, LB/CU FT 173 170 160 155 ACTIVITY ~ 0.9 0.82 0.81 ANALYSES CaO MgO Na20 Si02 SO3 R ''AI2O3 Ti02 FE2O3 K2O P2O5 ACTIVITY FRESH REGENERATOR BALLS FROM ACCEPTOR GLAZE DEPOSIT REGENERATOR 96.97 97.2 95.6 0.64 0.5 0.7 0.04 0.03 0.03 2.5 1.6 2.7 0.06 0.01 0.01 0.37 0.5 0.59 0.00 0.01 0.04 0.30 0.2 0.32 0.04 0.01 0.01 0.08 0.01 0.03 0.09 -NO CHAR BED --V.-CHAR BED HEIGHT, 17.5 FT Table 7-1. ACCEPTOR DATA FOR RUN 7 146 SIZE DISTRIBUTION MESH SIZE PERCENT 6 8 0.3 10 1.3 14 4.5 20 9.3 28 15.4 35 15.7 48 15.5 65 10.7 100 8.4 200 11.0 PAN 7.9 COMPOSITION PERCENT VOLATILE MATTER 13.5 C 72.8 H 2.1 N 1.1 S 2.5 ASH 20.2 CaO 18.2 MgO 4.8 Na20 2.1 Si02 28.5 SO3 20.8 \^ AI2O3 12.8 Ti02 0.4 FE2O3 8.1 P2O5 0.03 K2O 0.5 HEAT CONTENT - 11,650 BTU PER POUND Table 7-2. AVERAGE CHAR FEED DATA FOR RUN 7 147 NO CHAR IN GASIFIER GASIFIER FLOWS - SCFH REGENERATOR STEAM RECYCLE INERT TOTAL BOOT SIDE TOTAL 46,900 5,000 51,900 33,200 18,700 51,900 AIR RECYCLE INERT NATURAL GAS TOTAL AIR INLET ACCEPTOR LIFT CHAR LIFT TOTAL 36,300 92,700 7,300 136,300 36,300 92,700 7,300 136,300 TEMPERATURES - "F BOOT BOTTOM MIDDLE TOP 1000 950 (AVG.) BOTTOM MIDDLE TOP 1240 1320 1325 COMPOSITIONS - MOL. % CO COi CH4 H2S SOo 0.8 tr 9.0 90.2 0.0 0.0 0.0 0.0 CO CO. CH4 H2S SOo 16.8 0.0 2.1 81.1 0.0 0.0 0.0 0.0 Table 7-3. TYPICAL GAS FLOWS, TEMPERATURES AND COMPOSITIONS FOR RUN 7. FEBRUARY 22. 1973 CHAR BED IN GASIFIER GASIFIER FLOWS - SCFH STEAM 25,100 RECYCLE 12,000 INERT 5,000 TOTAL 42,100 BOOT 22,200 SIDE 19,900 TOTAL 42.100 REGENERATOR AIR RECYCLE INERT NATURAL GAS TOTAL AIR INLET ACCEPTOR LIFT CHAR LIFT TOTAL 23,500 111,800 5,200 1,900 142,400 40,800 94,500 7,100 142,400 TEMPERATURES - OF BOOT 1260 BOTTOM 1205 MIDDLE 1320 TOP 1264 COMPOSITIONS - MOL. 7o 02 CO 0.0 2.5 CO2 N2 H2 18.8 54.4 21.4 CH4 H2S SO2 2.6 0.3 0.0 BOTTOM NOT RELIABLE MIDDLE II TOP •1 02 CO C02 N2 H2 CH4 H2S SO2 0.0 0.4 12.4 86.4 0.4 0.4 0.0 0.0 Table 7-4. TYPICAL GAS FLOWS, TEMPERATURES, AND COMPOSITIONS FOR RUN 7, MARCH 5, 1973 149 RUN 8 MARCH 28 to APRIL 10, 1973 CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 150 FOREWORD Run 8 started March 28 and terminated April 10, 1973. The basic objective of the run was the same as Run 7: to achieve a demonstration gasification run. Significant changes from Run 7 were to eliminate all pauses in the run to conduct tests, and to return to use of dolomite as acceptor, rather than limestone which was used in Run 7. A thorough review of Run 7 took place on March 26 between Consol and Steams-Roger personnel, including the Shift Superintendents. The following day, general operating procedures for the run were estab- lished. They are recorded as Section 3 of this report. Detailed oper- ating instructions for the run are recorded as Section 4 of this report. Supplementary instructions for maintaining a reducing atmosphere in the regenerator were published during the run, and are recorded as Section 5. This report records the events of Run 8, the achievements accom- plished, the difficulties encountered, and significant data pertinent to the run. 151 1 SUMMARY Run 8 succeeded in establishing operation for a brief period at conditions very close to those desired. There were simultaneously: circulation of fully calcined acceptor, partial gasification of char in the gasifier, transfer of pregasified char (albeit somewhat unsteady) from gasifier to regenerator, and combustion of the pregasified char in the regenerator in order to recalcine acceptor. A new ring-type distributor was installed in the transition sec- tion of the gasifier during the shutdown prior to Run 8. This ring dis- tributes the sideflow gas more uniformly; the resulting more uniform bed facilitates showering of acceptor through the bed. Improved stability of the gasifier was probably the most significant result of this run. A new technique used in this run for the first time was to intro- duce air to the side of the gasifier (in combination with steam) . This speeded reduction of char density in the gasifier to a point where acceptor could easily shower down through the char bed. Some air was being fed to the gasifier throughout the run; thus, while the run demon- strated all the steps necessary for gasification, true gasification was not actually achieved. There were numerous difficulties encountered during the run. These included: broken end-plates on hot lines; agglomeration of ac- ceptor in the regenerator; plugging of the venturi at the entrance of the regenerator overhead gas to the quench tower. Heater tubes contin- ued to deteriorate from sulfur corrosion despite maintaining lower heater tube temperatures. heater. The run terminated when a tube ruptured in the regenerator air 152 2 DISCUSSION 2.1 INTRODUCTION Prior to Run 8, after thorough review of Run 7, the following changes were agreed to: (1) Dolomite was to be used instead of local limestone. (2) Quench systems were to be started just before recycle com- pressors were started. This was to help prevent dried solids in the system from getting to the compressors during startup. (3) Three batches of dolomite were to be half-calcined in the gasifier and transferred to the regenerator to provide a heat sink. The feed from both the gasifier and the fresh dolomite lockhopper were then to be continued. (4) Steam flow was to be established at the gasifier transition through the new distributor ring with no recycle gas. This was to be done before char addition. (5) Reaction temperature of 1500° F in the gasifier was to be obtained by controlled air introduction through the gasifier char bed for partial combustion of char. This was to assist in reducing char density sooner, to aid showering of cal- cined dolomite. 2.2 OPERATING SEQUENCE Run 8 was initiated Tuesday, March 27, 1973. Startup was normal except for a pause of about 5 hours in the heatup procedure at 250° F to allow curing for refractory repairs. A plug between the regenerator overhead cyclone and the "A" ash lockhopper resulted in a temporary depressuring for unplugging. Dolomite acceptor was heated to "half- calcined" temperature and circulation was established on March 30. Transfer of dolomite from the gasifier to the regenerator was blocked, so the gasifier was dumped to the purged dolomite lockhopper in an attempt to "shake up" the transfer system. This was unsuccessful, so the system was shut down. On March 31, it was found that the end plate on the flange at the top of the engager pot had broken, allowing the inner tube to slide down and block the flow. This was repaired and operation was resumed March 31 Pressuring, establishing gas flow, and heating were started March 31 and accomplished April 1. Then dolomite was added to the gasifier and transferred to the regenerator. A dolomite bridge in the gasifier was broken by lowering gas flow to the boot and increasing gas flow to the side of the gasifier. After a small inventory of dolomite had been established in the regenerator, dolomite was added directly from the dolomite lockhopper. Steam was fed to the transition (sideflow) distributor in the gasifier. Ground char was fed through the preheater to the gasifier. 153 By April 3, desired dolomite and char levels had been established in the regenerator and gasifier. Air was then fed with the steam to the gasifier to augment gasification of the char and lower char density, to allow for easier showering of dolomite through the char bed. Char samples were obtained while making brief transfers of char to the regen- erator. Char density seemed high, perhaps because of the presence of dolomite in the char bed. Some dolomite was removed from the boot to the purged dolomite lockhopper, gas flows were varied, char inventory was first increased then decreased by dumping to the purged dolomite lockhopper, all in an attempt to decrese the holdup of dolomite in the char bed. These actions accomplished a reduction in char bed density. Air was introduced to the regenerator, and natural gas was added to start calcination. Next char was transferred from the gasifier to the regenerator with some difficulty. Accomplishments on April 3 were: (1) Char bed density was reduced to tlie desired level. (2) Char was transferred (not smoothly) from gasifier to regenerator. (3) Dolomite acceptor was calcined. (4) Acceptor was circulated. Late that night problems developed with acceptor circulation. The solid seal above the valve in the transfer line from regenerator to gasifier was lost and not regained. Also, differential pressures in the regen- erator indicated probable agglomeration in the bed. On April 4, the plant was shut down and cooled so the top head of the regenerator could be removed for inspection. There was a 1/2-inch coating of yellow acceptor over the entire surface of the regenerator, the side- taps, and the transfer lines. There was also a considerable amount of agglomerate in the bottom of the regenerator. This material was cleaned out and the plant returned to operation April 17. During the next part of Run 8, operating conditions were altered to maintain a reducing atmosphere in the regenerator, in an attempt to avoid agglomeration in the regenerator. New controls were installed on both air and char feed to the regenerator. Air feed could be controlled either for a specific flow or to maintain a specific carbon monoxide concentration in the regenerator overhead gas stream. The char feed was controlled by maintaining a constant differential pressure across the char lift line. Immediately after startup on April 7, there was a high pressure drop across the venturi in the overhead gas line from the regenerator to the quench tower. There was a brief shutdown to clean out this restriction. By April 10, the regenerator was full and pregasified char from the April 4 dump was fed to the gasifier. (A high differential pressure across the baghouse prevented use of the preheater.) 154 While operating, new differential pressure recorders were in- stalled across the char and spent acceptor control valves. During this installation, all the acceptor in the gasifier boot, together with some char, were accidentally transferred to the regenerator. The acceptor- char interface could not be reestablished, so the gasifier was dumped. In attempting to switch the gasifier sideflow from steam to recycle gas for the dump, the system pressure dropped when the steam was cut off. After several switching attempts, the side flow was cut off completely, because either the feed line or the distributor ring had plugged. Late on the 10th, the regenerator air heater went out. On attempt- ing to relight the heater, a ruptured tube was discovered. (This explain- ed the system depressuring noted above.) The plant was shut down, terminating Run 8. 2.3 OPERATING CONDITIONS Typical operating conditions are shown in Tables 8-1 and 8-2. Table 8-1 shows conditions for April 2, 1973, when acceptor was circu- lating but there was no char in the system. Table 8-2 shows conditions for April 3 with char in the system. These data are for the brief period when operating conditions were nearly those desired for a full demonstration of gasification. At this time: (1) Char bed density was reduced to the desired level. (2) Char was being transferred from the gasifier to the regenerator. (3) Dolomite acceptor was fully calcined. (4) Acceptor was being circulated. 2.4 CHAR AND ACCEPTOR DATA Table 8-3 presents char data for this run. Average size distri- butions are given for fresh char feed and for char dumped from the gasifier. Analyses are given for two composites of fresh char and one composite of material dumped from the gasifier. Table 8-4 presents dolomite acceptor data for the run. Size distributions are given for average fresh acceptor feed; process samples taken from two locations on April 2, 1973, when there was no char in the system; two samples from the same locations on April 3, when there was char in the system; and a composite of material dumped from the regen- erator. The April 2 and 3 samples coincide with the operating condi- tions shown in Tables 8-1 and 8-2. Dolomite acceptor compositions are also given in Table 8-4 for fresh acceptor, material dumped from the regenerator, and the yellow shell or skin material on agglomerate spheres removed from the regenerator. 155 2.5 ACCEPTOR CIRCULATION Figure 8-1 is a time chart of regenerator temperature, equil- ibrium partial pressure of carbon dioxide for the calcination reaction, and actual carbon dioxide composition. This chart is similar to Figure 7-1 m the report on Run 7, and again shows that dolomite acceptor was rully calcined. ^ 2.6 GASIFICATION DATA Gasification data obtained on April 3 and 4 are shown in Figure 8-2, a time chart of important variables. Shown are flows, temper- atures, char feed, and composition of the gasifier overhead gas stream. As in similar charts of Run 6 and 7, some responses of gas composition to temperature, flow, and char feed are obvious and expected ""'P^''^'^" '° 156 STARTUP PROCEDURE FOR RUN 8 (1) (2) (3) (4) (5) (6) Pressure test at 150 LBS. Establish flows as follows Inert Gas Boot, Recycle Total, Recycle Char Lift Gas, I.G. Air Line, Recycle Lift Gas, Recycle Gasifier FRC-2126 FRC-2019 FRC-2020 Regenerator FRC-2015 FRC-2113 FRC-2014 5,000 SCFH 37,000 SCFH 57,000 SCFH 7,000 SCFH 50,000 SCFH 50,000 SCFH Bring quench systems on prior to heatup. Heat up system. Maintain B-204 outlet at 1050 F and set all other heater out- lets at 1600 F. Heat both reactors to 1300° F. During heat up, follow Resco procedure to cure new refractory in both vessels. Check low spots in system and drain any accumulated water. Set maximum recycle capacity and air to give 137,000 SCFH. Flows Lift, Recycle Air, Recycle Char Lift, I.G. Maintain heater outlets at 1600 F 90,000 SCFH 40,000 SCFH 7,000 SCFH Charge acceptor inventory to gasifier boot. Hold to allow bed to half calcine (1300 F) and then transfer to regenerator. Feed three batches to the regenerator before starting F-206 feed. Be sure to sample all tote bins and record charged weights and feeder RPM. Include time and notation of RPM changes. 157 4 DETAILED OPERATING INSTRUCTIONS FOR RUN 8 On March 26 and 27 meetings were held between Consol and Stearns- Roger concerning Run 7 and the plans for the next plant run. Run 8 The following procedure includes tests outlined in the meetings as well as previously established operations. 4.1 PRELIMINARY CONDITIONS AND INFORMATION (1) Initial steps will include the heat curing of the regenerator and gasifier refractory patching. (2) No air flow from J-202, the regeneration air compressor, is to be used initially. (3) All dPT's and dPR's are to have been zeroed per revised SK-245 . (4) All Moore regulators are to be bypassed. (5) All purges in service are to be at a reading of 2 during initial stages of pressurization and be at a reading of 7 when up to operating pressure except the following: FI SETTING FI SETTING 2154 3.5 2041 20 2153 3.5 2038 20 2152 3.5 2036 20 2278 20 2096 20 2277 20 2098 20 2276 20 2213 20 2275 20 2100 20 2280 20 2102 20 2104 20 During pressure testing and pressuring of system, bring all purges up slowly to values indicated above as system is brought to test or operating pressure. (6) Keep sample points open (not plugged) and dry. (7) Keep ash lockhoppers, F-207A/B, and purged dolomite lock- hopper, F-213, dry. Check often during initial startup phases. (8) Keep other low points in the system dry. (9) We will be using dolomite during this run. 158 4 . 2 PROCEDURE (1) Pressure test the reactor systems to 150 PSIG with inert gas in 25-PSI steps. Hold at each plateau and check for leaks. Do not go to 175 PSIG since PSV-2014 is now set at 175 PSIG to protect L-202. (2) Unless already done, fill the regenerator quench tower, gasifier quench water separator, and the foul water strip- per water separator to operating levels with boiler feed water. Fill the piping, regenerator, and gasifier jacket systems if not already filled. Start circulation of jacket systems and begin chemical treatment of the water. Do not start steam to the regenerator and gasifier jacket systems at this time. Do not pressure the gasifier steam drum with inert gas at any time. Minimize water to jacket of gasifier overhead line. With steam in the gasifier. we want the inlet to the quench tower between 400 and 500 F. (3) Fill seal leg on steam line from gasifier steam drum. (4) With the reactor system at 150 PSIG static pressure with inert gas, set FIC-2126 at 5,000 SCFH (inert gas) and set PRC-2113 at 390 PSIG (to obtain the total output of J-309 to FR-2015). (5) Line up PCV-2022 (PRC-2022 at 150 PSIG on automatic), PCV- 3009 A (with PRC-3009 at 100 PSIG on automatic), dPCV-2030-1 (dPRC-2030 at zero on manual), and PCV-2071 (with PRC-2071 at 80 PSIG on automatic) for normal operation. NOTE: PCV-3009A is the new small valve in parallel with PCV- 3009. In connection with PCV-3009A, a new small orifice FE-3000A is used. (6) Block in FCV-2032, FCV-2014 and FCV-2113. (7) Close XCV-2024 on manual. (8) Block in regulators on A and B purge systems from dryers. (9) Start circulation of gasifier and regenerator quench water systems. Line up SO scrubber and start its circulation Start J-201A/B compressors. Set PRC-2052 at 250 PSIG. (10) Start J-207A/B compressors. Set PRC-2041 at 250 PSIG. Be sure J-207A/B are lined up in parallel with J-203A/B. Start J-203A/B compressors. (11) On "A" and "B" dryers, open the valves to vent a few turns to put some load on the dryers. Check out the performance of each dryer with respect to dewpoint at least through one cycle of each chamber. When the dewpoints can be main- tained at least below -20° F, continue with this procedure. 159 (12) The regulators on the "A" and "B" systems are set at 200 PSIG. Be sure these settings are maintained. Activate these regulators and close XCV-2070 and XCV-2072. Both dryers will then take over the supply to the purge systems. (13) Recheck all rotameter settings. (14) Adjust all other rotameters to be in use in the structure. (15) Leave LCV-2003, LCV-2002, XCV-2073, TCV-2030 open with valve kickers deactivated. (16) With dPRC's on manual, establish maximuin flows through dPCV- 2026, 2036 and 2037. (17) Open XCV-2010 if it is not already open. (18) Set PIC-2047 at 200 PSIG on automatic. Open XCV-2024 if it is not already open. (19) Establish the following flows: (a) FIC-2126 5,000 SCFH (inert gas) to discharge of J-201A/B (b) FRC-2020 at maximum compressor capacity to B-201 A/B from J -201 A/B (c) Maximum of 40,000 SCFH through FR-2260 with balance through FIC-2019 (d) FRC-2015 Total output from J-309 to B-204 (inert gas) (e) FRC-2032 40,000 SCFH (recycle) to B-203 from J-203A/B and J-207A/B (f) FRC-2014 90,000 SCFH (recycle) to B-205 from J-203A/B and J~207A/B (g) FRC-2113 SCFH (air) to B-203 from J-202 (h) FRC-2013 SCFH (air) to B-201B from J-202 (i) FRC-2021 SCFH (steam) to B-201 (20) When the oxygen content of the recycle gases is less than 2 percent, start the process heaters. Use the following procedure for curing the new refractory in the reactors: (a) Establish 250° F in both the regenerator and gasifier at a rate of 50^ to 75° per hour. (b) Maintain 250° F for 5 hours at pt . 44. 160 (21) B-203 and B-205 are then to be brought to 1600° F final heater outlet temperatures and B-204 is to be brought to 1051° F. B-201 2A/1A and 2B/1B are to be brought to 1600° F final heater outlet temperatures. Raise all heater final outlet temperatures at an even rate of 200° F per hour until 1000° F is reached. Then raise temperatures at a rate of 100° per hour until the final outlet temperatures are reached. Adjust dampers and registers for proper heat combustion by stack analyses. Monitor final furnace outlet tubes with optical pyrometer every 4 hours. Monitor new pencil thermocouples in B-201 lA and IB outlet headers for unequal readings which would indicate an unequal gas flow through the heater tubes. (21a) When heater final outlets reach 700° F, start steam to the regenerator and gasifier jacket water steam drums. Hold regenerator steam drum at 200° F and the gasifier steam drum at 330° F. (22) When the reactors have reached 1000° F, close LCV-2003, LCV-2002, XCV-2073, and TCV-2030, but stroke them once per shift until we have solids in the system. (23) Hold at step 21 final heater conditions until the reactors have either attained a temperature of 1300° F each or the reactor temperatures have lined out whichever occurs first, Start hourly readings at this time. (24) Conduct regenerator flow tests to determine the maximum capacity of the recycle compressors. (25) Start the preheat er furnace, B-102, and warmup the pre- heater, D-101, to between 500 and 600° F. (26) With the regenerator and gasifier at 1300° F, establish the following flows in the regenerator: (a) FRC-2014 90,000 SCFH (recycle) (b) FRC-2032 40,000 SCFH (recycle) (c) FRC-2113 SCFH (air) (d) FR-2015 Total output of J-309 (inert gas) Maintain heater outlets as follows: B-203 at 1600° F, B-204 at 1050° F and B-205 at 1600° F. (27) Charge one lignite lockhopper with 2,000 pounds of 6 X 16 dolomite. Can be done earlier. (28) Crack open LCV-2003 by manually setting 5 PSI output on ij IC — /003 . 161 (29) Add dolomite to the gasifier from the lignite lock- hopper to a reading of 60 lines on dPR-2035. Start water sampling per Run 7 where applicable. Initiate other sampling schedules when applicable. (30) Set dPRC-2037 on automatic. (31) Start filling the regenerator as follows: (a) Batch feed from the gasifier. When the boot temper- ature recovers to 1300° F. This will calcine the magnesium portion of the dolomite. (b) Transfer to the regenerator with LIC-2003 on manual . Do not lose seal above LCV-2003 at any time. (c) Transfer down to a reading of 20 lines on dPR-2034 (d) Refill gasifier boot to 60 lines on dPR-2035 and re- peat "a" through "c" above. (32) When 3 batches of half-calcined acceptor have been trans- ferred from the gasifier, start feeding from F-206 with L-204. Prepare tote bins with 2,000 of acceptable ground 6 X 16 dolomite and charge F-206 with two 2,000-pound batches each time. When grinding dolomite, sample every 500 pounds for composite samples to lab. Feed from F-206 to the engager pot and thereby to the regenerator. Feed at a rate which allows the regenerator temperature to stay above 1100 F. Feed only until the low level alarm comes on before recharging F-206. Keep accurate records of feeder RPM and the time of feeding. Note any RPM changes and record the time of each change. This is very important. Keep complete records of all materials in and out of the reactors. Continue batchwise transfers of half-calcined acceptor from the gasifier also. Be sure each batch from the gasifier has been half-calcined before transferring to the regenerator, (33) When each of the following dPR's lift, note the time on the respective chart. Read and record on all dPR's: dPR-2074 dPR-2075, dPR-2076, dPR-2077. (34) Continue feeding until dPR-2077, equals dPR-2076. This will indicate about 25 feet of acceptor in the regenerator. (When dPR-2077 lifts, we will then have a seal above TCV-2030. Set dPRC-2026 on automatic.) Have both lignite lockhoppers empty when the operating level in the regenerator has been reached. Stop feeding from F-206 if necessary to be sure lignite lock- hoppers will be empty. 162 (35) When the regenerator acceptor bed has been established, set dPRC-2030 (using dPCV-2030-1) on 5 PSI . Set dPRC- 2026 on automatic. (35a) While continuing this procedure, fill the preheater to indicate 15 lines on dPR-1002 in preparation for intro- ducing char to the gasifier. Use steam in the preheater. Maintain a flow of 40,000 to 60,000 SCFH through the preheater. (36) Circulate acceptor for 2 to 3 hours to prove integrity of the system and to test and operate controller, LIC-2003. Check all instruments and other equipment for proper operation or problems. Obtain solids samples frum sampling points in order to test the sample collection systems. During this circulation, reduce B-201-1A, final outlet to 1150° F at 100° to 150° F per hour. Note: During the circulation of acceptor, be sure the temperature in the regenerator and gasifier are maintained at 1300° F or above in order to assure that the acceptor remains in the half -calcined state. Obtain solid samples from S-9 and S-10 for percent MgO. (37) Establish the incipient fluidizing velocity of acceptor in the gasifier boot without circulating acceptor. (38) With the incipient fluidizing velocity established in Step 37 maintained in the gasifier boot, establish a flow of 40,000 SCFH of steam to the side flow of the gasifier. The side flow is to be 100 percent steam with no recycle. The new piping configuration allows this to be accomplished with the steam flow rate being controlled by FRC-2021. The recycle gas flow to the gasifier boot will be controlled by FRC-2020. In order to establish the steam flow through the gasifier side, it will be necessary to open PCV-2047 fully. It will also be necessary to open fully FCV-2019 in order to use FRC-2020 on control. If, however, FRC-2020 does not operate properly, control of the boot flow will have to revert to FIC-2019. In order to do this, PRC-2052 will have to be set at 230 PSIG because PSV-2056 is now set at 250 PSIG. The above will be accomplished by adjustment of gas flows. (39) Check the oxygen content of the gasifier recycle gas to be sure it is less than 2 percent. When this is obtained, load char from the preheater to the lignite lockhoppers to the gasifier. Start filling the gasifier with char continuously at a minimum RPM. However, do not allow the char temperature in the gasifier to fall below 900° F. When dPR-2031 lifts, resume acceptor circulation with a 6 to 7 PSI loading on TCV-2030 and with LIC-2003 on automatic. Continue to fill the gasifier until a dP is shown on dPR-2033. We will then have a 25-foot char bed. When this occurs, have both lignite lockhoppers empty. Fill gasifier to the nearest lockhopper. 163 (40) In order to establish reaction temperature of 1500° F in the gasifier, air will be introduced to the gasifier for combustion with some of the char. The air will be introduced to the side flow along with steam and will be controlled by FRC-2013. Establish 10,000 SCFH of air to the gasifier side flow while reducing the steam in the side flow to 30,000 SCFH. As the air flow is established in the gasifier, the inert gas through FIC-2126 can be stopped. As combustion in the gasifier proceed^:, the temperature will rise. Control the gasifier temperature at 1500° F by adjusting the air flow. The reaction of steam and char at these elevated temp- eratures will reduce the density of char bed. The require- ment is a density of 25 to 33 pounds per cubic feet as read from dPR-2031. (41) During the density reduction phase of gasification, transfer char for sampling purposes through LCV-2002 at a 7-PSI load- ing for five minutes so that a sample can be obtained at LCV-2002 sample station. Then add approximately 10,000 SCFH of air briefly through FRC-2113. When the CO content of the regenerator overhead gas falls to about 1 percent or so, re- admit air to the regenerator and maintain less than 0.5 per- cent oxygen in the regenerator overhead. (42) This step is the calcination of the acceptor. Establish a minimum circulation of acceptor through the gasifier during calcination. Add char by means of a set flow on LCV-2002 (about a 6-PSI air loading) . Add air to burn char in the regenerator to maintain a CO content in the regenerator over- head of from 2 to 6 percent. The target value is 3 percent. The heat input to the regenerator by combustion is to be about 4 million BTU per hour. Therefore, the char combus- tion will be supplemented with natural gas combustion. A maximum of 40,000 SCFH of air is to be used with natural gas being added to maintain the CO content in the regenerator through FRC-2013. Reduce the amount of recycle on a one to one basis. We will also probably want to reduce the air pre- heat through B-203 during calcination. (43) The controls we have for maintaining the regenerator temp- eratures are: recycle and regeneration air heater temper- atures, the amount of air, the amount of natural gas and the amount of char. (44) The final objectives of gasification are to have the regen- erator at 1850° F maintaining a 25-foot acceptor bed, burn- ing char and not natural gas. The gasifier objectives are a temperature of 1500° F, a 25-foot char bed level and with no air to the gasifier. 164 (45) The foregoing procedure is a guide for realizing the gasification objectives. The critical portions of this procedure will be monitored on shift by Consol and Stearns engineers. The Shift Superintendent is to keep informed of all phases of this procedure and will make the operating decisions using the Consol and Stearns-Roger engineers as consultants. Any changes and their effects on the opera- tion, as well as the effects of going from step to step, are to be discussed by the Shift Superintendent, the Consol engineer, and the Stearns-Roger engineer on duty and this information is to be relayed to the controlman. We will attempt to minimize the number of people giving instruc- tions directly to the controlman. We will attempt to es- tablish the course of action before giving specific instruc- tions. This should result in a smoother operation. 165 5 MODIFICATION TO RUN 8 PROCEDURE TO MAINTAIN A REDUCING ATMOSPHERE IN THE REGENERATOR It is desired to keep a reducing atmosphere in the regenerator. The objective is to keep the CO content above 4 percent at all times while burning char in the regenerator. The steps outlined in this letter will be used to supplement the previously published program for Run 8. Steps 41, 42, and 43 are to be modified according to the information presented below. Two new control loops have been installed: (1) Char addition to the regenerator from the gasifier will be controlled by the input to dPR-2027 and dPR-2028. (2) Air addition to the regenerator will be controlled by the CO analyzer output. A detailed description of the system will be issued today. When char feed to the regenerator stops, air must be removed immed- iately. If recycle gas and air are on B-203, the excess air plus CO in the recycle plus a heater temperature of above 1400° F will cause burning in the heater. Therefore, with air and recycle gas through B-203 (see step 42) keep B-203 below 1400° F. With air only through B-203, have the heater off since the controller could reduce the flow below the low flow shut down rate. After establishing char feed and burning in the regenerator with the CO content above 4 percent then: (1) Reduce total gas flow to the regenerator and maintain a superficial velocity of not more than 1.8 FT/SEC in the regenerator. Also, reduce B-203 and B-205 temperatures to about 1050 to 1100° F for better char combustion in the bottom of the regenerator. (2) If char feed is lost, even for a minute (60 SEC) : (a) Push EHS-2002 to close LCV-2002. (b) Shut off air or at least reduce air flow to approxi- mately 10,000 SCFH. (c) If B-203 is being fired with recycle gas in the heater, increase recycle gas to prevent low flow shut down of B-203. Some flow is needed through B-203 so that solids do not enter the holes in the distributor in the regenerator. (d) Increase the flow of natural gas quickly to produce CO and heat. (e) Increase the air flow to bring CO back into control (4 percent CO minimum) . 166 (f) Reestablish char feed to regenerator by whatever means necessary. (g) Line out system again on char to regenerator, and slowly remove natural gas flow, etc. (h) REMEMBER: KEEP CO ABOVE 4 PERCENT AT ALL TIMES WHILE BURNING. ALLOW NO OXYGEN TO SHOW UP IN THE REGENERATOR OVER- HEAD GAS. 167 3 r:r*2igL C) o if) ■*- =3zinl-vaadv«aL 3o\s:imw^'=p-^zi OS 1- 00 o HI CO > CO (H •J i-i tu s a. u W cu u w a: CO CO m cu •J < a. r>i o u I 00 0) •H 168 NO CHAR IN SYSTEM GASIFIER FLOWS - SCFH STEAM RECYCLE INERT TOTAL 42,400 42,400 BOOT RING TOTAL 24,000 18,400 42,400 REGENERATOR AIR RECYCLE INERT NATURAL TOTAL AIR INLET ACCEPTOR LIFT CHAR LIFT TOTAL ir,ooo MOO 124, ,100 33, S3, ,000 ,500 ,200 124,000 TEMPERATURES - °F BOOT 1270 BOTTOM 1250 MIDDLE 1145 TOP 1090 BOTTOM MIDDLE TOP OUTLET 1290 1290 1275 1225 DENSITIES - LB/CU FT BOOT 62 ACCEPTOR BED 70 - 85 VELOCITIES - FT/SEC BOOT 1.11 ACCEPTOR BED 1.756 COMPOSITIONS OF OVERHEAD GAS - MOL. % CO CO2 N2 CH4 H2S SOo TRACE O2 CO 11.4 C02 88.6 N2 CH4 H2S SOo 0.5 15.6 83.9 Table 8-1. GAS FLOWS, COMPOSITIONS, INDICATED BED DENSITIES AND TEMPERATURES FOR RUN 8, APRIL 2, 1973 170 GASIFIER FLOWS - SCFH AIR 19,800 STEAM 40,200 RECYCLE 29,700 INERT TOTAL 89,700 BOOT 29,700 SIDE 60,000 TOTAL 89,700 CHAR BED ESTABLISHED IN GASIFIER AT 26.5 FEET REGENERATOR AIR RECYCLE INERT NATURAL GAS TOTAL 9,100 118,700 7,100 134,900 AIR INLET ACCEPTOR LIFT CHAR LIFT 40,700 87,100 7,100 134,900 TEMPERATURE - "F BOOT 1105 BOTTOM 1490 MIDDLE 1410 TOP 1280 BOTTOM MIDDLE TOP 1320 1320 1315 COMPOSITIONS OF OVERHEAD GAS - MOL. % 02 CO 0.0 12.3 C02 N2 "2 19.8 34.4 29.4 CH4 H2S 3.8 0.3 SO2 0.0 VELOCITIES - FT/ SEC BOOT 1.28 CHAR BED 0.95 02 CO C02 N2 H2 CH4 H2S SO2 0.0 3.3 9.3 87.0 0.4 0.0 0.0 0.0 ACCEPTOR BED 1.96 DENSITIES - LB/CU FT BOOT CHAR BED 70 45 ACCEPTOR BED 70 - 80 Table 8-2. TYPICAL GAS FLOWS, COMPOSITION, AND TEMPERATURES FOR RUN 8, APRIL 3, 1973 171 SIZE DISTRIBUTION MESH SIZE 10 14 20 28 35 48 65 100 200 PAN AVERAGE CHAR FEED tr 0.4 1.4 5.1 10. 1 15.8 16.4 15.6 10.8 7.5 9.7 7.2 AVERAGE CHAR DUMP 0, .1 1, .0 4, .4 9, .5 15, .2 17, .4 16. .2 16. ,1 10. ,6 5. ,8 2. ,7 1. ,0 CHAR ANALYSIS - WEIGHT PERCENT FRESH FRESH GASIFIER char(U CHAR(2) DUMP(3) VOLATILE MATTER 14.9 13.9 5.2 C 73.4 74.3 73.7 H 2.3 2.2 0.7 N - - - S 2.4 1.7 0.2 ASH 18.4 16.0 22.7 CaO 19.5 21.4 38.2 MgO 6.4 6.8 12.8 Na20 2.1 2.6 3.4 Si02 31.3 22.9 9.5 SO3 19.9 25.0 3.4 R^O AI2O3 10.3 12.1 28.8 Ti02 0.3 0.4 0.6 FE2O3 9.0 5.4 1.5 P2O5 0.03 0.03 K2O 0.5 0.4 0.5 HEAT CONTENT - 11,850 BTU PER POUND (1) (2) (3) COMPOSITE OF 3-30-73 to 4-11-73 COMPOSITE OF 3-28-73 to 3-30-73 COMPOSITE OF 4-5-73 to 4-6-73 Table 8-3. CHAR DATA FOR RUN 8 172 DATE ; TIME SAMPLE LOCATION; MESH SIZE AVERAGE ACCEPTOR FEED A 6 8 9,3 9 16.2 10 16.7 12 14.5 lA 16.0 16 12.8 20 11.4 24 2.4 28 0.4 PAN . 3 ACTIVITY BULK DENSITY - LB/CU FT PARTICLE DENSITY - LB/CU FT 4/2/73 1200'V S-9 TCV-2030 5.7 16.8 18.7 16.0 17.8 13.0 9.0 2.2 0.5 0.3 0.99 66 133 4/2/73 1200* S-10 LCV-2003 4.4 13.6 16.1 14.5 16.3 13.7 12.0 4.6 1.8 3.0 67 129 4/3/73 1600** S-9 TCV-2030 8.8 17.4 19.0 15.2 15.4 10.7 8.3 3.0 1.4 0.8 1.0 71 130 4/3/73 AVERAGE 1600** REGEN- S-10 ERATOR LCV-2003 DUMP 6.9 15.4 18.9 16.6 18.1 12.4 8.6 2.5 0.5 0.1 70 130 tr 0.9 3.8 9.3 21.8 26.4 27.0 7.9 1.7 1.2 COMPOSITION - WEIGHT PERCENT CaO MgO Na20 Si02 SO3 R^O AI2O3 Ti02 FE2O3 P2O5 K2O ACTIVITY FRESH ACCEPTOR 61.5 25.7 0.05 7.9 0.49 1.2 0.04 0.69 0.01 0.08 1.0 (1) REGENERATOR YELLOW SHELL FROM DUMP REGENERATOR SPHERE 68.2 63.8 17.7 21.5 0.1 0.08 9.8 4.6 0.65 0.2 1.67 0.9 0.0 0.0 0.8 0.8 0.02 0.01 0.01 0.04 0.38 0.22 *N0 CHAR BED **CHAR BED HEIGHT, 26.5 FT ^ ^COMPOSITE OF 3-30-73 to 4-4-73 Table 8-4. ACCEPTOR DATA FOR RUN 8 173 RUN 9 APRIL 14 to APRIL 19, 1973 CO2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 174 FOREWORD Run 9 began April 14 and terminated April 19, 1973. There were no significant changes in the objectives or procedures from Run 8. During the required shutdown to repair heater tubes, a new ring-type gas dis- tributor, similar to one installed earlier in the gasifier transition section, was installed in the regenerator. This change seemed signif- icant enough to identify it by a new run number, rather than designate it as a continuation of Run 8. No new general operating instructions were written for Run 9. Detailed operating instructions constitute Section 3 of this run report. This report records the events of Run 9 and presents the signif- icant data obtained. 175 1 SUMMARY This brief run was rather uneventful. It started April 14; by April 18, operating conditions approaching those desired for a full gasification demonstration were achieved. Mechanical problems encount- ered April 19 caused plant shutdown and termination of Run 9. The significant achievement of the run was that, for the first time, transfer of char from the gasifier to the regenerator was smooth and relatively trouble-free. New automatic controls had been installed for the transfer systems. These control the char feed rate as a func- tion of the char transfer line pressure drop, the two variables having a nearly linear relationship. The control system worked well, giving a smooth char feed. Significant achievements realized in earlier runs were repeated, including: (1) pregasification of char with both steam and air, and rapid reduction of char bed density, (2) full calcination and circula- tion of acceptor, and (3) balanced combustion of both char and natural gas in the regenerator to maintain desired calcination temperature. Termination of the run on April 19 resulted from plugging of heater tubes with iron-nickel-sulfide deposits, and plugging of the regenerator-to-gasifier acceptor transfer line. 176 2 DISCUSSION 2.1 OPERATING SEQUENCE Run 9 started the afternoon of April 14. There was a brief depressuring to fix a leak. Dolomite addition was started on the 15th and the preheater was started in preparation for char feed. Dolomite acceptor level was established and circulation tested on the 16th. After these tests, acceptor circulation was stopped, boot flow was reduced, and steam was fed to the transition section of the gasifier. Char was fed through the preheater, but the interface could not be maintained, so the gasifier was dumped. Acceptor level in the boot and char level in the gasifier, with an interface, were established April 18. Char bed density was reduced to about 35 pounds per cubic foot by partial gasification with steam and air. On the 18th, the following conditions were established: (1) Air and steam were fed to the transition section of the gasifier. (2) Recycle gas and steam were fed to the gasifier boot. (3) Acceptor was circulated between the regenerator and gasifier, (4) Air, char, and natural gas were fed simultaneously to the regenerator. (5) Char feed from the gasifier to the regenerator was on automatic control. Several problems developed on the 18th. The gas feed line to the side of the gasifier developed two hot spots, 500° F and 1100° F, indi- cating internal breakage. The filter on the gasifier recycle gas com- pressor plugged and had to be bypassed. High pressure drop developed across the gasifier recycle gas heater, indicating probable coking in the tubes. Finally, late that night, acceptor circulation from the regenerator to the gasifier stopped and could not be reestablished. Operations were maintained until the 19th to establish an inven- tory of partially gasified char for use in the next run. The plant was then shut down and the regenerator dumped on the 20th, terminating Run 9. When the regenerator was dumped, several balls of agglomerate rang- ing from 1/4 inch to 1 inch in diameter were found. 2.2 OPERATING CONDITIONS Operating conditions for April 16, 1973, when there was no char in the system, are recorded in Table 9-1. 177 Operating conditions for April 18, when the system was close to the conditions desired for a demonstration gasification run, are record- ed in Table 9-2. 2.3 CHAR AND ACCEPTOR DATA Char and acceptor data for Run 9 are recorded in Tables 9-3 and 9-4 respectively. 2.4 ACCEPTOR CIRCULATION Figure 9-1 is a time chart for the five days April 15 through 19 of regenerator temperature, air flow to the regenpr^tor, equilibrium carbon dioxide partial pressure and actual carbon dioxide partial pres- sure. As in the equivalent charts for Runs 7 and 8, it demonstrates that full calcination was achieved. 2.5 GASIFICATION DATA Gasification data obtained on April 18 and 19 are shown in Figure 9-2, a time chart of important variables. Shown are flows, temperatures, char feed, and composition of the gasifier overhead gas stream. As in similar charts of Run 6 and Run 7, some responses of gas composition to temperature, flow, and char feed are obvious and expected. 178 3 DETAILED OPERATING INSTRUCTIONS FOR RUN 9 The run started on April 14, 1973, is designated as Run 9. The main difference from Run 8 is the installation of a ring distributor on the regeneration air line similar to the distributor ring on the side flow to the gasifier. Several new dPT's have been installed and auto- matic control of char feed from the gasifier to the regenerator has been set up. Also, automatic control of air to the regenerator has been installed. 3.1 PRELIMINARY CONDITIONS AMD INFORMATION (1) Initial steps will include the heat curing of the regen- erator bottom head joint seal. (2) No air flow from J-202, the regeneration air compressor, is to be used initially. (3) All dPT's and dPR's are to have been zeroed per revised SK- 245 (Revision 7) plus various changes requested since the sketch was issued. (a) The low side of dPT-2028 has been connected in common with the low side of dPT-2029. (b) The dPT-2020 from the regenerator probe (not in use) is now connected low side in common with the low side of dPT-2032 and high side in common with the low side of dPT-2036. (c) The dPT-2019, also from the regenerator probe, is now connected low side in common with the high side of dPT-2034 and the high side in common with the low side of dPT-2037. (4) All Moore regulators are to be bypassed. (5) All purges in service are to be at a reading of 2 during initial stages of pressurization and be at a reading of 7 when up to operating pressure except the following: FI SETTING 2154 3.5 2153 3.5 2152 3.5 2278 20 2277 20 2276 20 2275 20 2280 20 FI SETTING 2041 20 2038 20 2036 20 2096 20 2098 20 2213 20 2100 20 2102 20 2104 20 179 During pressure testing and pressuring of system, bring all purges up slowly to values indicated above as system is brought to test or operating pressure. (6) In order to include additional TE's from the gasifier on TI- 2001 near the previously existing gasifier points some changes were made on TI-2001. Be sure these changes are noted. (7) In order to control the char feed rate to the regenerator, we can utilize dPT-2028 as an indication of flow into the regenerator. We have installed a new controller in lieu of the LHC-2002 Hand Loading Station. The new controller, LIC- 2002, will be used to control LCV-2002. LIC-2002 can be used in the manual mode, permitting manual control of LCV- 2002, the same as prior to the change. Or, the valve can be controlled in the automatic mode, using dPT-2028 as a rela- tive indication of char flow rate into the regenerator. (8) The control system for valve number FCV-2113 has been mod- ified to enable us to control air flow rate to the regener- ator, utilizing CO analyzer AIT-2002. The controller, ARC-2002, can be used in the manual mode to control FCV-2113, which will manually set the air flow rate, FR-2113 (green pen), to the regenerator. In the automatic mode the flow rate will be controlled according to the CO analysis of AR-2002 or ARC-2002. As the CO content rises, ARC-2002 will cause FCV-2113 to open, allowing more air to enter the regenerator, thus reducing the CO content. This controller can easily be switched to control the air flow rate, using FT-2113 by valving in the appropriate signal to the red pen and reversing the action of the auto- matic controller. An instrument technician must be used to make this change. Also, a two range system will be installed for the input to FRC-2113 so that the recorder scale will be expanded for a low flow range. The old control on PRC-2052-1 and 2 will be used to change ranges. (9) It is desired to keep a reducing atmosphere in the regener- ator. The CO content must be kept above 4 percent at all times while burr^' .g natural gas and/or char in the regen- erator. No oxygen is to be allowed to show up in the regenerator overhead gas at any time. (10) Keep sample points open (not plugged) and dry. 180 (11) Keep ash lockhoppers, F-207A/B, and purged dolomite lock- hopper, F-213, dry. Check often during initial startup phases. (12) Keep other low points in the system dry. (13) We will be using dolomite during this run. 3 . 2 PROCEDURE (1) Pressure test the reactor system to 150 PSIG with inert gas in 25-PSI steps. Hold at each plateau and check for leaks. Do not go to 175 PSIG since PSV-2034 i- r.ow set at 175 PSIG to protect L-202. (2) Unless already done, fill the regenerator quench tower, gas- ifier quench water separator, and the foul water stripper water separator to operating levels with boiler feed water. Fill the piping, regenerator, and gasifier jacket systems if not already filled. Start circulation of jacket systems and begin chemical treatment of the water. Do not start steam to the regenerator and gasifier jacket systems at this time. Do not pressure the gasifier steam drum with inert gas at any time. Minimize water to jacket of gasifier overhead line. With steam in the gasifier, we want the inlet to the quench tower between 400° and 500° F. (3) Fill seal leg on steam line from gasifier steam drum. (4) With the reactor system at 150 PSIG static pressure with inert gas, set FIC-2126 at 5,000 SCFH (inert gas) and set PRC-2113 at 390 PSIG (to obtain the total output of J-309 to FR-2015). (5) Line up PCV-2022 (PRC-2022 at 150 PSIG on automatic), PCV- 3009A (with PRC-3009 at 100 PSIG on automatic), dPCV-2030-1 (dPRC-2030 at zero on manual), and PCV-2071 (with PRC-2071 at 80 PSIG on automatic) for normal operation. NOTE: PCV-3009A is the new small valve in parallel with PCV-3009. In connection with PCV-3009A, a new small orifice FE-3000A is used. (6) Block in FCV-2032, FCV-2014 and FCV-2113. (7) Close XCV-2024 on manual. (8) Block in regulators on A and B purge systems from dryers. (9) Start circulation of gasifier and regenerator quench water systems. Line up SO2 scrubber and start its circulation. Start J-201A/B compressors. Set PRC-2052 at 250 PSIG. 181 riO^ Start •T-2n7A/B coinp-res«;ors. Set PRC-2041 at 250 pSI*^. Be sure J-207A/B are lined up in parallel with J-203A/B. Start J-203A/B compressors. (11) Prior to startup, operate A, B and C dryers on plant air to reduce the time required to obtain acceptable dew points. With the recycle compressors in operation, open the A and B dryers vent valves a few turns to put some recycle load on the dryers. Check out the performance of each dryer with respect to the dewpoint at least through one cycle of each chamber. When the dewpoint s can be maintained at least below -20°F, continue with this procedure. (12) The regulators on the A and B systems are set at 200 PSIG. Be sure these settings are maintained. Activate these regulators and close XCV-2070 and XCV-2072. Both dryers will then take over the supply to the purge systems. (13) Recheck all rotameter settings. (14) Adjust all other rotameters to be in use in the structure. (15) Leave LCV-2003, LCV-2002, XCV-2073, TCV-2030 open with valve kickers deactivated. (16) With dPRC's on manual, establish maximum flows through dPCV- 2026, 2036 and 2037. (17) Open XCV-2010 if it is not already open. (18) Set PIC-2047 at 200 PSIG on automatic. Open XCV-2024 if it is not already open. (19) Establish the following flows: (a) FIC-2126 5,000 SCFH (inert gas) to discharge of J-201A/B (b) FRC-2020 at maximum compressor capacity to B-201A/B from J-201A/B (c) Maximum of 40,000 SCFH through FR-2260 with balance through FIC-2019 (d) FRC-2015 Total output from J-309 to B-204 (inert gas) (e) FRC-2032 40,000 SCFH (recycle) to B-203 from J-203A/B and J -207 A/ B (f) FRC-2014 90,000 SCFH (recycle) to B-205 from J-203A/B and J-207A/B (g) FRC-2113 SCFH (air) to B-203 from J-202 182 (h) FRC-2013 SCFH (air) To B-201B from J-202 (i) FRC-2021 SCFH (steam) to B-201 (20) When the oxygen content of the recycle gases is less than 2 percent, start the process heaters. Use the following pro- cedure for curing the regenerator bottom head joint: (a) Establish 250° F in the regenerator at a rate of 50° to 75° per hour. (b) Maintain 250° F for 5 hours at nt. Z^ . (c) Proceed with the gasifier heatup according to step 21 during the above curing. (21) B-201 IIA/IA and IIB/IB are to be brought to 1600° F final heater outlet temperatures. After step 20 is completed, bring B-203 to 1200° F maximum, B-204 to 1050° F maximum, and B-205 to 1400° F maximum. The rate of heatup is to be at an even rate of 200° per hour until 1000° F is reached. Then raise temperatures at a rate of 100° F per hour until the final outlet temperatures are reached. Monitor each pass of B-203 hourly during heatup, visually and with the optical pyrometer to check for hot tubes which would indi- cate plugging or uneven flow. Do not let any pass become overheated. Monitor other heater tubes every four hours with the optical pyrometer. Record results. (22) When heater final outlets reach 700° F, start steam to the regenerator and gasifier jacket water steam drums. Hold regenerator steam drum at 200° F and the gasifier steam drum at 330° F. (23) When the reactors have reached 1000° F, close LCV-2003, LCV- 2002, XCV-2073, and TCV-2030, but stroke them once per shift until we have solids in the system. (24) Hold at step 21 final heater conditions until the reactors have either attained a temperature of 1300° F each or the reactor temperatures have lined out whichever occurs first. Start hourly readups at this time. (25) Start the preheat er furnace, B-102, and warm up the pre- heater, D-101, to between 500 and 600° F. (26) With the regenerator and gasifier at the lined out temper- atures of step 24, maintain the following flows in the regenerator: (a) FRC-2014 90,000 SCFH (recycle) (b) FRC-2032 40,000 SCFH (recycle) 183 (c) FRC-2113 SCFH (air) (d) FR-2015 Total output of J-309 (inert gas) Maintain heater outlets as follows: (a) B-203 1200° F (b) B-204 1050° F (c) B-205 1400° r (27) Charge one lignite lockhopper with 2,000 pounds of freshly ground 6 X 16 domomite in preparation for step 29. (28) Crack open LCV-2003 by manually setting 5 PSI output on LIC-2003. (29) Add dolomite to the gasifier from the lignite lockhopper to a reading of 60 lines on dPR-2035. Start water sampling per Run 7 where applicable. Initiate other sampling schedules when applicable. (30) Set dPRC-2037 on automatic. (31) Start filling the regenerator as follows: (a) Batch feed from the gasifier when the boot temperature recovers to 1300 F. This will calcine the magnesium portion of the dolomite. (b) Transfer to the regenerator with LIC-2003 on manual. Do not lose seal above LCV-2003 at any time. (c) Transfer down to a reading of 20 lines on dPR-2034. (d) Refill gasifier boot to 60 lines on dPR-2035 and repeat (a) through (c) above. (32) When 3 batches of half-calcined acceptor have been trans- ferred from the gasifier, start feeding from F-206 with L-204. Prepare tote bins with 2,000 of acceptable ground 6 X 16 dolomite and, charge F-206 with two 2,000 pound batches each time. When grinding dolomite, sample every 500 pounds for composite samples to lab. Feed from F-206 to the engager pot and thereby to the regenerator. Feed at a rate which allows the regenerator temperature to stay above 1100: F. Feed only until the low level alarm comes on before recharging F-206. After feeding the material that is in F-206 at the beginning of the run, charge F-206 with the "rescreened", half-calcined dolomite removed from the regenerator on 4-11-73 and "rescreened" on 4-13-73. (Tote bins 1, 8, and 12). Feed this material to the regenerator. 184 Keep accurate records of feeder RPM and the time of feeding. Note any RPM changes and record the time of each change. This is very important. Keep complete records of all materials in and out of the reactors. Continue batchwise transfers of half -calcined acceptor from the gasifier also. Be sure each batch from the gasifier has been half-calcined before transferring to the regenerator. (33) When each of the following dPR's lift, note the time on the respective chart. Read and record on all dPR's: dPR-2074, dPR-2075, dPR-2076, dPR-2077. (34) Continue feeding until dPR-2077 equals dPR-2076. This will indicate about 25 feet of acceptor in the regenerator. (When dPR-2077 lifts, we will then have a seal above TCV- 2030. Set dPRC-2026 on automatic.) Have both lignite lockhoppers empty when the operating level in the regen- erator has been reached. Stop feeding from F-206 if neces- sary to be sure lignite lockhoppers will be empty. (35) When the regenerator acceptor bed has been established, set dPRC-2030 (using dPCV-2030-1) on 5 PSI. Set dPRC- 2026 on automatic. (36) While continuing this procedure, fill the preheater to 15 lines on dPR-1002 in preparation for introducing char to the gasifier. Use steam in the preheater. Set 16,800 SCFH of steam on FRC-1037. (37) Obtain 1300° F in the regenerator by burning natural gas. It is desired to keep a reducing atmosphere in the regen- erator overhead. Introduce about 1000 SCFH of natural gas through FIC-2028. Add air through FRC-2113 to control CO content above 4 percent. Allow regenerator conditions to line out. If necessary, increase the natural gas and air flows to obtain 1300° F in the regenerator. NOTE: When burning natural gas and/or char in the regen- erator, adjust recycle flow to B-203 to maintain a superficial velocity in the regenerator of 2 FT/SEC. (38) Conduct acceptor circulation tests of about 10 minutes duration at TCV-2030 valve air loadings of 6, 7, 8, 9, 10, 11, 12 PSI. Be careful not to lose the seal at TCV-2030 at the higher loadings. The higher loadings may not be attainable. After the above tests, circulate at a loading of 10 PSI for at least one hour. During these tests, check performance of controller LIC-2003. Check all instruments and other equipment for proper operation or problems. Obtain solids samples from sampling points during the 10-PSI 185 loading test in order to test the sample collection systems and test the samples for percent MgO. During the circula- tion tests, reduce B-201-IA final outlet to 1150° F and 100° F per hour. NOTE: During the circulation of acceptor, be sure the temperatures in the regenerator and gasifier are maintained at 1300*^ F or above in order to assure that the acceptor remains in the half-calcined state. (39) Stop acceptor circulation. Establish incipient fluid- izing velocity of acceptor in the gasifier boot of about 28,000 SCFH. Maintain side flow of 40, nnn SCFH. (40) With the incipient fludiizing velocity established in Step 39 maintained in the gasifier boot, establish a flow of 40,000 SCFH of steam to the side flow of the gasifier. The side flow is to be 100 percent steam with no recycle. The new piping configuration allows this to be accomplished with the steam flow rate being controlled by FRC-2021. The recycle gas flow to the gasifier boot will be controlled by FRC-2020. In order to establish the steam flow through the gasifier side, it will be necessary to open PCV-2047 fully. It will also be necessary to open fully FCV-2019 in order to use FRC-2020 on control. If, however, FRC-2020 does not operate properly, control of the boot flow will have to revert to FIC-2019. In order to do this, PRC-2052 will have to be set at 230 PSIG because PSV-2056 is now set at 250 PSIG. Careful adjustment of flows will be required to accom- plish the above. (41) Check the oxygen content of the gasifier recycle gas to be sure it is less than 2 percent. When this is obtained, load char from the preheater to the lignite lockhoppers to the gasifier. Start filling the gasifier with char continuously at a minimum RPM. However, do not allow the char tempera- ture in the gasifier to fall below 900° F. Do not resume acceptor circulation. When dPR-2032 "lifts" (shows dif- ferential pressure), add 10,000 SCFH of air to the gasifier side flow through FRC-2013 and reduce steam to 30,000 SCFH. Continue to fill the gasifier until dPR-2033 lifts. We will then have a 2S-foot char bed. When this occurs, have both the lignite lockhoppers empty. Fill the gasifier to the nearest lockhopper. (42) After dPR-2033 lifts, adjust air flow to gasifier side to obtain and maintain 1500° F in the gasifier. As the air flow is increased in the gasifier, the inert gas through FIC-2126 can be stopped. The reaction of steam and char at these elevated temper- atures will reduce the char bed density. The required density is about 30 pounds per cubic foot as read on dPR- 2031. Do not circulate acceptor during this time. 186 (43) This step is the calcination of the acceptor. Establish a minimum circulation of acceptor through the gasifier during calcination. Establish the following flows: (a) FRC-2014 at 60,000 SCHF (recycle gas) to B-205 from J-203 A/B and J-207 A/B (b) FR-2015 at total output from J-309 to B-204 (probably inert gas and natural gas at this time) (c) FR-2113 at sufficient air to B-203 from J-202 to burn natural gas from J-309 (d) FRC-2032 with the rest of the recycle gas not used in FR-2014 from J-203NB and J-207A/B to B-203. Add char by means of a flow through LCV-2002 controlled by output of dPT-2028. Add air to burn the char in the re- generator and maintain a CO content above 4 percent. As air is added through FR-2113, reduce the amount of recycle on a one-to-one basis. Also, see NOTE step 37. B-203 outlet temperature can be reduced to 1050° F for better char con- sumption. Also, B-205 outlet temperature can be reduced. (44) If char feed is lost, even for a minute (60 SEC): (a) Push EHS-2002 to close LCV-2002. (b) Shut off air or at least reduce air to about 10,000 SCFH. (c) If B-203 is being fired with recycle in the heater, increase recycle to prevent low flow shut down of B-203. Some flow is needed through B-203 so that solids do not enter the holes in the distributor in the regenerator. (d) Increase natural gas quickly to produce CO and heat. (e) Increase air to bring CO back into control (4 percent CO minimum) . (f) Reestablish char feed to regenerator by whatever means are necessary. (g) Line out system again on char to regenerator, back out natural gas, etc. (h) REMEMBER: KEEP CO ABOVE 4 PERCENT AT ALL TIMES WHILE BURNING. DO NOT PERMIT OXYGEN BREAK-THROUGH IN THE REGENERATOR OVER- HEAD GAS. 187 (45) The controls we have for maintaining the regenerator tem- peratures are: recycle and regeneration air heater temper- atures, the amount of air, the amount of natural gas and the amount of char. (46) The final objectives of gasification are to have the regen- erator at 1850O F maintaining a 25-foot acceptor bed, burn- ing char and not natural gas. The gasifier is to operate at a temperature of 1500*^ F without combustion air and maintain a 25-foot char bed level. (47) The foregoing procedure is a guide for realizing the gas- ification objectives. The critical portions of this pro- cedure will be monitored on shift by Consol and Stearns engineers. The Shift Superintendent is to keep informed of all phases of this procedure and will make the operating decisions using the Consol and Stearns-Roger engineers as consultants. Any changes and their effects on the operation, as well as the effects of going from step to step, are to be discussed by the Shift Superintendent, the Consol engineer, and the Steams-Roger engineer on duty and this information relayed to the controlman. We will attempt to minimize the number of people giving instructions directly to the control - man. We will attempt to establish the course of action before giving specific instructions. This should result in a smoother operation. 188 It^M "imm ' ^Tl\0Tiy^\Lri^U'^ , 100C? I D ill 4 5 l2oG' \l>oo I4c6' I'^cx? ^tcc \'\oa I8oo Figure 9-1. REGENERATOR TEMPERATURE, AIR FLOW, AND ACTUAL AND EQULIBRIUM C0„ PARTIAL PRESSURE AS A FUNCTION OF TIME FOR RUN 9 189 100C? iii i iii iiin i i iTT,TTnir!rritriTtiiiiii'i':Mtirtfttt-t-ntt!i t) i -mint ! 1 1 1 ii-rit i rrttT tl UtTttt m m ! M 1 1 ' l nl-rl i H : 1 1 : t-JMit-tntt^'i )8ap \'Aoa 2QQ0 '2[oo 12do 2-boo 'Uoo a\oo ozoo o^vc oAoo o'i.oc oioou cnoo TT'i::::i::.:i:;: ii:;::i. .; ii, i i i t \ . i ii.:i i ■ .iii iJi..iii....i...-i-iiiii...i....i. ^ . ^ m t_^ o6-.'0 cf\uc \ooo WOQ \2oc' \'boo \icO l^x:C \^(jo nao i&oo Figure 9-1. REGENERATOR TEMPERATURE, AIR FLOW, AND ACTUAL AND EQULIBRIUM CO2 PARTIAL PRESSURE AS A FUNCTION OF TIME FOR RUN 9 189 4n-TS -pME (Ufua-s) ♦-i»-is Figure 9-2. GASIFIER OPERATION - RUN 9 190 -pME ((Je^i^a-s) 4.-i»--75 Figure 9-2. GASIFIER OPERATION - RUN 9 190 NO CHAR IN SYSTEM GASIFIER FLOWS - SCFH STEAM RECYCLE 53,900 INERT 4,400 TOTAL 58,300 BOOT 33,600 RING 24,700 TOTAL 58,300 REGENERATOR AIR RECYCLE INERT NATURAL GAS TOTAL AIR INLET ACCEPTOR LIFT CHAR LIFT TOTAL 116,800 6,900 122,700 31,400 85,400 6,900 123,700 TEMPERATURES - °F BOOT 1175 BOTTOM 1270 MIDDLE 1155 TOP 1130 DENSITIES - LB/CU FT BOOT 65 BOTTOM MIDDLE TOP 1115 1115 1100 BED 70 - 80 VELOCITIES - FT/SEC BOOT 1.47 BED 1.580 COMPOSITIONS - MOL. % NO SAMPLES NO SAMPLES Table 9-1. GAS FLOWS, COMPOSITIONS, INDICATED BED DENSITIES, AND TEMPERATURES FOR RUN 9, APRIL 16. 1973 191 CHAR BED AT 25.5 FEET GASIFIER FLOWS - SCFH AIR 17,600 STEAM 46,100 RECYCLE 8,300 INERT TOTAL 72,000 BOOT 24,000 SIDE 47,900 TOTAL 72,000 REGENERATOR AIR RECYCLE INERT NATURAL GAS TOTAL AIR INLET ACCEPTOR LIFT CHAR LIFT TOTAL 75,100 85,700 7,100 167,900 105,500 55,300 7,100 167,900 TEMPERATURES - Op BOOT 1240 BOTTOM 1315 MIDDLE 1240 TOP 1240 COMPOSITIONS - MOL. 7, 02 0.0 CO 1.9 C02 23.2 N2 54.1 "2 17.1 CH4 3.4 H2S 0.3 BOTTOM MIDDLE TOP SO- O2 CO C02 N2 «2 CH4 H2S SOo 1745 1730 1710 0.0 3.6 21.0 75.1 0.3 VELOCITIES - FT/SEC BOOT CHAR BED 1.12 0.68 ACCEPTOR BED 3.01 DENSITIES - LB/CU FT BOOT CHAR BED 67 38 ACCEPTOR BED 65 - 78 Table 9-2. TYPICAL GAS FLOWS, COMPOSITIONS, AND TEMPERATURES FOR RUN 9, APRIL 18, 1973 192 MESH SIZE 6 8 10 14 20 28 35 48 65 100 200 PAN FRESH CHAR CHAR DUMP 0.1 0.1 0.7 1.0 2.7 4.3 8.1 10.8 13.2 17.2 17.2 21.0 14.9 16.5 13.0 13.0 8.6 7.5 5.9 4.5 6.6 3.6 9.1 0.5 CHAR ANALYSIS, WT 7. VOLATILE MATTER C H N S ASH CaO MgO Na20 Si02 SO3 AI2O3 Ti02 FE2O3 P2O5 K2O FRESH CHAR CHAR DUMP 19.0 10.1 74.5 60.74 2.1 0.97 2.1 0.2 16.6 17.7 23.9 39.43 6.3 18.86 2.8 3.17 23.1 20.80 27.2 2.14 9.86 17.83 6.12 0.45 5.8 1.86 0.03 0.08 0.4 0.56 Btu/LB 12,000 11,450 (1) COMPOSITE OF 4-14-73 to 4-20-73 Table 9-3. CHAR DATA FOR RUN 9 193 DATE : AVERAGE 4/16/73 4/16/73 4/18/73 4/18/73 AVERAGE TIME : ACCEPTOR 2230* 2210* 2000** 2000** ACCEPTOR SAMPLE LOCATION: FEED S-9 S-10 S-9 S-10 DUMP TCV-2030 LCV-2003 TCV-2030 LCV-2003 MESH SIZE 4 3.7 6 0.6 8 9.0 6.4 7.3 6.8 7.8 5.5 9 16.3 14.7 14.2 15. G 15.4 10.2 10 17.0 17.1 15.2 17.3 17.2 12.4 12 14.6 14.1 13.4 14.9 14.7 12.0 14 15.9 16.0 15.2 16.8 16.9 13.7 16 12.4 12.6 12.1 12.3 12.2 10.7 20 10.7 10.9 11.5 10.7 10.3 10.5 24 3.2 4.1 5.1 3.8 3.7 5.8 28 0.6 1.8 2.6 1.6 1.3 4.4 PAN 0.3 2.3 3.4 1.3 0.5 10.5 ACTIVITY 1.0 - - - BULK DENSITY - LB/CU FT 71 70 68 70 PARTICLE DENSITY - • LB/CU FT 134 131 131 129 ACCEPTOR ANALYSIS COMPONENT, WT 'L CaO MgO Na20 Si02 SO3 R^O AI2O3 Ti02 FE2O3 P2O5 K2O ACTIVITY FRESH . . ACCEPTOR^ ^ SMALL SPHERE REGENERATOR FROM REGENERATOR DUMP 53.1 53.6 51.5 31.6 30.4 29.8 0.07 0.48 0.23 8.7 8.0 9.7 0.97 1.41 0.22 0.42 4.9 3.01 0.0 0.2 0.04 0.7 1.5 1.1 0.01 0.03 0.03 0.12 0.06 0.12 1.0 *N0 CHAR BED ^"VCHAR BED HEIGHT, 25.5 FT ^^ ^COMPOSITE OF 4-14-73 to 4-20-73 Table 9-4. ACCEPTOR DATA FOR RUN 9 194 RUN 10 MAY 18 to JUNE 3, 1973 CO 2 ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 195 FOREWORD Run 10 started May 18, 1973, and continued through June 3, with a two-day shutdown in the middle of the run for cleanout, repairs, and revisions. As in the most recent runs, the objective was to obtain a demon- stration gasification run of significant duration. General operating instruction for the run, prepared by Consol, are presented as Section 3. Detailed operating instructions for the run, prepared by Stearns -Roger, are presented as Section 4. Major procedure changes from the previous run include revised acceptor calcination conditions and use of the Hot Potassium Carbonate System to remove carbon dioxide from the regenerator recycle gas. This report records the history of the run, the achievements made, the difficulties encountered, and significant data recorded. 196 1 SUMMARY Run 10 was a significant break through in that conditions quite close to those desired for demonstrating gasification of char were ob- tained for a significant period of time. Startup activities followed a regular course, with minimal pro- blems. May 18 through May 23. For a brief period May 23, full gasification was achieved with all operating conditions at or near those desired. Mechanical and plugging problems, however, forced a two-day shutdown. May 23 to 25. The repairs and modifications made during the shutdown are recorded in Section 5. Operations resumed May 25. From the evening of May 29 to the afternoon of June 3, a period just short of five days, conditions were again very close to those de- sired for demonstration of the gasification of char. During most of the period air was being fed to the gasifier to maintain gasifier temperature. For a period of over nine hours on June 3, air feed was removed from the gasifier and all desired conditions were achieved except that the gas- ifier bed temperature dropped from the desired 1500° F to 1400° F. The principle problem preventing full satisfaction with this demonstration run was heat input to the gasifier. The char-steam gasifi- cation reactions are endothermic . The heat required for gasification comes from three sources: (1) sensible heat removed from the 1850 F acceptor showering through the 1500 F char bed, (2) heat of reaction of calcined acceptor with carbon dioxide to form carbonated acceptor, and (3) sensible heat of the recycle gas used to fluidize the beds in the gasifier. The first source of heat met expectations with good circulation of hot acceptor from the regenerator through the gasifier and back to the regenerator. The second source was less than desired because of low ac- tivity of the calcined acceptor for recarbonation. The third source of heat was actually a heat drain on the system, because sulfur corrosion problems with heater tubes has forced maintaining a maximum heater out- let temperature of 1150 F, once the sulfur-containing char is put in the gasifier. Note: Another heat -drain was the feed of char at ambient con- ditions rather then the normal 500 F. The preheater was not used be- cause it had generated excessive char fines in recent runs. Feeding air to the gasifier was originally intended as a startup measure of short duration to speed the reduction of density of fresh char so that acceptor would shower through it more easily. During most of Run 10, air was reacted with char in the gasifier as a supplemental source of heat to maintain temperature. As noted above, when air was removed from the gasifier for over nine hours on June 3, the gasifier temperature dropped about 100 F. 197 On the afternoon of June 3, fluidization in the gasifier boot was upset and acceptor circulation was interrupted by a line plug which could not be broken. These difficulties were coincident with, but not neces- sarily caused by, addition of steam to the gasifier boot in an attempt to improve acceptor activity and gasification rate. When operating conditions could not be restored, the plant was shut down, terminating Run 10. 198 2 DISCUSSION Plans for Run 10 were reviewed and formalized at a Consol/Stearns- Roger meeting on May 15. See Section 3 for general operating instructions provided by Consol, and Section 4 for detailed operating instructions pre- pared by Stearns-Roger . 2.1 OPERATING SEQUENCE A detailed operating chronology is recorded as Section 6. A description of the operation follows. Pressure testing of the system was begun on May 18th. The heaters were lit early on the 19th after only minor leaks were found and fixed. Minor refractory repairs made during the shutdown were cured during the heatup process. Minor problems with a pump on the HPC system, the heaters on the electrical switchgear for the regenerator recycle compressor, and the preheater furnace ignitor were corrected . Dolomite was started to the gasifier (batchwise) on Sunday, May 20. An excess of fines in the dolomite stored in the sized hopper required some rescreening. This had been ground and screened to storage. Appar- ently, the fines sifted down to the bottom of the hopper. Previously, dolomite had been ground directly to tote bins and this practice has been resumed. Some problems were encountered with transferring the acceptor from the gasifier to the regenerator. Note: At the time it was suspected that fines were the problem. After shutdown, however, pieces of the gas- ifier probe supports were found in the engager pot; these pieces had to pass through the acceptor transfer line between the gasifier and the engager pot. This seems a more likely explanation of the trouble. The preheater furnace was lit on May 20th. Char fines restricted the line between the furnace and preheater; these were cleared by the next day. Dolomite was fed continuously from the fresh dolomite lockhopper starting on May 20th. Acceptor circulation was started early Monday morning, as soon as the transfer line between the regenerator and the gasifier filled. The regenerator level was increased until the vessel was filled at 10 AM on Monday. The initial filling of the reactors was slower than usual since heater operating conditions had been modified in an attempt to minimize furnace tube deterioration. Steam was introduced into the gasifier (side flow) prior to char addition. One tote bin of char was added to the lignite lockhoppers so that char feed could be started to the gasifier before the preheater was at operating level. The preheater was filled by May 22. At 6 AM on Tues- day, air was started to the gasifier for pregasification of the char. This reduces the char bulk density so that it is easier for the acceptor to shower through the char bed. By 5 PM the solids levels had been estab- lished in the regenerator and the gasifier. The regenerator was at 1650 F with the burning of natural gas and char. 199 A hot spot was detected on the acceptor lift line and was cooled with the use of steam, applied externally. On Wednesday the 23rd, several problems arose. The pressure drop across the venturi inlet to the regenerator quench tower increased quickly. Solids carry-over to the quench systems required excessive operator atten- tion. Also, the gasifier compressor shut down several times because of high water levels in the suction scrubber. The acceptor was totally calcined at 1800° F on Wednesday, May 23. At 8 PM, the gasifier compressors were lost for the third time, causing the char/acceptor interface in the gasifier boot to be lost as well as acceptor circulation. Restoration of the interface and acceptor circu- lation was not possible, so the system was shut down for repairs. Between 6 PM and 8 PM May 23, there was no air in the gasifier and no natural gas in the regenerator. The system was operating at near optimum conditions. At this time the plant was producing gas from char. A short shutdown was taken to unplug the system. No plugging was found in the transfer line between the regenerator and the gasifier. The hot spot on the acceptor lift line, which was caused by a void space in the insulation, was repaired. The quench systems were cleaned. The regenera- tor quench tower inlet venturi was cleaned and revised. The revision pro- vided a water inlet upstream of the venturi instead of in the throat of the venturi. The gasifier heaters were inspected and thinned areas in the heat- er tubes were built up with weld metal. The preheater was opened but was still too hot for inspection; it was decided not to use the preheater until revisions could be made to reduce the amount of char attrition that occurs. Block valves were installed for on-stream addition of an exchanger in parallel with the HPC absorber overhead cooler (to reduce pressure drop in the system) and for the addition of the devolatilizer compressor suction scrubber in series with the gasifier compressor suction scrubber. The short shutdown was completed late Friday night and the system pressured that night. On Saturday the 26th it was necessary to depressure and replace the block valves for the parallel exchanger mentioned above because of leakage. The system was again at pressure by noon. This run included some minor changes such as: addition of steam to the gasifier side flow earlier in the startup, and shutting down one recycle compressor on the regenerator system when gas flow to the regenerator permitted. Acceptor circulation was started about 7 PM and the heaters were lit at 8 PM. The HPC system was then put into service. By 11 AM on the 27th dolomite was started batchwise to the gasifier. By 4 PM dolomite was being fed from the fresh dolomite lockhopper. Steam was started to the gasifier late Sunday night. On Monday, the regenerator bed height was sufficient to seal the transfer line by 6 AM. The purged tap in the gasi- fier differential pressure probe on the bottom differential pressure trans- mitters became partially plugged. During the course of trying to unplug It, another tap became plugged. These taps were on the transmitters that control the acceptor level in the gasifier boot. The signal from some side taps was used for subsequent level control. 200 At a little after 1 PM, Monday, May 28, the acceptor circulation tests were run. Char was started to the gasifier by 5 PM. Natural gas and air were burned in the regenerator by about 8 AM on Tuesday. At 1 AM on Wednesday, acceptor was being circulated and air was being fed to the gasifier. By about 8 AM char was started to the regenerator from the gasifier. The char bed bulk density had been reduced to 32 pounds per cubic foot. Total calcination of the acceptor had been accomplished by afternoon. Carry over of solids into the quench system gave problems on Wed- nesday. Considerable operator attention was required during these plant conditions. On Thursday, the purge to the top tap in the regenerator was lost, causing loss of level indication and differential pressure control between the regenerator and the gasifier. Erratic char feed and acceptor circula- tion resulted. The tap was cleared and the system stabilized. Several pins sheared in the fresh dolomite feeder during the day. This problem was resolved by a change in operating techniques. Gasification rate was low. Acceptor activity was low, and acceptor was being held up in the char bed. In accord with the process concept, spent dolomite was purged from the system and fresh dolomite added to re- place it. This procedure was limited by a low dolomite inventory. All operating conditions were essentially on target for a gasifica- tion demonstration run, except that air was being added to the gasifier to maintain temperature. (Gas heaters were being held at lower-than-desired temperatures because of tube deterioration.) The gasifier bed temperature was held at about 1475 F. These conditions were held until 2:45 AM Sunday, when air feed to the gasifier was discontinued. The gasifier bed temperature dropped to about 1400 F and held steady, until air feed was resumed at 12 noon and the gasifier bed temperature raised to 1500° F. Thus from 2:45 AM to 12 noon on Sunday, June 3, the system was at true gasification conditions, with the gasifier bed about 100° F lower than desired. At 1:30 PM Sunday, steam was added to the gasifier boot in an at- tempt to increase acceptor activity and gasification rate, both of which were lower than desired. When steam flow to the boot was initiated, the instrumentation responded by cutting off recycle flow faster than antici- pated. This upset the boot fluidization conditions. Shortly thereafter the acceptor transfer line from the gasifier boot to the regenerator plugged. Attempts to break the transfer line plug were not successful. About midnight Sunday the decision was made to shut down. 201 2.2 OPERATING CONDITIONS AND RESULTS Operating conditions and results for the last four days of the run, both for the gasifier and the regenerator, are presented in Tables 10-1 through 10-4. The Tables record simultaneous data at a specific time on May 31, June 1, June 2, and June 3 respectively. Figures 10-1 through 10-4 are time charts of key variables for the gasifier and regenerator from May 30 through June 3. For the gasifier, Figure 10-1 records bed temperatures, gas flow rates, and overhead gas compositions; Figure 10-2 records char feed rate and apparent char density, bed temperatures, the instrument air pressure loading on the acceptor inlet valve (an indicator of acceptor feed rate), and the activity of the acceptor. For the regenerator. Figure 10-3 records air and recycle flow rates, bed temperature, and overhead gas composition. Figure 10-4 records temperature, the corresponding equilibrium carbon dioxide pres- sure, acceptor activity, and the flows of fresh acceptor makeup and spent acceptor removal . Table 10-5 presents selected data for one time on each of the last three days of the first part of the run. May 21, 22, and 23, and for several times on the last eight days of the run. May 28 through June 3. Figures 10-5 and 10-6 record regenerator temperature, equilibrium carbon dioxide pressure, and actual carbon dioxide pressure during the two periods when the calcium portion of the acceptor was brought from the uncalcined to the calcined state (May 23, and May 30 and 31). 2.3 SYSTEMS PERFORMANCE 2.3.1 Char Grinding and Drying (100 area) In past runs the char grinding has resulted in a product con- taining 20 to 25 percent smaller than 100 mesh. During Run 10, a special effort was made to decrease the time spent by the feed 'char in the roller mill. This was done by increasing the volume and velocity of the drying and carrier gas to and through the mill. XCV-1037 (value controlling recycle inlet gas to mill) was fully open, as was XCV-1003 (recycle tempering gas to the furnace). The cone in this mill was at the full down position, increasing the velocity in the mill. The result was a ground and dried char with approximately 10 percent smaller than 100 mesh material. The mill was run constantly rather than in the "on-off" condition used in some prior runs. With the above "full open" flows, the drying furnace was held at 775 to 800 F, maintaining the mill at 290 to 300® F with a resulting product rate of 100 LB/MIN or 6000 LB/HR. 202 The baghouse temperatures were maintained above 200° F. At startup, the baghouse is about 175 to 185° F and levels out at 220 to 240° F during the run. During Run 10 the baghouse blower shaft had to be repaired. This caused a problem of scheduling char supply to the main unit, but did not cause any unnecessary delay in the run. The preheater was not operated during the last part of Run 10. The product char was dropped into tote bins, hauled to the 8th floor and unloaded into the feed lockhoppers there. Following is a sample set of run conditions for the char grinding and drying: Dryer Furnace Temp (TSH-1002) 775°/800° F Roller Mill Inlet Temp (TRC-1000) 290°/300° F Gas Inlet Pressure (PRC-1000) 7.5 IN W.C. Delta Pressure (dPI-1007) Velocity Separator Cone Dryer Furnace Recycle (XHC-1003) Dryer Furnace Bypass (XHC-1037, inlet to mill) Lignite Lift Line Skin Temp, BTM (TE-1006) Middle (TE-1007) Top (TE-1008) Cyclone Separator, Inlet Pres (PI-1005) Outlet Pres (PI-1006) Outlet Temp (TE-1009) Baghouse Delta Pressure (dPI-1008) Outlet Temp (TE-1029) 2.3.2 Dolomite Handling 6 IN W.C. Full Down 15 PSI Loading (Full Open) 3 PS I Loading (Full Open) 220° F 215° F 200° F -2 IN W.C. -4 IN W.C. 250°/260° F 4 IN W.C. 220°/230° F The Tymochtee dolomite used in Run 10 was brought in by bulk carrier and unloaded at the Hills Materials Company yard. There it was dried and loaded into dump trucks and then delivered to the pilot plant location. After conveying to the dolomite silos, the rock is ground in a hammer mill and sized with a vibrating screen. The resulting product is a nominal 6 X 20 mesh size. 203 A test run during Run 10 indicated that only 45 percent of the dolomite feedstock ends up in the sized product bin. The other 55 percent goes into the fines bin and is discarded. The sized product is put into tote bins, sampled, weighed, and hauled to 6th floor for unloading into F-206, the dolomite feed lock- hopper . 2.3.3 Quench Systems During Run 10 there was some trouble with the gasifier quench system. The circulating pumps, J-301 A/B, for the quench towers were plugged off because of excessive carry-over of solids to the separator drum, F-319. The regenerator quench system was a constant source of problems. The areas causing the most trouble were the gas inlet to the quench tower, E-302, and the slurry outlet from the quench tower. The venturi on the inlet of the regenerator quench tower kept trying to plug during the first part of Run 10. The pressure drop across the venturi kept increasing until approximately 10 PSI pressure drop existed. The venturi was kept open and the differential pressure across the venturi was reduced by hammering on the throat of the venturi and flushing it with water. Inspection after the run showed the two -inch throat of the venturi to be reduced to about the size of a half dollar. The venturi was modified before starting the second part of Run 10. A spool piece containing a 6 X 4 swedge with a 4 -inch extension on the 4-inch part of the swedge was installed in the existing 6-inch line up- stream of the venturi. Tangential nozzles, 180 degrees apart, were in- stalled on the spool piece for water addition in the spool piece rather than in the venturi throat. (See Figure 10-7.) Boiler feed water was used in the spool piece rather than quench water from the system. This arrangement proved no more effective than the venturi itself. A high differential pressure still developed at the tower inlet and the venturi still required external massaging. The buildup with this arrangement was in the inlet to and throat of the venturi. The level control valve, LCV-3002, on the bottom of the regener- ator quench tower plugged, causing high levels in the tower. When the valve was removed and cleaned during the two-day shutdown, it was plugged with large solids that should have been removed in the cyclone. A considerable amount of solids was carried over because of pressure surges in the regenerator when breaking loose the venturi plugs. During the second part of the run, the level control valve could not handle the throughput, so the bypass had to remain partially open. High levels in the quench tower may have caused high pressure drops across the venturi because the liquid level apparently was going above the gas inlet 204 The quench water pumps, J-302 A/B, did not function well during the second part of the run, so the foul water stripper pumps, J-314 A/B, were used to put water into the quench tower. Either the suction to the quench water pumps was plugged or the pumps were cavitating. The pumps did perform better when the cases were externally cooled with water. Boiler feed water was added directly to the bottom of the quench tower in an effort to flush solids from the tower through LCV-3002 to the pond. Use of the foul water stripper pumps, and putting boiler feed water into the tower, contributed to the high levels in the quench tower because of the uncertainty of the amount of water going to the tower. 2.3.4 Solid Feed and Removal Systems Leaking valves on the lignite lockhoppers, F-204 A/B, caused some problems. All char was fed from tote bins because the preheater was out of service. Leakage through the valve on the lockhopper under pressure would keep the char from going into the depressured lockhopper. Manual vents had to be opened and considerable effort expended by the operator to fill the lockhoppers. XCV-2086 on F-204B lockhopper had a particu- larly bad leak. It was found, in the after-run inspection, to have a very large pit on the valve ball. The lignite and fresh dolomite lockhoppers vent through a common header to the vent stack. If the dolomite lockhopper, F-206, was de- pressured while a lignite lockhopper was being filled, char would be blown all over the 8th floor from the tote bin station. The packing in the dolomite rotary feeder, L-204, blew out once and two pins sheared. This seemed to occur because the recommended procedure for filling the fresh acceptor lockhopper, F-206, was not followed. If the valve above the feeder is open when the valve below the feeder is closed, and the feeder is left running, it packs with solids and blows the packing and/or shears pins. The recommended pro- cedure is to close the upper valve, fill the hopper, open the lower valve, start the feeder, and open the upper valve. The lower valve must be closed because the upper valve will not hold the system pressure. The ash lockhoppers, F-207 A/B, performed well during the run. The weigh cells are still not reliable but do give indication of weight gains. The Posi-Seal valves above these lockhoppers performed well. During the first part of the run, the hand-operated valves were not used. During the second part of the run, the hand valves were always used because the lockhoppers could not be depressured otherwise. When the valves were inspected, fines were found behind the seats. The seats on the automatic valves were replaced and the seats on the hand valves were cleaned. 2.3.5 Hot Potassium Carbonate System The Hot Potassium Carbonate (HPC) system was run for the first time during Run 10. Several things hinder proper evaluation of the system. The 2-inch bypass around the HPC system was partially open most 205 of the time because of high pressure drop through the absorber overhead condenser, C-303. Adjustment of flow through the bypass was being made constantly. An additional cooler is being put in parallel to C-303 so the need for the 2-inch bypass next run should be eliminated. Absorb- tion of CO2 from the overhead gas that did pass through the HPC system appeared to be good. All of the available potassium carbonate was used before Run 10 was terminated, so the concentration of potassium carbon- ate in the system could not be maintained. The drains on the two knock- out pots, F-304 and F-303, have been piped to return to the HPC system in an effort to reduce potassium carbonate losses. Prior to the next run, a program will be established for evaluation of the HPC system. 2.3.6 Material Balance The report on Run 7 showed the results of the first serious effort to accurately measure the acceptor and char fed to the system and balance it against the solids that were removed from the system and the gases that were produced. The balance was 25 percent deficient in product materials. Several measures have been taken since that time to more accurately measure the inputs and outputs. In the second part of Run 10, balances were made on total material, contained clacium oxide, and elemental carbon. The resulting balances came out within two percent, which is strictly fortuitous because the measurements and estimates were not that accurate. 2.3.7 Total Solid Balance The weights used in the material balance were taken from the log sheets except where noted. Typical laboratory analyses were used to segregate the various forms of char and acceptor. Following are the theoretical weight percentages used for dolomite in each case: Fresh Acceptor (100 LB basis): 20.6% MgO 22.5% CO2 with CaCOj 22.5% CO2 with MgCOj 5.8% Inert Calcined Acceptor (100 LB basis): 28.6 CaO - 20.6 MgO - 37.5 5.8 Inert- 10.5 55.0 LB solid 45.0 LB CO2 52% of solid of solid of solid 206 Acceptor out of Gasifier, assumed 0.25 activity: 12.7 LB Ca CO 20.96% of solid 21.5 LB Ca 35.48% of solid 20.6 LB Mg 33.99% of solid 5.8 LB Inert 9.57% of solid 60.6 LB 100.00% In calculating the acceptor coming out of the gasifier, an activity of 0.25 (R) was used. When dealing with the fines and ash-out lockhoppers, it must be noted that the inert rock fines and the ash portion cannot be separated. The Ca and Mg portions are separated but the other 33.1 percent is lumped together as "Other". This same designation is used on other stone also, due to a deposit of this material (i.e., SiO^) on the stone. Sample weights were estimated. There was no measure of carbon dioxide removed; it was accounted as the total carbon dioxide fed in as carbonate, minus the carbon dioxide contained in the estimated quantities of carbonate removed from the system. The overall material balance is shown in Table 10-6. The ac- counted input is 243,050 pounds, the output 247,360 pounds an imbalance of only 4,310 pounds, or 2 percent. 2.3.8 Calcium Oxide and Carbon Balances Balances on calcium oxide and carbon were made by calculating the contained portions in the overall balance. Results are shown in Table 10-7. The calcium oxide imbalance is about two percent. The car- bon imbalance is nil. 207 3 STARTUP PROCEDURE FOR RUN 10 (1) Pressure test at 150 pounds. (2) Establish recycle as follows: Gasifier Inert Gas FRC-2126 5,000 SCFH Boot, Recycle FRC-2019 40,000 SCFH Total, Recycle FRC-2020 90,000 SCFH Regenerator Char Lift Gas, I.G. FRC-2015 7,000 SCFH Air Line, Recycle FRC-2032 40,000 SCFH Lift Gas, Recycle FRC-2014 90,000 SCFH (3) Bring quench systems on prior to heatup. During system heat- up, hold temperatures in both reactors at 250° F for 2 hours to cure new refractory. Then increase reactor temperatures to 1300° F while maintaining heater temperatures as follows: Heater Temperature, ^F B-201 1600 B-203 1200 B-204 1050 B-205 1400 (4) Check low spots in system and drain any accumulated water. (5) Observe operation of hot pot system and adjust carbonate sol- ution concentration as necessary. (6) Charge acceptor inventory to gasifier boot. Hold to allow bed to half calcine (1300° F) and then transfer to regener- ator. Feed three batches to the regenerator before starting F-206 feed. Be sure to sample all tote bins and record charged weights and feeder RPM. Include time and notation of RPM changes. (7) Keep feed rate at level which allows regenerator temperature to remain above 1100° F. Continue to half calcine acceptor in gasifier and transfer to regenerator. (8) Note when following regenerator bed differential pressure re- corder pens lift (show differential pressure): dPR-2074 2075 2076, and 2077. (9) Continue feeding until regenerator is full rdPR-2077 equals dPR-2076). 208 (10) Set dPRC-2030 at 5 PSI. If necessary, adjust regenerator recycle rate to maintain discharge pressure. (11) Briefly circulate acceptor to prove integrity of system and operate controllers while maintaining 1300° F temperature in both reactors. Allow gasifier boot heater outlet to drop to 1150° F. Test circulation at various valve loadings (TCV- 2030) from 6 to 15 PSI. Stop circulation and observe res- ponse of new thermocouples in line CD-206. (12) Run gasifier flow tests to determine incipient fluidizing velocity. Following this, add 40,000 SCFH steam to gasi- fier side inlet while removing all recycle gas from the con- nection. Stop acceptor circulation prior to char addition to gasifier. (13) After ensuring oxygen concentration in preheat gas is below 2.0 percent, put char preheater into operation. Feed char from preheater to lockhoppers. Establish continuous feed (use both lockhoppers) to gasifier at minimum fee*<3r RPM. Bring char bed level to 25 feet (lift pen on dPR-.z: 33) . Add acceptor to gasifier from regenerator to make up any boot losses. Slowly decrease setting on dPR-2030 as char bed level increases. At bed level of 25 feet set dPR-2030 at 0.0 and shut off balance gas to line CD-206. Reduce all line purges to minimum. (14) Add 10,000 SCFH air to gasifier side flow while backing out 10,000 SCFH steam. Bring gasifier temperature to 1500° F. After air addition, cut out inert gas makeup to gasifier. (15) When char leg is sealed, start natural gas combustion in regenerator. Maintain temperature at 1300° F and decrease B-203 heater outlet to 800° F. Start shifting gas from acceptor lift line to regenerator air side entry. Decrease lift gas rate to 60,000 SCFH when possible. Control O2 con- centration at 0.5 percent. (16) After partially gasifying char bed to reduce density (indi- cated by dP readings) to 35 LB/CU FT, resume acceptor cir- culation. Increase valve TCV-2030 loading to 9 pounds. If all goes well, start char combustion in regenerator. For regenerator bed temperature below 1600° F, maintain 0.5 per- cent CO concentration in the overhead. Above 1600° F, in- crease CO concentration to 5.0 percent. Slowly increase air rate to 40,000 SCFH maximum and adjust char feed rate to regenerator accordingly. Also feed fresh char to gasifier and watch char bed density. (17) Keep maximum recycle gas in regenerator. Reduce only if super- ficial gas velocity exceeds 3 FT/SEC. Following calcination, increase regenerator bed temperature to maintain 1 atmosphere CO2 partial pressure driving force. 209 (18) As circulation rate is increased and char bed temperature is maintained at 1500 F, gradually back out air from gasifier (19) Adjust system operation to obtain gasifier char bed tempera- ture of 1500 F without air addition and calcination condi- tions specified by item 17 without methane addition. 210 4 DETAILED OPERATING INSTRUCTIONS FOR RUN 10 Our next run is to be designated Run 10. The main differences from Run 9 include use of the HPC system and modifications in acceptor calcination conditions and procedure. Instrumentation changes, re- pairs and revisions to hot lines and process heaters, and valve re- visions to the ash lock hoppers have been made. 4.1 PRELIMINARY CONDITIONS AND INFORMATION (1) Initial steps will include the heat curing of the regenerator and gasifier refractory patching. (2) No air flow from J-202, the regeneration air compressor, is to be used initially. (3) All dPT's and dPR's are to have been zeroed per revised SK-24S (Revision 8). Note the instrumentation changes. (4) All Moore regulators are to be bypassed. (5) All purges in service are to be at a reading of 2 during initial stages of pressurization and be at a reading of 7 when up to operating pressure except the following: FI SETTING PI SETTING 2154 3. 5 2041 20 2153 3. 5 2038 20 2152 3. 5 2036 20 2278 20 2096 20 2277 20 2098 20 2276 20 2213 20 2275 20 2100 20 2280 20 2102 2104 20 20 During pressure testing and pressuring of system, bring all purges up slowly to values indicated above as system is brought to test or operating pressure. (6) The control system for valve number FCV-2113 has been modified to enable us to control air flow rate to the regenerator, utilizing CO analyzer AIT-2002. Use the controller, ARC-2002, in the manual mode to control FCV-2113, which will set the air flow rate, FR-2113 (green pen), to the regenerator. (7) Open XCV-5056 and leave open during the run. (8) Open level alarm radiation source on regenerator over- head cyclone separator, L-202. 211 (9) Operate A, B, and C dryers on plant air prior to startup to be sure they are dried out. (10) Have all recorder strip charts on the right time of day. When marking dates and times on charts, indicate exact pen location so that charts can be compared after a run. If a chart is rolled forward, be sure to mark length that chart was rolled. When charts are changed or pulled for any reason, record range of instrument on chart. (11) The HPC system will be used during this run. Have system operational and ready for regenerator overhead gas prior to startup. Potassium carbonate concentration to be 20 percent initially. Operators will check concentration by use of hydrometer. (12) Keep sample points open (not plugged) and dry. (13) Keep ash lockhoppers, F-207A/B, and purged dolomite lock- hopper, F-213, dry. Check often during initial start-up phases. (14) Keep other low points in the system dry. (15) We will be using dolomite during this run. (16) Pushbutton controls for the solenoid valve in the natural gas line to J-309 have been installed in the 200 control room, along with an indicator light. The red (close) button on the first floor has been deactivated electrically. 4.2 PROCEDURE (1) Pressure test the reactor systems to 150 PSIG with inert gas in 25-PSI steps. Hold at each plateau and check for leaks. Do not go to 175 PSIG since PSV-2014 is now set at 175 PSIG to protect L-202. (2) Unless already done, fill the regenerator quench tower, gasifier quench water separator, and the foul water strip- per water separator to operating levels with boiler feed water. Fill the piping, regenerator, and gasifier jacket systems if not already filled. Start circulation of jacket systems and begin chemical treatment of the water. Do not start steam to the regenerator and gasifier jacket systems at this time. Do not pressure the gasifier steam drum with inert gas at any time. Minimize water to jacket of gasifier overhead line. With steam in the gasifier we want the inlet to the quench tower between 400 and 500^ f 212 (3) Fill seal leg on steam line from gasifier steam drum. (4) With the reactor system at 150 PSIG static pressure with inert gas, set FIC-2126 at 5,000 SCFH (inert gas) and set PRC-2113 at 390 PSIG (to obtain the total output of J-309 to FR-2015). (5) Line up PCV-2022 (PRC-2022 at 150 PSIG on automatic), PCV- 3009A (with PRC-3009 at 100 PSIG on automatic), dPCV-2030-1 (dPRC-2030 at zero on manual), and PCV-2071 (with PRC-2071 at 80 PSIG on automatic) for normal operation. NOTE: PCV-3009A is the new small valve in parallel with PCV- 3009. In connection with PCV-5009A, a new small orifice FE-3000A is used. (6) Block in FCV-2032, FCV-2014 and FCV-2113. (7) Close XCV-2024 on manual. (8) Block in regulators on A and B purge systems from dryers. (9) Start circulation of gasifier and regenerator quench water systems. Priority of makeup water to the quench systems is as follows: (a) Boiler blowdown (regenerator quench only). (b) Potable water (foul water stripper only) . (c) Boiler feed water. (d) Cooling water (foul water stripper only) . (10) Line up SO^ scrubber and start its circulation. (11) Start J-201A/B compressors and set PRC-2052 at 230 PSIG. (12) Start J-207A/B compressors. Set PRC-2041 at 250 PSIG. Be sure J-207A/B are lined up in parallel with J-203A/B. Start J-203A/B compressors. (13) Prior to startup. A, B, and C dryers are to have been operated on plant air to reduce the time required to ob- tain acceptable dew points. With the recycle compressors in operation, open the A and B dryers vent valves a few turns to put some recycle load on the dryers. Check out the performance of each dryer on recycle gas with respect to dewpoint at least through one cycle of each chamber. When the dewpoints can be maintained at least below -20 F, continue with this procedure. 213 (14) The regulators on the A and B systems are set at 200 PSIG. Be sure these settings are maintained. Activate these regulators and close XCV-2070 and XCV-2072. Both dryers will then take over the supply to the purge systems. (15) Recheck all rotameter settings. (16) Adjust all other rotameters to be in use in the structure. (17) Leave LCV-2003, LCV-2002, XCV-2073, TCV-2030 open with valve kickers deactivated. (18) With dPRC's on manual, establish maximum flows through dPCV- 2026, 2036, and 2037. (19) Open XCV-2010 if it is not already open. (20) Set PIC-2047 at 200 PSIG on automatic. Open XCV-2024 if it is not already open. (21) Establish the following flows: (a) FIC-2126 at 5,000 SCFH (inert gas) to discharge of J-201A/B (b) FRC-2020 at maximum compressor capacity to B-201A/B from J-201A/B (recycle) or 90,000 SCFH, whichever occurs first. (c) FR-2260 at 40,000 SCFH (recycle gas) with balance of recycle through FIC-2019 (d) FRC-2013 at SCFH (air) to B-201B from J-202. (e) FRC-2021 at SCFH (steam) to B-201. (f) FRC-2015 at total output from J-309 to B-204 (inert gas) (g) FRC-2032 at 40,000 SCFH (recycle gas) to B-203 from J-203A/B and J-207A/B (h) FRC-2014 at 90,000 SCFH (recycle gas) to B-205 from J-203A/B and J-207A/B (i) FRC-2113 at SCFH (air to B-203 from J-202) (22) With the HPC system in operation, establish regenerator recycle gas flow through the absorber. The pressure drop through C-303 will limit the amount of gas that can be sent to the absorber. Maximize gas to absorber and minimize bypass gas. Be sure automatic drainer on C-303 outlet is working properly at all times. 214 (23) When the oxygen content of the recycle gases is less than two percent, start the process heaters. Use the following procedure for curing the refractory patching: (a) Establish 250° F in the regenerator and gasifier at a rate of 50 to 75° per hour. (b) Maintain 250° F for 2 hours at PT 34 in the regen- erator and PT 45 in the gasifier. (Temperature points are on TI-2001.) (24) After step 23 is completed, bring the heaters to the following temperatures: B-203 1200° F Maximum B-204 1050° F Maximum B-205 1400° F Maximum B-201 I A 1600° F Maximum B-201 IB 1600° F Maximum As before, B-201-IIA and TIB are to provide 70 percent of the total temperature rise across IIA plus lA and IIB plus IB respectively. The rate of heatup is to be at an even rate of 200° F per hour until 1000° F is reached. Then raise temperatures at a rate of 100° F per hour until the final outlet temperatures are reached. Monitor each pass of each heater every four hours during heatup, visually and with the optical pyrometer. Record results. Do not let any pass become overheated. Monitor TE's on heater tubes and headers to check for uneven heating. Note any unusual readings and act accordingly. When final temperatures are reached, the Shift Superintendent and Chief Operator will visually check all passes of all heaters once per shift and note results in the log book. Also monitor heaters pressure drops for changes, taking into account flow changes. Monitoring of the fired heaters is of utmost importance. (25) When heater final outlets reach 700° F, start steam to the regenerator and gasifier jacket water steam drums. Hold regenerator steam drum at 200° F and the gasifier steam drum at 330° F. (26) When the reactors have reached 1000° F, close LCV-2003, LCV- 2002, XCV-2073, and TCV-2030, but stroke them once per shift until we have solids in the system. (27) Hold at step 24 final heater conditions until the reactors have either attained a temperature of 1300° F each or the reactor temperatures have lined out whichever occurs first. Start hourly readups at this time. 215 (28) Observe and evaluate operation of the HPC system while the heaters are being brought up to temperature. Deter- mine effectiveness of removing CO2 and he sure system oper- ates properly. (29) Start the preheater furnace, B-102, and warmup the pre- heater, D-101, to between 500 and 600° F. (30) Charge one lignite lockhopper with 2000 pounds of freshly ground 6 X 16 domomite in preparation for step 32. (31) Crack open LCV-2003 by manually setting 5 PSI output on LIC-2003. (32) Add dolomite to the gasifier from the lignite lockhopper to a reading of 60 lines on dPR-2035. Start water sampling per Run 7 where applicable. Initiate other sampling schedules when applicable. (33) Set dPRC-2037 on automatic. (34) Start filling the regenerator as follows: (a) Batch feed from the gasifier when the boot temperature recovers to 1300° F. This will indicate calcination of the magnesium portion of the dolomite. (b) Transfer to the regenerator with LIC-2003 on manual. Do not lose seal above LCV-2003 at any time. (c) Transfer down to a reading of 20 lines on dPR-2034. (d) Refill gasifier boot to 60 lines on dPR-2035 and repeat (a) through (c) above. (35) When three batches of half-calcined acceptor have been trans- ferred from the gasifier, start feeding from F-206 with L-204. Prepare tote bins with 2000 LBS of acceptable ground 6 X 16 dolomite and charge F-206 with two 2000 pound batches each time. When grinding dolomite, sample every 500 pounds for composite samples to lab. Feed from F-206 through the engager pot to the regenerator. Feed at a rate which allows the regenerator temperature to stay above 1100° F. Feed only until the low level alarm comes on before recharging F-206. Keep accurate records of feed- er RPM and the time of feeding. Note any RPM changes and record the time of change. This is very important. Keep complete records of all materials in and out of the reactors. Continue batchwise transfers of half-calcined acceptor from the gasifier also. Be sure each batch from the gasifier has been half-calcined before transferring to the regenerator. 216 (36) When each of the following dPR's lift, note the time on the respective chart. Read and record on all dPR's: dPR-2074, dPR-2075, dPR-2076, dPR-2077 . (37) Continue feeding until dPR-2077, equals dPR-2076. This will indicate about 25 feet of acceptor in the regenerator. (When dPR-2077 lifts, we will then have a seal above TCV- 2030. Set dPRC-2026 on automatic.) Have both lignite lockhoppers empty when the operating level in the regen- erator has been reached. Stop feeding from F-206 if neces- sary to be sure lignite lockhoppers will be empty. (38) When the regenerator acceptor bed has been established, set dPRC-2030 (using dPCV-2030-1) on 5 PSI . Set dPRC- 2026 on automatic. dPR-2030 has been revised to read -10 to +10 PSI. Also, dPR-2030 will equal the algebraic sum of dPR-2025 and dPR-2026. (39) While continuing this procedure, fill the preheater to 15 lines on dPR-1002 in preparation for introducing char to the gasifier. Use steam in the preheater. Set one root (16,800 SCFH) of steam on FRC-1037. Be sure char from the preheater is available when needed in this procedure. (40) Conduct acceptor circulation tests of about 10 minutes duration at TCV-2030 valve air loadings of 6, 7, 8, 9, 10, 11, 12 PSI. Be careful not to lose the seal at TCV-2030 at the higher loadings. The higher loadings may not be attainable. After the above tests, circulate at a loading of 10 PSI for at least one hour. Check all instruments and other equipment for proper operation or problems. Obtain solids samples from sampling points during the 10-PSI loading test in order to test the sample collection systems and test the samples for percent MgO. During the circu- lation tests, reduce B-201-IA final outlet to 1150 F and o 100 F per hour. During the circulation of acceptor, half -calcine all of the acceptor. (41) Stop acceptor circulation. Compare readings from new TE's in line CD-206 above TCV-2030 during circulation with those after circulation has been stopped to see if the TE's can be used to indicate flow of solids in CD-206. Record results. (42) Run tests to establish the incipient fluidizing velocity of acceptor in the gasifier boot. Maintain side flow of 40,000 SCFH. (43) Switch from PCV-3009A to PCV-3009 prior to steam addition to gasifier. 217 (44) With the incipient fluidizing velocity established in Step 42 maintained in the gasifier boot, establish a flow of 40,000 SCFH of steam to the side flow of the gasifier. The side flow is to be 100 percent steam with no recycle. The new piping configuration allows this to be accomplished with the steam flow rate being controlled by FRC-2021. The recycle gas flow to the gasifier boot will be controlled by FRC-2019. In order to establish the steam flow through the gasifier side, it will be necessary to open PCV-2047 fully. (45) Check the oxygen content of the gasifier recycle gas to be sure it is less than 2 percent. When tlils is obtained, load char from the preheat er to the lignite lockhoppers to the gasifier. Start filling the gasifier with char continuously at a minimum RPM. However, do not allow the char tempera- ture in the gasifier to fall below 900° F. Do not resume acceptor circulation. When dPR-2032 lifts, add 10,000 SCFH of air to the gasifier side flow through FRC-2013 and reduce steam to 30,000 SCFH. Continue to fill the gasifier until dPR-2033 lifts. We will then have a 25-foot char bed. When this occurs, have both the lignite lockhoppers empty. Fill the gasifier to the nearest lockhopper. While filling the gasifier, maintain a constant acceptor level in the boot with makeup from the regenerator. As char is fed, reduce dPRC-2030 so that when the gasifier char bed of 25 feet has been established, dPRC-2030 reads zero with the balance gas (dPCV-2026) off and other purges to CD-206 reduced. (46) Obtain 1300° F in the regenerator by burning natural gas. Introduce about 1000 SCFH of natural gas through FIC-2028. Add air through FRC-2113 to maintain 0.5 percent O2 in the regenerator overhead gas. Allow regenerator conditions to line out. If necessary, increase the natural gas and air flows to obtain 1300° F in the regenerator. Reduce B-203 final outlet to 800° F. When burning natural gas on control, adjust flow through FRC-2014 to 60,000 SCFH (recycle) with the rest of the recycle (about 70,000 SCFH) through FRC-2032. (47) After the 25-foot char bed has been established in the gasifier, increase air and decrease steam side flows to obtain 1500° F in char bed or to a maximum of 20,000 SCFH of air. Maintain a flow of air plus steam to side flow of 40,000 SCFH. As the air flow is increased in the gas- ifier, the inert gas through FIC-2126 can be stopped. (48) After partially gasifying the char bed to a char bulk den- sity of 35 LB/CU FT, resume acceptor circulation up to 9 PSI loading on TCV-2030. As circulation rate is increased 218 and char bed temperature can be maintained at 1500° F, gradually remove air from the gasifier and replace with steam. (49) After one hour of acceptor circulation at 9 PSI loading on TCV-2030, initiate char combustion in the regenerator. Add char by means of a flow through LCV-2002 controlled by the output of dPT-2028. Add air to burn the char in the regenerator and maintain a CO content of 0.5 percent until the regenerator temperature reaches 1600° F. Then decrease air to raise the CO content to 5 percent. Slowly increase air and char addition until 40,000 SCFH of air is obtained. (Feed fresh char to maintain the gasifier bed level and watch char bed density.) Do not adjust regenerator recycle rates until 1600° F is reached unless carryover of large- sized acceptor to ash lockhoppers is experienced. Then consult with Consol and Stearns-Roger engineers for course of action. Make up fresh dolomite continuously to maintain the proper regenerator bed level. Be prepared for the loss in bed on calcination. NOTE: Once calcination begins, keep temperature up and increasing to prevent recarbonation of acceptor. (50) If char feed is lost, immediately: (a) Push EHS-2002 to close LCV-2002. (b) Shut off air or at least reduce air to about 10,000 SCFH. (c) If B-203 is being fired with recycle in the heater, increase recycle to prevent low flow shutdown of B-203. Some flow is needed through B-203 so that solids do not enter the holes in the distributor in the regenerator. (d) Increase natural gas quickly to produce CO and heat . (e) Increase air to bring CO back into control (about 5 percent) . (f) Reestablish char feed to regenerator by whatever means are necessary. (g) Line out system again on char to regenerator, back out natural gas, etc. (h) REMEMBER: KEEP CO ABOUT 5 PERCENT WHILE BURNING WITH REGENERATOR ABOVE 1600° F. DO NOT PERMIT OXYGEN BREAK-THROUGH IN THE REGENERATOR OVER- HEAD GAS. 219 (51) The controls we have for maintaining the regenerator tem- peratures are: recycle and regeneration air heater temper- atures; the amount of air; the amount of natural gas; and the amount of char. (52) When regenerator temperatures reach 1600^ F, try to establish a superficial velocity of 3 FT/SEC maximum. Again, watch for carryover of large acceptor particles. (53) Calcination temperature will probably be over 1800° F; how- ever, do not go over 1900° F maximum. (Increasing acceptor circulation would decrease regenerator temperature.) (54) The final objectives of gasification are to have the regen- erator at some maximum temperature as determined by CO2 partial pressure (see Consol or Steams-Roger engineers) , circulating acceptor, maintaining a 25-foot acceptor bed, burning char and not natural gas. The gasifier is to operate at 1500°F without combustion air and maintain a 25 -foot char bed level. (55) The foregoing procedure is a guide for realizing the gas- ification objectives. The critical portions of this pro- cedure will be monitored on shift by Consol and Stearns engineers. The Shift Superintendent is to keep informed of all phases of this procedure and will make the operating decisions using the Consol and Stearns-Roger engineers as consultants. Any changes and their effects on the operation, as well as the effects of going from step to step, are to be discussed by the Shift Superintendent, the Consol engineer, and the Stearns-Roger engineer on duty and this information relayed to the controlman. We will attempt to minimize the number of people giving instructions directly to the control - man. We will attempt to establish the course of action be- fore giving specific instructions. This should result in a smoother operation. 4.3 SOME SHUTDOWN NOTES (1) Specific shutdown instructions will be given when necessary. (2) Do not shut down either quench tower circulation until after recycle gas circulation has been stopped. Continue cir- culation while depressuring. Keep high makeup water flows to keep lines from plugging, especially WQ-328. A flush with a hose would be a good idea after system is depressured. Check for solids at various points and when water is rea- sonably clean, circulation and makeup can be stopped. (See item (3) also.) (3) Shut off steam to F-218 and F-219 as soon as shutdown is begun. F-218 should vent to the gasifier quench tower. Keep 220 gasifier quench system circulating until F-218 is below 200OF. Then vent F-218 to the atmosphere. The gasifier quench system can then be shut down. (4) As system cools down, be sure to keep low points drained of water and dry. 221 5 SHUTDOWN PROGRAM FOR RUN 10 May 24 and 25, 1973 (1) Rotate CD-206 for inspection and cleaning. MWO-4091 . (2) Remove 180-degree bend for emptying regenerator. Reinstall upon approval. MWO-4092. (3) Remove regenerator basket, inspect regenerator and reinstall. MWO-4093. (4) Open regenerator quench tower inlet venturi; inspect, clean, and close. Open 2-inch drain line on bottom of regenerator quench tower, clean, and close. MWO-4094. (5) Open F-139 and F-321 for cleaning. Close upon approval. MQO-4095, (6) Pull burner on B-203 for inspection of tubes. MWO-4096. (7) Inspect J-201 A/B. MWO-4097. (8) Inspect J-203 A/B. MWO-4098. (9) Inspect area of hot spot on CD-208. MWO-4099. (10) Clean LCV-3002 in place. MWO-4100. (11) Install level switch on F-308. EWO. (12) Pull blind on bottom of gasifier tee and reinstall upon ap- proval. MWO. (13) Stub-ins and valves on GQ2-301-3" (Overhead line from F-308) for addition of F-314, DV KO pot in series with F-308. ENG. (14) Check out pressure control on F-204 A/B, Lignite Lockhoppers. Operations and Instrumentation. (15) Check out operation of PRC-2022, PCV-2022. Instrumentation. (16) Check and replace if necessary, TE-2012, char to the gasifier, PT 9 on TR-2000. Instruments? (17) Repair area of hot spot on CO-203 just upstream of XCV-2013. MWO. (18) Remove, inspect and replace orifice in FE-2020-A. MWO 5306. (19) Open, inspect and close upon approval, D-101, Preheater. MWO- 5305. (20) Install pH meter on K CO- from SO^ Scrubber. MWO-5307. 222 (21) Remove breeching from B-201-IA and IB. (22) Check out TC's on B-203 heater. Instruments? (23) Route drain line from F-308 to downstream of LCV-3078 (drain from GF Venturi Scrubber). Note: this valve will be moved in the future. ENG. (24) Change range of AR-3001 to to 20 percent CO^. Move location of sample point to downstream of F-304, RG KO Pot. ENG and Instrumentation . (25) Connections for additional cooling at C-303, HPC Absorber Cooler. ENG. (26) Move high side of dPT-2028 to PI-2028 (upstream of Y pickup point) MWO-3919. (27) Check TC on Regenerator (at 8th floor level) PT 31 on TI-2001, Instrumentation . (28) Repair flame failure light on B-102. MWO-5309, Check TE MWO-4083, (29) Check TE's 2057 and 2087. They are reading 100° F apart. 223 DATE HOUR 5/18/73 1500 1725 2000 5/19/73 0330 0530 2100 2300 5/20/73 0420 0835 S/2\/l'5 0230 0430 5/22/73 0745 1000 1140 1350 1500 1925 2100 0400 0510 0535 0600 0815 0930 0955 0955 1315 1500 1710 1815 6 CHRONOLOGY OF OPERATIONS OR RUN 10 EVENT Several small leaks, no major leaks. 150 PSIG on system. Establishing gas flows. Reactors at 250° F, curing refractory repairs. Completed curing. Started feeding dolomite to gasifier. Transferred first batch to regenerator. High fines content in dolomite. Feeding dolomite to regenerator from F-206. Having trouble transferring from gasifier to regenerator. Started dolomite circulation. Initiated solids circulation tests at various valve loadings. Stopped circulation to check thermocouple in CD-206. Regenerator up to level. Started cutting back on B-201 heater (step 40) . HPC system circulating. B-201 at 1150° F. During this period, circulation tests and fluid- ization velocity tests were run. Char feed to gasifier started. Started filling lockhoppers from preheater. Lost char feed to gasifier due to plugged feed line, Recovered char feed. Started rocks to regenerator to hold level. Air introduced to gasifier (10,000 SCFH) . Raised air to 14,000 and reduced steam to 25,100. Reduced boot flow. Added CH4 to regenerator. Cut B-203 to and reduced lift line flow to 62,000. Put rest through air line. Started natural gas to regenerator. Transferred dolomite from gasifier to regenerator for 3 minutes. Continue to feed char from lignite lockhoppers to gasifier. Increased air to gasifier to 15,000 SCFH. Shut off inert gas to gasifier. Continue to add dolomite to regenerator as needed. Backed out 5,000 steam and added 5,000 SCFH air to gasifier. Bringing levels in regenerator and gasifier up in preparation for char burning and calcination of CaCOj . 224 S/21/1Z 0120 0330 0415 0445 0505 0525 0540 0610 0645 0700 0725 0800 0845 0900 Stopped dolomite feed. Both char feed lockhoppers empty. Hot spot noted below thermocouple on line CD-208 (Lift line to regenerator) on third floor. Steam hose put on. Circulation of dolomite begun. Flow to gasifier boot raised from 4.4 to 4.7 and corrected dPR-2035. Starting to cut air out of gasifier to hold temperature down. LCV-2003 on "auto". TCV-2030 valve loading is 6 PSI (TCV-2030 had been up to 8 PSI but slugged gasifier bed before showering through) . Stopped circulation from regenerator through TCV-2030. Losing in regenerator and not showering. Dolomite feed to regenerator resumed, starting circulation again. TCV-2030 loading at 9 PSI. LCV-2003 on auto loading Charging "A" lignite lockhopper. Found CO analyzer full of water. Raised air from 26,000 to 40,000 SCFH. Cut natural gas to hold regenerator heat 1600 Regenerator venturi causing pressure drop. DV compressors alarming on low suction pressure. F. 5/26/73 0945 1140 2000 2345 5/27/73 1150 5/28/73 1305 1505 1550 1700 5/29/73 0100 0810 1055 5/30/73 1500 1900 2045 0100 0810 Started pressuring up system. System up to 150 PSI . Quenches, foul water stripper, SO stripper, HPC systems pressured and circulating. Heaters lit. Added steam to gasifier. Started addine dolomite. Started acceptor circulation tests. Completed circulation tests. Dolomite inventory established, stopped feed. Started feeding char to gasifier. Started air flow to gasifier. Started natural gas addition to regenerator. HPC system coming down for some valve modifications. During day shift, some flows were adjusted and char feed varied. Also, making corrections and modifications to some questionable instruments. Received four truckloads of dried dolomite. B-203 heater cut. Main gas off. HPC system started back up. Heater inspection and all tubes look okay. Work in instrumentation continues. Circulation of acceptor begun. LCV-2003 on "auto" controlled by dPR-2003 level. TCV-2030 loading at 9 PSI. Began burning char in regenerator. 225 0345 0400 0415 0445 0520 5/30/73 0845 Lost char feed to regenerator. 0915 Regained char feed. 0945 Lost char feed momentarily. 1000 Circulating acceptor and transferring char. Quench systems fouling. 1545 Lost and regained char transfer. 1800 Calcining in regenerator. 5/31/73 0030 FI-2278 plugged. Note: This FI is common to dPR-2076 and dPR-2077 as well as the low side of dPR-2030 and low side of dPR-2025. This affects the control of the whole system. 0035 Put dPT-2030 on manual to attempt to hold unit while correcting FI plugging problem. 0215 J-207B taken off line. 0230 Sampling of S-13 shook-up unit. Regenerator temper- ature went to 1870 F and then dropped below 1800° F. Unit still shook up, losing char feed and regenerator temperature is fluctuating. Stopped dolomite feed to regenerator due to the lack of level indication. 0415 Attempting to put dPRC-2030 on "auto". " Temperature drop in regenerator, circulation overhead and through char line erratic. Starting to remove air from gasifier and adding steam- slight shake-up and loss of acceptor circulation. 0530 Lost overhead again and started acceptor back feeding regenerator. 0545 Reversing (lowering) dPRC-2030 to try to get back circulation. Recovered acceptor overhead circulation. Rodded out FI-2278 tap. Cleared dPRC-2030, looking normal . Sample points S-9 and S-13 plugged. Steam hose put on hot spot on first floor at char pickup point. 1130 Sheared pin on L-204 raw dolomite feeder. 1210 Started raw feed to regenerator. 1300 Char grinding resumed after repair of primary fan. Lit off B-203 heater to assist in holding regenerator temperature. 1420 Hot spots noted on overhead acceptor line from regenerator to gasifier 350° F and 450° F. Decreasing air flow to gasifier. Adjusting flows. Pulled S-13 (char from gasifier to regenerator) sample and lost char flow. Regained and back in line at 1915. Preparing to remove spent dolomite from gasifier to F-213. First dump completed with 800 pounds. 2315 Second dump to F-213 started. 0610 0630 1000 1000 1830 2000 226 6/1/73 0010 Finished dump to F-213 (990 pounds) . Had a fire on floor in 100 area under the fines bin. (Report being written.) 0230 Shear and in dolomite feeder sheared at higher rate. Unit holding while repair work being done. 0325 J-207A compressor off line. 0415 Feeder repaired, acceptor feed started. 0500 Sheared pin in dolomite feeder. 0540 Closed bypass on HPC absorber completely; absorber now completely in system. Working on closing the bypass around C-303 gas cooler. 0715 Testing out feeder (dolomite) . 0915 Dumped spent acceptor to F-213 with subsequent upset in boot. 0945 Boot lined out again. 6/2/73 1215 Baghouse blower shaft repaired and turned over to operations. 1300-1840 Dumped to F-213. 2030 B-203 heater kicked out. 2135-2305 Dumped to F-213. 6/3/73 0005-0115 Dumped to F-213. 0245 Air to gasifier shut off at panel. 0345-0615 Dumped to F-213. 0530 B-203 heater kicked out. 0600 Air to gasifier manually valved off. 0800 Maintenance patched hole in line from lignite cyclone to 100 area. 0915 Dump to F-213. 0930 Having trouble with plug at venturi at regenerator quench tower inlet. 1210 Put 10,000 SCFH air back into gasifier and took 10,000 SCFH steam out. 1300 Put steam into gasifier boot. PRC-2020 closed cutting off recycle. Within a couple minutes there was an upset in the boot and acceptor transfer to the regenerator was lost. 227 ^^ c ti!'' P^J ^ : Figure 10-1. GASIFIER CONDITIONS FOR RUN 10 228 icao ^ 1300 ia» lUO 2400 Ki00 JUUfc 3^ Hlft Figure 10-2. GASIFIER CONDITIONS FOR RUN 10 229 1907 \400 Figure 10-3. REGENERATOR CONDITIONS FOR RUN 10 230 Figure 10-4. REGENERATOR CONDITIONS FOR RUN 10 231 -1 r hJi-h - \\ :-.■'■ -iP'- .,:'r'" ;l--;- r. o u~ oi o t- o, w u u < z o 5 < 232 mm Or- '-.'O i'riO' :i>': . H-T— -i— I — ;ri 1— Ir^v-'rHT- i — -ir-'ri-- ^Jo'££ INIOd-IOQZ-U •y:: '■], .■^!; rill li'jfni'iffvfuif :I;H r^O.-'rb.' .'i '-'.SiiuL.z-' sii aaixoia MoeyvDi? to Q < O lO OS oi O u- o E- w u u < o o 1—1 U < O 3 •H 233 3 u. o < u I— I (X, 1— I a o Z > o to I UJ I o •H 234 GASIFIER REGENERATOR PRESSURE, ATM 11.10 10.98 BOOT SIDE GAS PREHEAT TEMPERATURES, °F 1150 1325 AIR ACCEPTOR LIFT GAS CHAR LIFT GAS 1100 1200 1050 BED TEMPERATURES BOOT, 24 IN BOOT, 62 IN BED, 6 FT BED, 12 FT BED, 26 FT CHAR FEED BOOT FLOWS AIR STEAM RECYCLE INERT SIDE FLOWS AIR STEAM OUTLET TO FLARE 1155 BED, 0.0 FT 1500 BED, 2.0 FT 1495 BED, 8.3 FT 1495 BED, 14.5 FT 1510 BED, 20.5 FT 80 BED, 29.5 FT FLOWS, SCFH 21,189 10,214 46,285 29,842 INLET DIRECT AIR ACCEPTOR LIFT GAS AIR RECYCLE GAS CHAR LIFT GAS INERT GAS NATURAL GAS RECYCLE GAS OUTLET 1755 1878 1838 1848 1848 1830 77,161 64,262 7,014 85,793 Table 10-1. CONDITIONS AND RESULTS FOR RUN 10, MAY 31, 1973, 1730 HOURS (Sheet 1 of 3) 235 GASIFIER REGENERATOR 3.2 JACKET STEAM PRODUCTION, LB/HR • 297.7 OUTLET GAS COMPOSITIONS, MOL % CH^ CO CO^ H2O H2S 33.39 7.88 15.76 15.17 27.80 N/A 0.00 CO CO^ SO' 78.25 4.53 17.22 0.00 0.00 0.441 CO^ DRIVING FORCE, ATM 2.280 BOOT BED INLET BED OUTLET BOOT BED INTERFACE, IN TOP OF BED, FT GAS VELOCITIES, FT/SEC 0. ,932 INLET 0. ,838 OUTLET 0. ,844 BED DENSITIES, LB/CU FT 65, .0 BED 40, .0 BED LEVEL 49, .9 25, .65 2.771 2.783 67.39 Table 10-1. CONDITIONS AND RESULTS FOR RUN 10, MAY 31, 1973, 1730 HOURS (Sheet 2 of 3) 236 GASIFIER REGENERATOR SOLIDS ANALYSES, WT 7. SCREEN CHAR CHAR SCREEN RECARBONATED ACCEPTOR SIZE FEED 0.40 ASH 0.00 SIZE +4 GASIFIER TO REGENERATOR +6 0.00 6X8 2.20 0.00 4X6 0.00 8 X 10 5.50 0.00 6X8 3.82 10 X 14 12.60 0.00 8X9 ^ 11.46 14 X 20 15.40 0.00 9 X 10 18.39 20 X 28 15.60 0.00 10 X 12 14.87 28 X 35 11.70 0.00 12 X 14 16.28 35 X 48 9.30 0.00 14 X 16 11.86 48 X 65 5.90 0.00 16 X 20 10.55 65 X 100 4.60 50.00 20 X 24 5.73 100 X 200 6.50 12.40 24 X 28 3.82 -200 10.30 37.60 -28 3.22 CHEMICAL COMPOSITION ACTIVITY C 76, .0 66.5 H 2. .2 0.78 S 2. .0 0.82 ASH 15. .39 26.90 SOLIDS RATES, LB/HR CHAR FEED 1200 ACCEPTOR MAKEUP 851 ASH OUT 250 0.30 Table 10-1. CONDITIONS AND RESULTS FOR RUN 10, MAY 31, 1973, 1730 HOURS (Sheet 3 of 3) 237 GASIFIER REGENERATOR PRESSURE, ATM 11.10 10.94 GAS PREHEAT TEMPERATURES. "F BOOT 1155 AIR 1060 SIDE 1350 ACCEPTOR LIFT GAS CHAR LIFT GAS 1100 1050 BED TEMPERATURES, °F BOOT, 24 IN 1360 BED, 0.0 FT 1830 BOOT, 62 IN 1475 BED, 2.0 FT 1865 BED, 6 FT 1475 BED, 8.3 FT 1840 BED, 12 FT 1475 BED, 14.5 FT 1845 BED, 26 FT 1500 BED, 20.5 FT 1845 CHAR FEED 80 FLOWS , BED, 29.3 FT SCFH 1835 BOOT FLOWS INLET AIR DIRECT AIR 68 ,939 STEAM ACCEPTOR LIFT GAS RECYCLE 23 ,068 AIR INERT RECYCLE GAS 62 ,108 SIDE FLOWS CHAR LIFT GAS AIR 9 ,331 INERT GAS 6 ,759 STEAM 42 ,077 NATURAL GAS OUTLET TO FLARE 36 ,298 RECYCLE GAS OUTLET 80 ,247 Table 10-2. CONDITIONS AND RESULTS FOR RUN 10, JUNE 1, 1973, 2130 HOURS (Sheet I'of 3) 238 .GASIFIER CHAR SOLIDS ANALYSES, WT 7. REGENERATOR SCREEN CHAR SCREEN RECARBONATED ACCEPTOR SIZE FEED 0.60 ASH 0.00 SIZE •f4 GASIFIER TO REGENERATOR +6 0.00 6X8 2.90 0.00 4X6 0.00 8 X 10 7.90 0.00 6X8 2.30 10 X 14 13.60 0.00 8X9 8.08 14 X 20 18.20 0.00 9 X 10 14.17 20 X 28 16.90 0.00 10 X 12 13.37 28 X 35 11.80 0.00 12 X 14 16.67 35 X 48 9.00 0.00 14 X 16 13.07 48 X 65 5.50 0.00 16 X 20 12.28 65 X 100 3.80 26.31 20 X 24 7.58 100 X 200 4.70 25.90 24 X 28 6.39 -200 5.10 47.79 -28 6.09 CHEMICAL COMPOSITION ACTIVITY C 76.0 0.27 H 2.2 S 2.0 ASH 15.34 SOLIDS RATES, LB/HR CHAR FEED 1300 ACCEPTOR MAKEUP 851 ASH OUT 250 Table 10-2. CONDITIONS AND RESULTS FOR RUN 10, JUNE 1, 1973, 2130 HOURS (Sheet 2* of 3) 239 GASIFIER REGENERATOR JACKET STEAM PRODUCTION, LB/HR 19.1 367.1 CH^ CO CO. H2O H2S OUTLET GAS COMPOSITIONS, MOL 'L 48.19 8.02 11.08 11.78 20.83 0.10 CO C02 SOo 75.28 6.83 17.89 0.00 0.00 0.324 CO^ DRIVING FORCE. ATM 2.199 BOOT BED INLET BED OUTLET GAS VELOCITIES. FT/SEC 1.144 0.795 0.805 INLET OUTLET 2.582 2.587 BOOT BED BED DENSITIES. LB/CU FT 70.0 BED 41.0 73.88 INTERFACE, IN TOP OF BED, FT BED LEVEL 68.5 22.46 '-NOT MEASURED OR NO SAMPLE Table 10-2. CONDITIONS AND RESULTS FOR RUN 10, JUNE 1, 1973, 2130 HOURS (Sheet 3 of 3) 240 GASIFIER REGENERATOR PRESSURE, ATM 11.10 10.89 BOOT SIDE GAS PREHEAT TEMPERATURES 1150 1350 AIR ACCEPTOR LIFT GAS CHAR LIFT GAS 1070 1100 1050 BED TEMPERATURES, °F BOOT, 24 IN BOOT, 62 IN BED, 6 FT BED, 12 FT BED, 26 FT CHAR FEED BOOT FLOWS AIR STEAM RECYCLE INERT SIDE FLOWS AIR STEAM OUTLET TO FLARE 1380 BED, 0.0 FT 1445 BED, 2.0 FT 1500 BED, 8.3 FT 1450 BED, 14.5 FT 1460 BED, 20.5 FT 80 BED, 29.3 FT FLOWS , SCFH 20,639 7,078 39,894 44,964 1835 1855 1830 1830 1830 1825 INLET DIRECT AIR ACCEPTOR LIFT GAS AIR RECYCLE GAS CHAR LIFT GAS INERT GAS NATURAL GAS RECYCLE GAS OUTLET 66,265 64,546 6,746 75,883 Table 10-3. CONDITIONS AND RESULTS FOR RUN 10, JUNE 2, 1973, 1630 HOURS (Sheet 1 of 3) 241 GASIFIER REGENERATOR SOLIDS ANALYSES, WT 7. SCREEN CHAR CHAR SCREEN RECARBONATED ACCEPTOR SIZE FEED 0.80 ASH 0.00 SIZE +4 GASIFIER TO REGENERATOR 4« 0.00 6X8 2.90 0.00 4X6 0.00 8 X 10 7.21 0.00 6X8 2.60 10 X 14 14.71 0.00 8X9 8.59 14 X 20 16.82 0.00 9 X 10 14.39 20 X 28 15.72 0.00 10 X 12 13.39 28 X 35 11.31 0.00 12 X 14 16.78 35 X 48 9.01 0.00 14 X 16 12.89 48 X 65 5.71 0.00 16 X 20 11.99 65 X 100 4.20 24.32 20 X 24 7.19 100 X 200 5.31 21.71 24 X 28 5.79 -200 6.31 53.97 -28 6.29 CHEMICAL COMPOSITION ACTIVITY C 76.0 61.1 0.31 H 2.2 .66 S 2.0 .88 ASH 15.34 29.57 SOLIDS RATES, LB/HR CHAR FEED 1650 ACCEPTOR MAKEUP 568 ASH OUT 250 Table 10-3. CONDITIONS AND RESULTS FOR RUN 10, JUNE 2, 1973, 1630 HOURS (Sheet 2 of 3) 242 GASIFIER REGENERATOR JACKET STEAM PRODUCTION, LB/HR 19.1 347.3 OUTLET GAC COMPOSITIONS, MOL % "2 CH4 CO C02 N2 H20 H2S 55.20 N2 12.42 CO 9.76 C02 9.86 S02 .76 02 (1) 0.00 76.81 2.71 20.48 0.00 0.00 0.238 CO DRIVING FORCE, ATM 1.599 BOOT BED INLET BED OUTLET GAS VELOCITIES, FT/SEC 1.035 INLET 0.731 OUTLET 0.716 2.578 2.578 BED DENSITIES, LB/CU FT BOOT 70.0 BED BED 46.0 BED LEVEL INTERFACE LEVEL, IN 43.0 TOP OF BED, FT 26.06 72.38 (1) NOT MEASURED OR NO SAMPLE Table 10-3. CONDITIONS AND RESULTS FOR RUN 10, JUNE 2, 1973, 1630 HOURS (Sheet 3* of 3) 243 GASIFIER REGENERATOR 11.10 PRESSURE, ATM 10.84 BOOT SIDE GAS PREHEAT TEMPERATURES, °F 1150 1350 AIR ACCEPTOR LIFT GAS CHAR LIFT GAS 1070 1100 1050 BED TEMPERATURES, BOOT, 24 IN BOOT, 62 IN BED, 6 FT BED, 12 FT BED, 26 FT CHAR FEED BOOT FLOWS AIR STEAM RECYCLE INERT SIDE FLOWS AIR STEAM OUTLET TO FLARE 1180 BED, 0.0 FT 1420 BED, 2.0 FT 1470 BED, 8.3 FT 1415 BED, 14.5 FT 1425 BED, 20.5 FT 80 BED, 29.3 FT FLOWS, SCFH 28,974 46,285 16,336 INLET DIRECT AIR ACCEPTOR LIFT GAS AIR RECYCLE GAS CHAR LIFT GAS INERT GAS NATURAL GAS RECYCLE GAS OUTLET 1835 1870 1840 1850 1850 1840 51,380 70,745 7,035 58,120 Table 10-4. CONDITIONS AND RESULTS FOR RUN 10, JUNE 3, 1973, 0930 HOURS (Sheet 1 of 3) 244 GASIFIER REGENERATOR SOLIDS ANALYSES, WT 7. SCREEN CHAR CHAR SCREEN RECARBONATED ACCEPTOR SIZE FEED 0.20 ASH 0.00 SIZE -h4 GASIFIER TO REGENERATOR 4« 0.00 6X8 1.30 0.00 4X6 0.00 8 X 10 3.80 0.00 6X8 2.55 10 X 14 10.10 0.00 8X9 7.84 14 X 20 14.40 0.00 9 X 10 12.63 20 X 28 15.80 0.00 10 X 12 12.83 28 X 35 13.30 0.00 12 X 14 15.89 35 X 48 11.30 0.00 14 X 16 13.14 48 X 65 8.10 0.00 16 X 20 12.42 65 X 100 6.20 22.80 20 X 24 7.65 100 X 200 8.10 21.60 24 X 28 6.82 -200 7.40 55.60 -28 8.25 CHEMICAL COMPOSITION ACTIVITY C 76.01 64.8 H 2.2 0.90 S 2.0 0.79 ASH 15.34 31.08 SOLIDS RATES, LB/HR CHAR FEED 1350 ACCEPTOR MAKEUP 568 ASH OUT 150 0.27 Table 10-4. CONDITIONS AND RESULTS FOR RUN 10, JUNE 3, 1973, 0930 HOURS (Sheet 2 of 3) 245 GASIFIER REGENERATOR JACKET STEAM PRODUCTION, LB/HR 19.1 347.3 REACTOR OVERHEAD GAS COMPOSITIONS, MOL "L "2 CH^ CO CO2 N2 H2S 62.16 N2 12.69 CO 9.69 CO 9.79 so 5.66 02 (1) 0.00 78.54 1.20 20.26 0.00 0.00 0.387 COq driving force, ATM 2.028 BOOT BED INLET BED OUTLET GAS VELOCITIES, FT/SEC 1.295 0.913 0.783 INLET OUTLET 2.440 2.450 BED DENSITIES, LB/CU FT BOOT 70.0 BED BED 46.0 BED LEVEL INTERFACE, IN 46.6 TOP OF BED, FT 26.04 64.90 (1) NOT MEASURED OR NO SAMPLE Table 10-4. CONDITIONS AND RESULTS FOR RUN 10, JUNE 3, 1973, 0930 HOURS (Sheet 3 o£ 3) 246 00 NO en o •^ vD f^ CM r^ ^o -J m o^ en ^I> — < iTi m 'J- ^ y£> r-- GO • I r- o m o \0 vO NO P^ ^0 O ^8l *0 r^ tn fn o c< 00 en m -» -» O CO -* * ^XJ " - m CM O o c r^ in O CM o o ^ ^ O 00 • ^* O r-v O CO O vD en O^ o o >o o 00 tn VO fO -3- O O -■ T o tn ■J- o J 00 —t rsi tn Ucn b oo h* (I, <: to (<■ >• < oe Id ■ t-3 .-) g ."B H u o! o « tz: u. u >j -I o M z - b] U U -1 ce o :^ H > O u t-t u o •2 ee < of S a a o y M M u u ■< o <: H la a cB 247 INPUT, LB ACCEPTOR FEED CaO IN CaC03 MgO IN MgC03 CO2 IN CaC03 CO2 IN MgC03 INERT 20,429 (28.67o) 14,715 (20.67o) 16,072 (22.57o) 16,072 (22.57c) 4.142 (5.87,) 17,430 CHAR FEED C OTHER TOTAL INPUT 128,715 (757o) 42.905 (257,) 171,620 243,050 OUTPUT, LB DUMP TO F-213 DURING OPERATION CaO IN CaC03 CO IN CaC03''f CaO UNCARBONATED MgO INERT FINES TO ASH-OUT LOCKHOPPERS CaO IN CaC03 CO2 IN CaC03-v CaO UNCARBONATED MgO OTHER 2,005 1,577 6,064 5,809 1.635 422 332 6,218 3,702 5.926 17,090 16,600 Table 10-6. OVERALL MATERIAL BALANCES FOR RUN 10, SECOND PART OF RUN (Sheet 1 of 3) 248 REGENERATOR DUMP AT END OF RUN CaO MgO OTHER GASIFIER DUMP AT END OF RUN 2,733 1,803 929 5,465 ACCEPTOR CaO IN CaC03 CO2 IN CaC03* CaO UNCARBONATED MgO OTHER ACCEPTOR-CHAR MIX (35-65) CHAR CaO IN CaC03 CO2 IN CaC03'V CaO UNCARBONATED MgO OTHER 234 184 703 604 175 1,900 6,588 436 344 1,312 1,128 327 10,135 12,035 TO WATER RETENTION POND CaO MgO OTHER 408 294 83 785 TO ORGANIC RETENTION POND CHAR MISCELLANEOUS CLEANUP 30,065 SIXTH FLOOR GASIFIER QUENCH 7,250 500 7,750 Table 10-6. OVERALL MATERIAL BALANCES FOR RUN 10, SECOND PART OF RUN (Sheet 2 of 3) 249 SAMPLES CHAR ACCEPTOR CaO IN CaC03 CO2 IN CaC03* CaO UNCARBONATED MgO INERT CHAR CONSUMED, GASIFIER CHAR FED TO REGENERATOR CARBON DIOXIDE VENTED CO2 IN ACCEPTOR FEED CO2 IN CaC03 0UT(1) TOTAL OUTPUT INPUT LESS OUT 82 65 248 238 67 32,144 (2,494) 300 700 1,000 46,290 80,630 29,650 247,360 4,310 (1) SUM OF * VALUES ABOVE Table 10-6. OVERALL MATERIAL BALANCES FOR RUN 10, SECOND PART OF RUN (Sheet 3 of 3) 250 CALCIUM OXIDE BALANCE, LB INPUT CaO IN ACCEPTOR FEED 20,430 OUTPUT CaO IN DUMP TO F-2I3 8,070 CaO IN ASH-OUT LOCKHOPPERS 6,640 CaO IN DUMP FROM REGENERATOR 2,735 CaO IN DUMP FROM GASIFIER 2,685 CaO TO RETENTION POND 410 CaO IN SAMPLES 330 20,870 INPUT LESS OUTPUT 440 CARBON BALANCE, LB INPUT (75% OF CHAR FEED) 128,715 OUTPUT CONSUMED IN GASIFIER 42,495 CONSUMED IN REGENERATOR 53,190 GASIFIER DUMP 4,355 SAMPLES 200 TO RETENTION POND 22,550 MISCELLANEOUS CLEANUP 5,810 128,600 INPUT LESS OUTPUT 115 Table 10-7. ELEMENTAL BALANCES FOR RUN 10, SECOND PART OF RUN 251 RUN 11 JUNE 16 TO JULY 10, 1973 CO^ ACCEPTOR PROCESS GASIFICATION PILOT PLANT RAPID CITY, SOUTH DAKOTA 252 1 SUMMARY During the period of June 16 to July 10, 1973, two runs were made in the pilot plant. Since there were no major revisions in the plant or the run objectives, these runs were designated as Run llA and Run IIB. Both runs were terminated in the first 24 hours after calcination before the run objective of steady state operation was achieved. In each run, the cause for termination was the inability to return calcined acceptor from the regenerator to the gasifier. In both Run llA and Run IIB, plugging of the venturi scrubber upstream of the regenerator quench tower resulted in loss of control of the system pressure balance and regenerator fluidizing velocity. Loss of acceptor circulation is attributed to a high fines content of the calcined acceptor and/or backflushing of steam from the gasifier up the calcined acceptor standleg. Elimination of the venturi plugs is a prerequisite to maintaining fluidizing velocities which are sufficient to strip fines from the regenerator and to obtain suitable pressure balance control to prevent steam backflushing. In Run llA, steam rather than recycle gas was used to fluidize the gasifier boot. The plant pressure balance dictated that a portion of the boot fluidizing gas flow down the recarbonated acceptor standleg. A low acceptor circulation rate was used to prevent a buildup of the showering acceptor inventory in the gasifier char bed which would further disrupt the pressure balance. However, pressure upsets occurring in the regenerator quench tower inlet resulted in uneven acceptor flow down the standleg. Apparently, the standleg cooled to the critical temperature range of 1200" to 1300°F where liquids occur in the CaC03-CA(0H) 2 system, and the line plugged. This plug was broken by "blasting" gas through the standleg sample station, but flow through the calcined acceptor standleg,, which had been stopped when the other standleg plugged, could not be resumed. Attempts to free the calcined acceptor standleg dis- rupted the system pressure balance such that the fuel char standleg seal was lost and backflow through the transfer line resulted in a plug in the fuel char disengager pot. During Run llA, the effects of breaking plugs at the venturi scrubber were greater than the effects of the plugs themselves. The plugs were broken by rapping the venturi with a hammer after the pressure drop had built up to about 12 PSI. The resulting pressure surge heaved coarse solids into the quench tower, caused loss of the fuel char standleg seal and loss of char feed, and upset the pressure balance in the acceptor loop, Prior to Run IIB, a continuous vibrator was installed on the venturi scrubber. A differential pressure alarm was provided to indicate the presence of a potential plug. 253 Run IIB was made with recycle gas rather than steam as boot fluidizing gas to avoid the possibility of plugs occurring by the CaCO -Ca(OH) system. The objective of the run was to reach steady state and obtain data on acceptor performance and system pressure balance. Despite constant vibration, the plugs which formed in the venturi scrubber during Run IIB could not be broken. Although pressure balance upsets were minimized, the regenerator recycle compressor suction pressure dropped off drastically, limiting the amount of recycle gas available to fluidize the regenerator bed. Since the regenerator fluidizing velocity could not be maintained at the programmed rate of 3 FT/SEC, fines were not adequately stripped from the bed. The apparent cause for loss of circulation in Run IIB was a plug consisting primarily of fine acceptor particles. Sulfur corrosion in the boot-fired heater plagued the Run IIB startup^ While feeding char to the gasifier with the heater operating at 1100 F, a plug developed. The restriction was such that the boot could not be kept fluidized either with recycle gas or steam. The gasifier was emptied so that a steam-air mixture could be used in an attempt to "burn" out the restriction. The plug was partially removed and the startup was continued with the heater gas outlet temperature limited to 600 F. In Run llA and Run IIB, control over the regenerator CO concentra- tion was less than desired. In both runs, low CO content occurring at temperatures above 1700 F in the presence of char ash and sulfided acceptor led to the formation of transient liquid type deposits in the regenerator. An acceptor agglomerate was found in the boot following Run IIB. This was formed as a result of long periods of operating with the acceptor in the boot unfluidized while the heater was plugged. Bench scale results showed that acceptor would agglomerate in the boot if not fluidized, particularly prior to being exposed to char combustion in the regenerator. In addition to the heater problems, a 10 minute power failure caused loss of fluidization in the boot. The results of two plant revisions made prior to Run llA were encouraging. First, the replacement of the gas distributor plate in the char preheater with a ring-bubble cap distributor was effective in reducing attrition. Furthermore, by disabling one of two internal cyclones, elutriated fines were removed, thus providing a gasifier feedstock with a minimum of undersized material. Second, enlargement of the fuel char standleg from 2 inches to 3 inches in diameter improved the stability of the char feed to the regenerator. In Run IIB, where surges related to quench system plugs were minimized, not a single loss of fuel char feed occurred. 254 Plans for Run 12 are as follows: (1) Recycle gas to gasifier boot with heater outlet at 600°F. (2) The regenerator bed will be calcined without circulating acceptor to minimize the required heat duty, and minimize quench system loading. (3) Prior to resuming acceptor circulation, heat and material balance data will be obtained in order to calculate the system heat loss. (4) The major objective will be steady state operation with acceptor circulation, acceptor makeup, and purposeful withdrawal. Plant pressure balance and acceptor behavior will be studied and a heat and material balance calculated 255 TEST DATA Run 11 data are presented graphically and/or tabularly at the end of this run report. These figures and tables include: Page Figure 11-1. Ring Type Gas Distributor 270 Figure 11-2. Acceptor Calcination Curve-Run llA 271 Figure 11-3. Acceptor Calcination Curve--Run IIB 272 Figure 11-4. Regenerator CO Concentration and Bed 273 Temperature During Calcination, Run llA Figure 11-5. Regenerator CO Concentration and Bed 274 Temperature During Calcination, Run IIB Figure 11-6. Regenerator Bed Gas Velocity During Calcination, . . ..275 Run IIB Figure 11-7. Solids Deposits at Venturi After Run IIB 276 Table 11-1. Preheater Test--Char 277 Table 11-2. Preheater Test (4 sheets) 278 Table 11-3. Gasifier-Regenerator Data, Run llA (2 sheets) 282 Table 11-4. Gasifier-Regenerator Data, Run IIB (2 sheets) 284 Table 11-5. Solids Analyses (Average) 286 Table 11-6. Solids Analyses (Average) 287 256 3 CHRONOLOGY OF OPERATIONS 3.1 GENERAL Run 11 was divided into two parts. Run llA from June 15 through 21, and Run IIB from June 27 through July 10. Program for Run 11— plant startup and gasification is presented in Appendix 11-A-l; program for Run 1 IB- -plant startup and gasification with revisions made prior to Run lie is presented in Appendix ll-A-2. The daily operations chronology of Runs llA and IIB are presented in Appendix IIB. Additionally, the shutdown repairs and revisions prior to Run 11 are presented in Appendix 11-C-l, and the shutdown repairs and revisions performed between Runs llA and IIB are presented in Appendix ll-C-2. 3.2 RUN llA Run llA started on Friday, June 15, with a pressure test of the system. During Friday night, potassium carbonate solution was carried through the carbonate absorber and into the system. This occurred when the inlet gas valve was opened. Liquid was apparently carried through the absorber condenser, C-303, and then flowed backwards down line GRF-202 and through PCV-2041 into the lift heater, B-205. During the subsequent clean out period, carbonate solution was found in the gasi- fier boot and in the engager pot. The solution was drained from the gasifier boot into the acceptor dump hopper, F-213. On Saturday the system was depressured, and the 180 degree pipe bend below the engager pot was removed to complete the draining. The system was repressured Saturday afternoon and the recycle heaters were lit at 1800 hours. By early Sunday morning, June 17, the heaters were up to desired temperature. Steam was supplied to the system via the gasifier side flow on Sunday afternoon. By 1300 hours on Monday, the regenerator acceptor bed operating level had been established Char was started to the gasifier Monday afternoon and the op- erating level was established by 0630 hours on Tuesday, June 19. Char bed density was reduced to 32 LB/CU-FT by partial gasification with air and steam. Acceptor circulation was then started. The char-acceptor interface was lost at 0800 hours when steam was introduced to the boot but was regained by boot flow adjustments after removing the steam. Steam was successfully admitted to the boot by 1115 hours, June 20. Char combustion was initiated in the regenerator at 1300 hours on Wednesday, and acceptor calcination was begun. Just prior to the start of calcination, the regenerator quench tower venturi began to plug. Plugging of the venturi continued until calcination was completed.* 257 Thereafter, solids deposition in the venturi continued to be a problem but not to the extent it was during calcination. The total pressure drop across the quench system dropped from a high of 30 PSI during calcination to about 9 PSI. At 1730 hours on Wednesday, the acceptor transfer from the gasi- fier to the regenerator was lost. Acceptor transfer from the regenerator to the gasifier was stopped to prevent over-filling of the boot. The steam to the boot was then replaced with recycle gas. By blowing through the S-10 sample point with inert gas, the bottom standleg was cleared. Circulation was regained and steam again replaced the boot recycle gas. However, the calcined acceptor standleg was partially plugged, restricting acceptor flow. At 2230 hours, flow of calcined acceptor to the gasifier stopped. All attempts to clear the line were unsuccessful. Finally, the regenerator pressure was increased above that of the gasifier in an effort to force the plug into the gasifier. This resulted in blowing the char standleg above LCV-2002 and caused a backflow of gas and solids to plug the char transfer line. At 0830 hours on Thursday, June 21, the decision was made to shutdown. During the run the gasifier quench pumps could not maintain the re- quired flow. To make up the difference, one of the foul water stripper pumps, J-314 was used to help supply the quench tower. The loss of pump capacity was probably due to foaming in the quench water separator. 3.3 RUN IIB Run lis started Wednesday evening, June 27. As in Run llA, potas- sium carbonate solution again escaped the HPC absorber and collected in the engager pot. Apparently, the absorber gas outlet was valved closed while the inlet was valved open. The liquid level in the absorber in- creased until liquid backed through the gas inlet line and into both the three-inch and two-inch absorber bypass lines. The liquid again passed through the absorber condensers, C-303 and C-313, and the acceptor lift gas heater, B-205; eventually, it accumulated in a low spot, the engager pot. The system was shutdown for draining. When the system was repressured on June 28, a leak at the regenerator overhead line expansion joint was discovered. The system was again de- pressured to fix the leak and clear a plug in the line between the gasifier and the dump hopper, F-213. The leak could not be found so the system was repressured. Two leaks were then discovered in the expansion joint and the system was again shutdown. The repair work was finished on Sunday, July 1. On Friday, June 29, char was inadvertently fed to the gasifier. Most of the char, 1070 LBS, was removed through F-213 on Sunday, How- ever, the recarbonated acceptor standleg was plugged when gas circulation was attempted. The system was depressured and the lines were cleared of an additional 170 LBS of char on Monday, July 2. 258 Operations resumed again. Acceptor feed to the system was initiated on Tuesday and completed on Wednesday afternoon. The acceptor was circulated successfully. Then circulation was discontinued during the char addition and while the steam-air pregasification procedure was conducted to reduce the char bed density. By Thursday, July 5 a restriction across the gasifier boot heater, B-201-IA, had developed. Steam was substituted for the boot recycle gas in an attempt to clear the tubes while char filling continued. Steam failed to clean the boot heater tubes of what was believed to be an iron-nickel-sulfide deposit. On Friday, July 6, the gasifier was dumped while the regenerator was maintained in a standby condition. A steam and air mixture was then passed through the heater tubes to oxidize the gulfide deposit. The heater outlet temperature was maintained at 1100 F. After 14 hours of this procedure, five of the six tube passes in the heater were cleared. The heater pressure drop, which had been 67 PSI before the oxidization, decreased to 23 PSI. The steam-air mixture was then replaced with regycle gas after the heater outlet temperature had been decreased to 600 F. The run continued with the gasifier boot being filled with acceptor from the regenerator. This material was dumped to F-213 with difficulty. About 300 LBS of fines- laden (23 percent, -20 mesh) acceptor was recovered. After several attempts, circulation was established. During attempts to regain circulation, six hundred pounds of acceptor had been drained to F-213. This acceptor contained about 25 percent, -20 mesh material. On Sunday, July 8, the pregasified char which had been drained from the system before the heater tubes were cleared was fed back to the gasifier. The char level was increased while steam-air pregasification of the char took place. On Monday methane combustion was resumed to bring the regen- erator temperature to 1300 F. Methane had been burned Saturday but was discontinued during the furnace cleaning procedure. Later on Monday, a ten minute power failure caused loss of fluidization in both the regenerator and gasifier beds. The power failure was caused by the power company's transmission system and not by the plant equipment. Both beds were easily fluidized once power was restored, and the char-acceptor interface remained intact. However, the gasifier quench pumps had to be assisted by the foul water stripper pumps following the power loss. Solids partially plugged the quench pumps' suction lines and reduced the pumps' output. With the char bed density (as determined by dP measurements) at 35 LB/CU-FT, acceptor circulation was established. Acceptor calcination via char combustion was completed in three hours. Almost immediately after the start of calcination, the regenerator quench tower venturi began to plug. The plugging problem became progressively worse causing 259 the recycle compressor suction pressure to drop from 135 PSI to a low of 100 PSI, All attempts to break the plug were unsuccessful. Finally, the calcined acceptor circulation ceased twice without warning following the calcination. Circulation was regained four hours after the first stoppage, but could not be regained after the second transfer loss. After the second acceptor circulation loss, a crack in the regenerator quench tower venturi throat was discovered. In order for welders to repair the leak, the combustible regenerator overhead had to be made inert. By cutting back in the char feed and the air rate, the regenerator was cooled and the CO in the overhead gases was consumed. Following the repair, calcination conditions were reestablished until the shutdown . 260 4 DISCUSSION AND ANALYSIS 4.1 SOLIDS FEED PREPARATION FOR RUN 11 (100 AREA) 4.1.1 Char Feed Preparation: During Run lOB, tote bins were used for the char feed transfer from the grinding and drying area to the main unit. The main difference m the materials handling operation during Run 11 was the use of the lignite preheater, D-lOl, in the circuit. Char was added to the system via tote bins during startup. Afterward, the preheater was placed in service. The char was ground and dried in the roller mill and trans- ferred to the lignite cyclone, L-109-L5, where it was disengaged from the transfer gas. The solids were then dropped into tote bins until size specifications were met. Then the discharge of the cyclone was switched to the hot preheater. Most of the heat to the preheater is supplied by the preheater furnace, B-102. Steam, regenerator flue gas, and the combustion gases from the furnace provide the heated fluidizing medium for the preheater bed. The hot char was then fed into the lig- nite feed lockhoppers as needed. A typical set of grinding, drying and preheater conditions are: Roller mill velocity separator cone position Full Down Dryer Furnace (XHC-1003) Full Open Dryer Furnace Bypass (XHC-1037, inlet to mill) Full Open Lignite Lift Line Skin Temperature, Bottom (TE-1006) 250°F Middle (TE-1007) 245°F Top (TE-1008) Cyclone Separator, Inlet Pressure (PI-1005) Outlet Pressure (PI-1006) Top (TE-1008) Baghouse Delta Pressure (dPI-1008) Outlet Temperature (TE-1029) Preheater Gas Velocity Preheater Furnace Outlet Temperature (TE-1015) Preheater Bed Temperature, Bottom (TE-1014 Middle (TE-1013) Top (TE-1012) Gas Out (TISH-1020) 500-600°F Preheater Gas Outlet Venturi Scrubber, Water Flow 40 GPM 240°F -3.0 IN. WC -7.0 IN. W 260-280*^F 4 IN. WC 270-285°F 0.37 FT/SEC 750-900°F 500-600°F 500-600°F 500-600°F 261 The preheater solids are sampled once per shift. Average char size analyses for Runs llA and IIB are presented in Table 11-6. 4.1.2 Preheater Studies: In previous runs when the preheater was operated, char attrition in the preheater was suspected. Originally the preheater had a gas distribution grid which consisted of a 3/8 inch thick 316 SS plate with 223 holes 1/2 inch in diameter. The char size analyses from the pre- heater indicated that attrition was occurring. The attrition probably resulted from (1) the locally high gas velocities through the gas distri- butor holes (approximately 100 FT/SEC), and (2) the battering of char particles against the under side of the grid due to char circulation through the grid. Since the grid was large (8 feet 11 inches diameter), char leakage through the outside holes with subsequent re-entrainment through the center holes was likely. Prior to Run 11 the grid plat was replaced with a ring type distributor similar to the ones in the gasifier and regenerator. As shown by Figure 11-1, the ring is four feet in diameter and has 40 gas risers. A hole was also cut in the internal primary cyclone to allow elutriated fines to leave rather than be returned to the preheater. Between Runs llA and 118, a preheater velocity variable test was run to determine the effect of the new modifications at various veloc- ities. These tests consisted of (1) fluidizing the preheater char bed at different gas rates, (2) maintaining the bed temperature at 525° to 550 F, and (3) taking samples of the bed char and vent gas venturi scrubber water. Seven tests, each lasting six hours, were conducted. Temperature, pressure, and flow rate readings were taken every hour on the half hour, while the char and vent gas venturi water samples were taken every two hours. Total feed was 25,000 pounds. The preheater data are shown in Tables 11-1 and 11-2. The data shown in Table 11-1 were condensed to more clearly show trends and are presented in total in Table 11-2. In Table 11-1, two solids size anal- yses are shown for each test, because the first solid sample of any test always differed considerably from the final sample or samples. The last column of Table 11-1 is the preheater solids analysis after 2-1/2 days of fluidization at a given condition. The column shows that nearly all the -100 mesh fines had been elutriated. The following observations were made: (1) The actual loss of char from the preheater cannot accu- rately be determined. The loss determined from the venturi quench water solids content is not accurate because of the few samples taken and the large differences between the solids content of samples in a given test. 262 Based on water samples, this loss was 3700 pounds, in- cluding approximately 200 pounds lost to char samples. The solids loss based on differential pressure measure- ments was 3000 pounds. This is out of a total char weight of 25,000 pounds. (2) Char attrition losses are normally insignificant. A com- parison of the first solids sample with the last samples taken during a given test (see Table 11-1) shows that the last samples were finer for the tests which had gas superficial velocities above 0.6 FT/SEC. Therefore, some attrition was occurring. For gas velocities below 0.6 FT/SEC the last solids samples were always coarser than the first. This indicates that elutriation or possible bed segregation was occurring and that attrition was low. For these velocities, the venturi water samples show an insignificant solids content of 25 pounds per hour. Comparing the average -100 mesh content of the feed with that of the final two days (Table 11-2), a loss of 3000 pounds is apparent. However, an unknown portion of this loss occurred during feeding. This figure does indicate that elutriation has accounted for much of the char loss. (3) Much of the fine material, i.e., -100 mesh particles, is removed instantaneously as the char enters the preheater. This is demonstrated by the difference between the feed char fines content (14.97 percent of -100 mesh) and the average fines content for the first test (6.9 percent of -100 mesh) . (4) The heat loss from the preheater is about 70,000 BTU/HR. This was determined by making a heat balance for the steady state conditions of the last test. 4.1.3 Acceptor Feed Preparation: In Run 11, two different sizes of acceptor were used. This necessitated the change of screen size used in the vibrating dolomite screen, L-155. The startup acceptor was ground and screened into tote bins first. This consisted of 6 X 16 mesh material. Later the 6 X 16 mesh screen stock was replaced with a 6 X 9 mesh stock. The 6 X 9 mesh material was charged to the system after the 6 X 16 mesh material was calcined. This was done to improve the acceptor showering in the gas- ifier and eliminate some char bed acceptor fines. The 6X9 mesh acceptor could not be charged to the system until the regenerator bed was cal- cined since sufficient fluidizing gas for this size raw stone was not available. During both screening operations, the normal sampling procedure was used; i.e., one composite sample of each tote bin was obtained, the sample being a composite of four samples, one taken every 500-600 pounds screened. Each tote bin holds 2000-2500 pounds of acceptor. 263 The tote bins, after inspection of lab size analysis, were put into the dolomite feed lockhopper, F-206, for feed to the main unit. 4.2 PROCESS SECTION (200 AREA) Runs llA and IIB progressed through the stage of acceptor cal- cination. Both shutdowns occurred during the line out of calcined acceptor circulation. Operating conditions at different times are presented in Tables 11-3 and 11-4. Tables 11-5 and 11-6 show the solids analyses. Figures 11-2 and 11-3 are provided to demonstrate that ac- ceptor calcination was achieved during both runs. Steady state operation of the plant was hindered during Run 11 by two mechanical (as opposed to process related) problemis. These were: (1) severe plugging of the regenerator quench tower venturi scrubber; and (2) corrosion of the gasifier heater tubes due to sulfur attack. 4.2.1 Effects of Regenerator Quench System Problems Plugging of the venturi caused the following problems: (1) recycle compressor capacity was decreased, thereby limiting the maximum regenerator bed velocity and reducing the ability to strip fines from the bed; and (2) when plugs were broken, as in the case of Run llA, system pressure surges resulted. These pressure surges caused momentary loss of fuel char feed to the regenerator, momentary loss of acceptor circulation, and resulted in the carry-over of coarse acceptor particles with the regenerator overhead gases. These particles at times over- loaded the down stream cyclone and were carried into the quench tower where they plugged the water effluent control valve. 4.2.2 Regenerator Deposits and Loss of Acceptor Transfer Following both runs, the regenerator top head was removed for vessel inspection and to clean out transient liquid deposits. Deposits were found on the walls and substantial buildups were located around and just above the air distributor. Run 118 deposits were a little more extensive than those for Run llA. Approximately one-half the air distri- butor holes were found to be plugged following Run llA while only two plugged holes were discovered at the end of Run 118, These two holes were the same holes which could not be cleared during the Run llA shutdown, During the runs, circulation was lost through the calcined acceptor standleg. Both the loss of acceptor circulation and the formation of transient liquid deposits can be attributed almost entirely to the venturi plugging problem. In Run llA, the breaking of venturi plugs caused pressure upsets which made the regenerator fuel char flow er- ratic. Loss of char fuel made control of the regenerator overhead gas CO concentration difficult. As shown in Figure 11-4, the CO concentra- tion^was often less than 0.5 mole percent when bed temperature exceeded 1750 F (the temperature at which transient liquid is known to exist) . 264 In Run IIB, pressure upsets were less frequent because the venturi deposits could not be dislodged. Although this led to a steady deteri- oration of the recycle compressor suction pressure, regenerator char feed was reliable. The simultaneous conditions of low regenerator CO concentration and high bed temperature (see Figure 11-5) were primarily due to operator judgment errors. Failing to anticipate the system response to some char feed rate changes and overcompensating the air flow when CO concentration was high accounted for the errors A little more operator experience would have prevented this from occurring. u inD^°"'^?''^f°" °^ ^^® regenerator dumps from the rather successful Run lOB with that from Run IIB reveals that: (1) the Run 10 acceptor has a thick hard shell (probably the result of 'several eye es through the o? l5o"m;sh mL%'''/'" '' r^^P'^^ '^^ "° ^^^^^' -^ ^2) the amount ot -100 mesh material is much greater for the Run IIB dump. DUMP SCREEN ANALYSES Screen Size Run lOB Run IIB Mesh + 20 76.9 78.7 20 X 28 15.2 78.7 28 X 35 5.2 7.5 35 X 48 1.6 2.4 48 X 65 0.5 0.3 65 X 100 0.2 0.1 llfZ P^^^f'"^ ^" ^^" ^1^' ^hile not hindering the fuel char feed, did 3 F?/SF?^ ir^''r°^ capacity. Therefore, the desired velocit^ of 3 FT/SEC could not be maintained (see Figure 11-6). This resulted in fines accumulation in the bed, which (1) probably promoted trans ent ac?:;tor1?:;Jlet^"'^"^ ^"' ''' ''''''' ''' ^^"^^^"^ ^' ^'^ ^^'^' Another factor affecting the fines buildup in the regenerator bed may be excessive bed level. A high level would restrict the free-board th Hhrdiffere'^tL'^ ''"^ ''"'^^'"^ '^"^^ ^^^^^P^^^' There irevldLce that the differential pressure measurements made in the bed indicate only the minimum average bed level. Near the end of Run IIB the dif- rn^fi 'k /'"^"'''''^ indicated a bed level of 26 feet. Howeve^, using the bed height „7-%-\-7-l-tion and the final regenerator bed weight a F?/<;pr^ J ^"^ ^^ ^^^^ '" calculable for velocities of 2.3 and 2 5 FT/SEC respectively. Data for this calculation are given beliw. Particle density (assumed) 93 lb/CU-FT Temperature ^^3 o^ ^""^^^"^^ 11 ATM Bed dPR Readings, in H 0/IN dPR-i074 0.768 dPR-2075 0.720 dPR-2076 0,642 dPR-2077 ''68 Pounds of Acceptor Dumped 5420 265 Bed Screen An£ ilyses Mesh +4 1.2 4X6 0.8 6X8 11.5 8X9 19.7 9 X 10 17.4 10 X 12 11.6 12 X 14 10.7 14 X 16 6.7 16 X 20 5.4 20 X 24 2.4 24 X 28 1.5 -28 10.7 A high bed level would also explain the carryover of coarse acceptor particles into the ash lockhoppers and quench system. 4.2.3 Recarbonated Acceptor Standleg Problems and Gasifier Deposits The replacement of gasifier boot recycle gas with steam during Run llA made the recarbonated acceptor standleg sensitive to plugging. This was caused by maintaining a low acceptor circulation rate, which allows the acceptor in the standleg to cool, and by poor system pressure balance, which allows gasifier gas to flow down the standleg. At a steam partial pressure of 11 atmospheres, and at temperatures between 1200° and 1300 F, liquids occur in the CaCO_-Ca(OH) 2 system and agglomera- tions occur in the acceptor. This is apparently what happened in the standleg during the run. Once the system is lined out so that pressure balance can be ad- justed, steam flow down the standleg should be eliminated. Until that time or until the circulation rate can be increased so that the standleg temperature is always above 1300 F, the boot flow will have to be re- cycle gas. The Run IIB shutdown included the removal of the gasifier bottom head. This was done to inspect the reactor and to determine why the bed could not be drained into F-213. An 18 inch diameter by 2 foot high ac- ceptor agglomerate was discovered. The material filled the boot to the acceptor standleg outlet, thereby blocking the gasifier dump hopper out- let. This agglomerate resulted from long periods of operation with the acceptor in the gasifier boot unfluidized. Bench scale results showed that acceptor will agglomerate in the boot if it is not kept fluidized, parti- cularly prior to its being exposed to char combustion in the regenerator. Inspection of the vessel revealed that: (1) the refractory was in good condition; (2) the temperature probe had a serpentine bend between probe supports (off center by about one foot); (3) the probes 266 and supports have suffered no noticeable corrosion; (4) the walls were covered with a thin layer of black material (iron rich deposit); (5) ten "bubble caps" in the ring gas distributor were plugged; and' (6) a buildup of material existed around the ring gas distributor. Plugging of the bubble caps probably occurred during shutdown. The solids buildup around the ring was located in a nonfluidized zone and so presented no operating problem. The deposit was mostly silica which would indicate that char slag was probably formed during the shut- down of Run llA when air without steam was allowed in the gasifier. 4.3 HPC AND QUENCH SYSTEMS (300 AREA) 4.3.1 Regenerator Quench The venturi plugging became a problem just after acceptor calcina- tion was initiated. Normally the quench system pressure drop is 9-12 PSI. Of this, 7.5-8.5 PSI is taken across the venturi at gas rates ranging from about 120,000-140,000 SCFH. Maximum quench system pressure drops of 32 PSI and 51 PSI were experienced during calcination for Runs llA and IIB respectively. In Run llA the plugs were partially cleared by tapping on the outside of the venturi with a small hammer. However, in Run IIB the plugs could not be dislodged and became progressively worse. After each shutdown the venturi inlet piping was disassembled and inspected. A circular solids buildup in the spool piece ahead of the venturi was found following Run llA. The venturi was essentially clean. Inspection following Run IIB showed extensive solids deposits from just upstream of the spool piece to within about 3 inches of the quench tower inlet (see Figure 11-7). Plugging downstream of this zone does not normally occur. The deposits found in the venturi diverging nozzle following Run 118 probably resulted from poor gas distribution caused by the upstream deposits. Modifications to the quench system to eliminate the plugging problem are discussed in the Section on Future Plans. 4.3.2 HPC System The total regenerator overhead flow could not be put through the hot potassium carbonate (HPC) absorber because of excessive pressure drop. A high absorber pressure drop limits the suction pressure for the recycle compressors and can cause the compressor to over heat. The present system has 2 inch and 3 inch bypasses around the absorber.* Normally the 3 inch bypass is closed and the 2 inch is partially open. During the run, the absorber pressure drop varied between 40 and 80 inches of water with some gas bypassed. There was also con- siderable liquid hold up in the absorber since increased gas flow to 267 the absorber reduced the level in the HPC stripper and increased the absorber pressure drop. The pressure drop and liquid loading problems were probably due to improper installation of the tower packing (cera- mic intalox saddles) . The packing was apparently dumped into the tower rather than being floated in. About 20 percent of the packing material was found to be broken after Run IIB. The packing has been properly reinstalled. To date the HPC system has never been completely lined out. Since detailed heat and material balances are scheduled for Run 12, tests will be made to determine the absorber efficiency and capacity. 4.3.3 Gasifier Quench System Low flow through the gasifier quench water pumps, J -301 and B, was the only problem experienced with the gasifier quench system through- out the run. After Run 11 A, the suction line to the piamps was found to be clear. No problems were found when 170 F water was circulated through the quench tower. However, a high level had to be maintained in the solids separator during Run IIB to eliminate the low flow problem. There is some indication of foaming in the separator which would indi- cate a higher level than actually available, thereby starving the pumps. Following the July 9 power failure, both pumps had to be sup- plemented by the foul water stripper pumps since solids clogged the quench pump suction line. Modifications to the system are being con- sidered to eliminate the low flow problem. 4.3.4 Gasifier Boot Heater Operation In Run IIB, a high pressure drop developed across the gasifier boot heater, B-201-IA. This occurred while heating 1100 F recycle gas to be circulated through the tubes. Previous experience indicates that the restriction was caused by the formation of an iron-nickel-sulfide deposit. The sulfur contained in the recycle gas is responsible for the formation of this material. By injecting an air-steam mixture into the heater tubes, the sulfide was oxidized. This cleared five of the six tube passes and reduced the pressure drop from 67 PSI to 23 PSI. Sulfur attack in the lA heater has been rapid. Since the ori- ginal coil was replaced with an identical coil from the B-207-IA heater, the heater has been exposed to sulfur (0.1-0.3 percent H^S) at temperatures of 1000°-1200°F for only about 280 hours. Plans are to issue a detailed report covering sulfur attack in the process heaters in the near future. 268 5 FUTURE PLANS Clearly, to improve the chances for a successful run, plugging of the regenerator quench system and sulfur attack in the gasifier process heaters must be eliminated. For Run 12 the regenerator quench system was modified in the following manner: CI) The quench tower venturi was reinstalled in a vertical position with the water inlet at the throat. A rod-out device was also provided at the 90 degree bend down- stream of the venturi expansion nozzle. If necessary, this device will be used to clear the horizontal pipe' section between the bend and the quench tower. (2) (3) (4) Provision was made to install the quenching device proposed by Mr. J. H. Smith of Conoco in parallel with the venturi scrubber. During operation, the regenerator flue gas would be routed through either the quenching device or the venturi. The quencher device is designed to provide considerable turbulence for gas-solids-liquid contacting, to be self-cleaning and to be removable from the system during operation for manual cleaning, if necessary. However, because of materials delivery, the device will not be fabricated in time for Run 12. Zinc oxide or sponge iron systems are being considered for removing sulfur from the gasifier recycle gas. One of the systems will be installed dependent upon equip- ment delivery. Until a sulfur removal system is installed, the gasifier boot heater will be limited to a recycle gas outlet temperature of 600Of when char is in the gasifier. Plans for Run 12 are to obtain accurate heat loss data for the system, particularly for the 200 area. This data will be obtained under conditions of: No acceptor circulation with the reactors maintained near their normal operating temperature (i.e., regenerator at ISOQOF, gasifier at 1500OF) by burning char in the regenerator and adding air and steam to the gasifier. Since this data represents a base condition, it will be very useful in future heat and material balance calculations. Afterward, attempts will be made to obtain additional steady-state data at some acceptor circulation rate. Pressure balance data are also important. The use of steam as fluidizing gas for the gasifier boot requires further understanding of the plant pressure balance. 269 O E- t— I CO CO < CJ m a. oi 270 Oi 00 > U ^ Q, z o rs 1— 1 i ■^ u (V —1 3- < V) ^ u •^ OC > w 3 . u 1a h < • CM 1 1— t 3- i-H 271 CO z UJ > z o I— I H < z u < u o E- a. w u u I u 272 rNoiivalrs--3DP*oD OD (^ «o r- vS lo '^j 2 OS 2: o < 2 M U < u (—1 a: Q U Oi W cx s: w Q W ISO 2 O 2 U U 2 O U o u Ds: o w 2 W a: I •H J. ^anivagdH^i 273 % ' Mc>avairi-3or^co o-d CO 3 E- < u oi Q w a; w o. H Q UJ oa o ^ E- UJ U 2 O U o u a: o z UJ UJ 1/1 I 0) u DO "5: i2iniva^diAnj. 274 OQ 2 O i-i U •J < u 2 HH Di Q I— ( U o > < Q PJ 03 DS o 2 U w Pi \o 0/ •H 'O'^s/a^ '>di9c?n^aA 275 VENTURI INLET VENTURI OUTLET Figure 11-7. SOLIDS DEPOSITS AT VENTURI AFTER RUN IIB 276 O r^ O r-- rvi 00 m -£) Q W (X, r^ in CT o^ - ffJ E- S 1—1 H a 2 o W kJ > w > CO >- w f^ CQ CO hJ H < CL, :2 Q o s W < « > hJ W w O < NJ s l-l li, M o w u o CO in o Pi 1— 1 vO r— 1 iu cC 2 00 o CO oi w w t X X o Q W CQ w 1— 1 HH CU s as 00 m 1 hJ 3 5 a — I 00 r-^ CM 00 vD • • . « 00 CN CO 00 vD CO in \0 f^ 1 — 1 H CO CO . W o CN 1^ .-4 O E- • • • . 00 r-^ in \0 vO in ,-1 CM r-l sO f^ O O^ CM O r-~ in vO v£) r- H (T) CO . w o vO CO r-- 00 in CN 00 vO 00 CN ^^ 1— 1 CN CO . w o r-( 77.2 9.5 vO CM • • v£> CM in r~- in r- • . • • r^ CN CN 00 m CO a^ CN - Cd E-i & 1— 1 E- U 2 O W hJ > w > CO >- Ijj ^s CQ CO J E-" < cu :s Q o s » > hJ CO u o <: IS] s h-i ta M o w a o CO m o ol h-l vO f— 1 fc oi 2 00 o CO OS w W CQ ? 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O ( ^ -£> CT- O O -J "-< -J O s 3 o >, E o 13 O 1 o u. Li- O o ^ OL T3 □£ < ^ U O TJ O 'I H 3: •y. CO c O W < *T CO eo CQ CD O f- O *J -O -O T) 2 cQ m m 284 r- in CM m <-g r^ 0> — CO O <-sj rsi — ' O sO — ' UJ -- O O — CT> -) - r- . . O CU ^ — • c fN oo 2 :c o U-1 o o u-1 o^ r- °° m o o — t r^ 'V. CO f-- O O O O CO o o o^ 0^ rM CO O xD CO r^ ^ ! OO O — r- 00 -J O O O 00 -J fN ^D o CO rsj CM rsj o -J —• o o -^ O O O^ CT' o r^ o >o CJ> cr cr OO — . CD rM o f^ O sD (T 00 cr □c t-i (N CO m o o ^ o r- O o o cr cr rvi 00 o — -J .£> OO cvj rsj -J o o ^r> sC 00 CM cr o ^ ^O T "^ O c-^ O^ •J- — ' o — « o 3 < < Q O CM r- o r^ O O — sD I— I Uh I— I CO < I XXX X X X X X X b. u. u. U. Ci. U. U. Ci. U. U- t-; u o U '^ c; o u u o C/3 'Jl (/I VI (A 0-. 'y, (— H aa CD X X X X X U- U. U. U. U, I '-, '-J o u u « Q. < >. X2 3 > 3 u- o U o t/: o CO a: T3 oc < '/■, 0/ E Q, -" O C o -o o T3 on rt) z: •-■cQciaacocD^iix nj O A- o ■ *J Q. o O -^ E — i-- n -^ -u 4j -O -D TD < (1) I c o o m o n — I ro o o' in ci o' Oco-Hr^Ommin>j-o OO00in00pri^^ w CO >- .J < CO Q I— I o I "~i fN O -T ^ o o a^ r^ 00 •-I CJ £ iJ 286 ^^ (U Q. r^ -H Q n) O rsi OrnO^ ,—1 ^ -C f-4 1-1 I (U ^ C (U ON a; 3 >^ OO 6l, a: .— I fSI ^^ ,-^ I 00 J r<) (Nj — ■■ vj3fvicjNi— lOfNO^rMLCiO OvDo-ir^OvOCJ^O^O^'— imroOO^ —I ,-^ ,— I ■— 1 u~i .— I mQ0r--'-J00"~ii^O00'— I iriO-— i<^oOOrOt^-^oO PJ 5 en 1—1^ — ' CM )-l >-l ^^ o <0 vo -u x: < CO a ^ I u C'-'03- P^CVI. 0^<3-^vOr-c 01 DS P Z CO vOXXXXXXXXXXO q; -f i-M KS vcooo^rooou'ioo'j^o I M .— I.— irvicNiro^vDO o oj) to C o •f-( -f-i *j 6 to . 10 (U 4J 9-A •1-4 tu X CO •o <4-l e C CO M »-i >^ 0) q; r-H ^-H 0) 4J ■u CO c 4.) CO to •H o CO ' ^h^ °"tP^t of dPT-2028. (See letter dated April 9 1973, from F. A. Plut to N. R. Krebs, subject, Modified Con trol Svstems.) Add air to burn the char in the regenerator and maintain a CO content of 5% until the regenerator temperature reaches 1600°F. Then decrease air to In'nnn'5rPM° f"'""' '°, ^"': ^^""''^^ increase air and char addition until 40 000 SCFH of air IS obtained. (Feed fresh char to maintain the gasifier rate un iri60o\ '' \^d density.) Do not adjust regenerator Recycle Lb ?n^i\i • '■^^''''''^ ""^"^'^ carryover of large-sized acceptor to ashlockhoppers is experienced. Then consult with Consol and Stearns-Roger engineers for course of action. Make up fresh dolomite conUnuousIy ^?a n- tain the proper regenerator bed level. Adjust fresh dolomite feed rate so that m order to maintain the regenerator bed level, it will be necessary to wi hdraw acceptor to F-213. Time the filling of F-206 and the empt" n of t;m';er:?ur:s":nd^levli:^ '''' '''''' ''' ''^^ "^^^ ^ ^'^ regeneJaLr^ed 296 APPENDIX 11-A-l (Sheet 10 of 11) Once calcination begins, keep temperature up and increasing to prevent recarbonation of acceptor. If possible, take out the natural gas during calcination. When the regenerator temperature and gas make allow, shutdown one J-207 compressor. (50) If char feed is lost, immediately: (a) Push EHS-2002 to close LCV-2002. (b) Shut off air or at least reduce air to one root. (c) If B-203 is being fired with recycle in the heater, increase recycle to prevent low flow shut down of B-203. Some flow is needed through B-203 so that solids do not enter the holes in the distributor in the regenerator. (d) Increase natural gas quickly to produce CO and heat. (e) Increase air to bring CO back in to control (about 5%) . (f) Reestablish char feed to regenerator by whatever means are necessary. (g) Line out system again on char to regenerator, back out natural gas, etc. (h) REMEMBER: KEEP CO ABOUT 5% UllILE BURNIN'G WITH REGENERATOR ABOVE IGOQOF. ALLOW NO OXYGEN BREAK-THROUGH IN THE REGENERATOR OVERHEAD GAS . (51) The controls we have for maintaining the regenerator temperatures are: recycle and regeneration air heater temperatures; the amount of air; the amount of natural gas, and the amount of char, and acceptor circulation. Record an^l regenerator temperature runaways, char feed losses, etc., and state the time. (52) l\'hen regenerator temperatures reach 1600^F, try to establish a superficial velocity of 3 ft. /sec. maximum. Again, watch for carryover of large acceptor particles. (53) Calcination temperature will probably be over 1800°r, however, do not go over 1900OF maximum. (Increasing acceptor circulation would decrease regenerator temperature.) 297 APPENDIX 11-A-l (Sheet 11 of 11) (54) The final objectives of gasification are to have the regenerator at some maximum temperature as determined by CO partial pressure (see Consol or Stearns-Roger engineers), circulating acceptor, maintaining a 25 foot acceptor bed, burning char and no natural gas. The gasifier objectives are a temperature of 1500°F, a 25 foot char bed level and no air to the gasifier. (55) The foregoing procedure is a guide for realizing the gasification objectives. The critical portions of this procedure will be monitored on shift by Consol and Steams-Roger engineers. The Shift Superintendent is to keep involved in all phases of this procedure and will make the operating decisions using the Consol and Stearns-Roger engineers as consultants. Any changes and their effects on the operations, as well as the effects of going from step to step, are to be discussed by the Shift Superintendent, the Consol engineer, and the Steams-Roger engineer on duty and this information relayed to the control- man. We will attempt to minimize the number of people giving instructions directly to the controlman. We will attempt to establish the course of action before giving specific instructions. This should result in a smoother operation. SOME SHUTDOWN NOTES (1) Specific shutdown instructions will be given when necessary. (2) Do not shut down quench towers circulations until after recycle gas circulation has been stopped. Continue circulation while depressuring. Keep high makeup water flows to keep lines from plugging, especially WO-328. A flush with a hose would be a good idea after system is depressured. Check for solids at various points and when water is reasonably clean, circulation and makeup can be stopped. (See item 3, also.) (3) Shut off steam to F-218 and F-219 as soon as shutdown is to be taken. F-218 vents to the gasifier quench tower. Keep gasifier quench system circulating until F-218 is below 200 F. Then vent F-218 to the atmosphere. The gasifier quench system can then be shut down. (4) As system cools down, be sure to keep low places drained of water and dry. (5) When gas circulation has stopped and pressures of reactors are equal and the system is still hot, open TCV-2030 to drain line CD-206. Initials used herein refer to the following individuals: N. R. Krebs H. K. Long P. J. Boland F. A. Plut APPENDIX ll-A-2 Program for Run IIB - Plant Startup and Gasification This part will be designated Run IIB. The principal difference from Run 11(A) will be to leave steam out of the gasifier boot during gasification until maybe late in the run. These instructions list the changes from Run 11 (A) using the Program for Run 11 dated June 15, 1973, as a reference. CHANGES : 14. The regenerator acceptor bed level control (LlC-2001, etc.) has been revised. See letter dated June 26, 1973, to N. R. Krebs from P. J. Boland, subject "Automatic Regenerator Level Control." 15. A differential pressure switch will be added across the regenerator inlet venturi to alarm in the 200 Control Room when solids start to build up. 16. An air actuated vibrator will be added to the spool piece upstream of the regenerator quench tower inlet venturi. The vibrator is to be used to prevent and/or dislodge solids buildups. We want to avoid system surges when large buildups break loose by keeping pluggages and subse- quent breakages small. 17. New gas/steam ratio sampling equipment is to be installed on the fifth floor. 18. The "no plug" purge fittings have been removed from FI-2280 and FI-2041 on the gasifier. 19. PCV-5152 has been repaired and will be set at 14 psig. 20. Unions have been added to LCV-3002 bypass for easier cleaning. 21. A CO addition line to the gasifier boot has been installed. It uses PCV-2004. PRELIMINARY CONDITIONS AND INFORMATION: (3) The latest revision to SK-245 is revision 9 dated 6-19-73. (5) Set FI-2280 at 20 units. Set FI-2041 at 20 units. (11) The HPC system will be used during this run. Have system operational and ready for regenerator overhead gas prior to startup. Potassium carbonate concentration to be held between 20 and 25% equivalent K CO . Regenerate carbonate prior to startup. During the run, line out the HPC system at some set of conditions and hold it there. Last run, the 2" bypass around the absorber was open two rounds and the system seemed to operate satis- factorily. J 299 APPENDIX ll-A-2 (Sheet 2 of 3) (15) We will be using dolomite during this run. We will switch to a 6 X 9 mesh product right after calcination. The target usage is about 300#/hr of sized dolomite. (17) During acceptor circulation through the char bed, minimize the acceptor holdup. This means low circulation rates and proper gas rates in the gasifier. (18) Getting air out of the gasifier is not as important as lining out the plant at some sort of conditions so data can be taken. (19) After solids beds are established, hold the levels constant since bed level affects the system pressure balance. (20) Watch FRC-2013. Last run, a flow was indicated when valve was blocked in. Open bleed valve when no air is in gasifier to be sure no air is flowing through FCV-2013. (21) It may be necessary to operate dPRC-2030 on manual during the run to solve pressure balance problems with the system. (22) We may use the CO addition to F-223 during this run to convert CaS to CaCO . PROCEDURE : (2) Use boiler feed water to fill the regenerator quench tower and potable or cooling water to fill the gasifier quench water separator and the foul water stripper water separator. (5) Line up PCV-2022 (PRC-2022 at 150 psig on automatic), PCV-3009A (with PRC-3009 at 10 psig on automatic), dPCV-2030-1 (dPRC-2030 at zero on manual), and PCV-2071 (with PRC-2071 at 20 psig on automatic) for normal operation Be sure only PCV-3009A (FE-3009A) is in service at this time, not both PCV-3009A and PCV-3009. (23) This step will be used for drying the regenerator. (24) Revision: (As before, B-201-IIA and IIB are to provide 70 to 75% of the total temperature rise across IIA plus lA and IIB plus IB respectively. (25) Replace side flow recycle with steam with controllers on AUTO to test this method. Revise the third paragraph as follows: After steam has been substituted for recycle in the side flow, introduce steam to the gasifier boot using PCV-2019. FlC-2019 indicates the total flow to the boot, while FRC-2020 will record the recycle flow to the. boot. Make changeover with instruments in AUTO to test smoothness in the AUTO mode. Before proceeding with the run, re-establish recycle flow to the boot, again in AUTO. (32) Add dolomite to the gasifier from the lignite lockhopper to a reading of 50 lines on dPR-2035. Start water sampling per June 18, 1973, schedule unless more samples are needed for proper system surveillance. Initiate 300 APPENDIX ll-A-2 (Sheet 3 of 3) other sampling schedules when applicable. Solids sampling is to be as follows : (a) Acceptor from the gasifier, S-10 (first floor) every two hours. (b) Acceptor from the regenerator, S-9 (sixth floor) every four hours. (c) Char from the gasifier, S-13 (third floor), every two hours. (d) Fines and ash from alternate ash lockhoppers every two hours. The above solids sampling is in addition to any other solids samples desired. (39) Unless already done, fill the preheater to 10 lines on dPR-1001 in pre- paration for introducing char to the gasifier. Use about three roots of steam in the preheater (PRC-1037) . Grind char with the cone all the way down and with XCV-1003 and XCV-1037 fully open. Be sure char from the preheater is available when needed in this procedure. When the preheater char level drops to 10 lines on dPR-1002, refill to 10 lines on dPR-1001. (43) Maintain gasifier side flow at 40,000 SCFH (steam) before and during char addition. (48) Revise: "...resume acceptor circulation up to 7 psi loading on TCV-2030. Delete the second paragraph which begins: "Also, after acceptor circulation has been resumed..." (53) Addition: After acceptor calcination have 6X9 screen dolomite available for makeup. The 9 mesh screen is on hand and has the rectangular openings. Have maintenance change the 16 mesh for 9 mesh when necessary. Establish a steady system state after calcination so data can be obtained over an extended period of time. 301 APPENDIX 11-B RUNS llA ^ IIB DAILY OPERATIONS CHRONOLOGY Run 11 A DATE HOUR EVENT 6-15-73 1500 System at 250 psig for check 1720/2045 Dumping slumpted bed from preheater 1900 Circulating system 2040 Recycle driers in service 2110 Hot pot system put on line. Blew liquid into reactor system. Unit brought down to clean up. Depressured. 6-16-73 1420 System back up to 150 psig 1800 Heaters lit off. Circulation ok. 1900 Recharged hot-pot system on stream, 1920 Grind to preheater complete 6-17-73 AM Bringing heaters up to temperature 1345 Started first batch feed of dolomite to gasifier. PM Continue batch feed to gasifier, and then to regenerator 1720 Started grind to raise level in preheater. 6-18-73 AM Continue batch feed operation. 1000 Transferring batch #13. Preheater at 0800, 90,000 SCFH' steam, 520°F. 1300 Regenerator full of acceptor. Started circulation tests. 1415 Steam hose on hot spot on acceptor lift line to regenerator. 1625 Started char addition to gasifier. 2218 Started air to gasifier to begin pre-gasification. 6-19-73 0130 Started air and natural gas to regenerator. 0630 Stopped char feed, level established. 0715 Increasing air to gasifier, decreasing steam and inert. Adding char to gasifier and adjusting flows. 2150 Took hot-pot system out of service pending repair of pump seal. 6-20-73 AM Unit on hold preparing for morning operation. 0215/0225 Checked out TCV-2030 - OK. 0515 Transfer from regenerator to gasifier, and to 0520 hours - transfer from gasifier to regenerator. 0750 Started circulation. 0800 Started steam to boot, in process, lost interface. 1030 Regained interface. 1040 Started circulation of acceptor. 1055 Started steam to boot, all steam to boot at 1100 hours. Early AM Unit on "hold" condition. 0750 Dolomite circulation started. 0800 Steam introduced to gasifier boot, lost interface. Removed steam. 1000 Hot pot system put onstream, partially bypassed. Interface restored. 1100 Established steam flow to gasifier boot. 1300 Char transfer to regenerator begun. 1430 J-201A, gasifier compressor, shut in. During this period problems were encountered with plugging at the regenerator quench inlet venturi. Some pressure shakeups encountered. 302 Run IIB APPENDIX 11-B (Sheet 2 of 2) 6-21-73 1600 All recycle flow to regenerator shut in. 1730 Flow through LCV-2003 from gasifier to regenerator stopped, Circulation overhead through TCV-2030 stopped. Unable to regain circulation. Steam taken out of gasifier boot, J-201A compressor back on and recycle back in. 1800/1900 Blew up through gasifier to unplug. Shook up unit some. 1915 Transfer established through LCV-2003. 2100 Steam flow back into gasifier boot and recycle being cut back. Raising B-201-IA heater (heating steam). 2230 Recycle to gasifier boot cut off and J-201A compressor shut in . During this period, problems encountered with circulation of acceptor. 0100 Side flow to gasifier cut back. 0130 Lost interface. Cut out steam, recycle in. Cutting boot flow. 0200 Lost char transfer on regenerator due to low level in gasifier. 0202 Interface coming back. 0830 Decision made to shut down. DATE HOUR EVENT 7-9-73 7-10-73 1025 More air being added to gasifier to raise temperature. 1440 Power Failure! Lost power for 10 minutes. Plant brought back on stream OK - Lining out. 1820 Acceptor circulation started through TRC-2030, from regenerator to gasifier. 1850 Acceptor circulation started through LIC-2003, from gasifier to regenerator. 2030 Char transfer from gasifier to regenerator begun. High pressure drop across venturi inlet nozzle to flue gas quench causing low compressor suction pressure. 2330 Calcination curve plot indicates calcination to be complete. During this time, the valve loading (to increase circulation of acceptor overhead) on TRC-2030 increased up to 10 psi, 0320 Lost circulation through TRC-2030 for no known reason. Tried all known methods of recovery to no avail. 0730 Regained circulation. 1830 Decision made to shut down. 303 APl'BNDIX 11-C-l SHUTDOWN LIST Repairs and Revisions Between Runs 10 and 11 (1) Clean ball valves on sample stations on F-207 A/B Ash Lockhoppers, 4th floor. (2) Cooling tower shutdown. Clean basin and sump and install new screens between basin and sump. (3) Clean or replace element in HPC side stream filter L-303. Also, repair block valves around filter, they leak through, (MWO-5321, IWD) (4) Change print out of gasifier and regenerator TR's to record on individual temperature recorders for each vessel. This will include installing a new metal duct. Job P-3-73-6, X-36000, EWO-0639, (5) Install purge gate valves below lignite lockhoppers. Job A-200-11-72-2, X- 30400, EWO-0610. (6) Install drain valves for the purpose of emptying lockhoppers F-204 A/B and F-206 per DWG's LN-204 and CD-201. Job A-200-4-73-8, X-39300, EWO-0735. (7) Install operable level gauge glass on F-223 Ash Slurry Tank, Job A- 200-11-72-6, X-30900, EWO-0517. (8) Reroute line WQ-331 to prevent solids build-up in gasifier venturi scrubber, L-314. Job A-300-2-72-1, X-34600, EWO-0546, (9) Install flushing system to clean out C-301 exchanger while on stream, Eng. (10) Relocate sample station on S-8 (preheater to F-204 A/B) , Eng, Ball valves have not yet arrived, (11) Install gravitar seats in blue handled ball valves in S-9 and S-10 sample stations. Seats not here yet, (12) Install coil supports in B-203 heater. Eng, (13) Install heat packs on FT-2113 A/B and dPT-2028. (MWO-4187 and 4188) (14) Remove, inspect and clean suction bottles and gas by-pass piping on J-201 A/B compressors. (MWO-5278, JEG) (15) Remove 180 under engager pot for emptying regenerator, (fWO-5293, WWD) (16) Pull old dP basket on regenerator top head for vessel operation. (MWO-5294, WIVD) (17) Remove spool piece upstream of regenerator quench tower inlet venturi for inspection. (MWO-5295, WWD) (18) Open and clean F-319, (MWO-5297, WWD) (19) Open and clean F-321, (^fWO-5296, WWD) (20) Inspect J-201 A/B and clean discharge blowdown lines. (MWO-5265, IVWD) 304 APPENDIX 11-C-l (Sheet 2 of 5) (21) Raise gasifier dP probe for vessel inspection. (22) Instrument Department: a. Stroke control valves for 2 vessel operation. b. Calibrate instruments (recorders, indicators) on the board. c. Check alarm switches on panel board. d. Loop check instrument lines on purge drawing SK-245 and make sure purge taps are clear. e. Calibrate dP and flow transmitters for 2 vessel operation. (23) Clean 6th floor purge FI's. (MWO-5240, RED) (24) Install a WR in 200 Control Room for F-206 fresh dolomite hopper. (25) Cut and inspect where the two hot spots are located in line CD-206. Just exit of regenerator, 7th floor. (MWO-5269, RED) (26) Inspect hot spot on line CO-204 on first floor. (MWO-5299, WIVD) (27) Pull LCV-2002 for inspection and repair. (MlVO-5300, WWD) (28) Pull LCV-2003, line CD-204, for inspection and cleaning of line. Rotate line if necessary. (MWO-5298, WWD) (29) Inspect UAD-206 and XCV-2073, gasifier to F-213. (MlVO-5266, WIVD) (30) Remove LCV-3002 in E-302 water outlet line, for cleaning and inspection. Also clean line above this valve. (MWO-5268, WWD) (31) TCV-2030: Repair manual air loading station on 200 Control Room panel. It is erratic and sticks at 3# A/L. (MWO-5267, WWD) (32) Pull "T" below gasifier and remove distributor. (MWO-3591, JCG) (33) Clean the pressure taps in the gasifier probe for dPT '5-2034 and 2035. (MWO-5264, WWD) (34) Repair mechanical seal on gasifier quench water pumps J-301-A/B. (MWO-5207, 5213, RED) (35) Disconnect continuous blowdown line from boiler feed water line on 3rd floor going to regenerator quench tower venturi inlet on 4th floor. (MWO-5238, RED) (36) Rig a temporary hose under F-204-A lockhopper for emptying to tote bin. (MWO-5270, RED) (37) Replace leaky gasket on J-304 hot pot charge pump, 2nd floor. (MWO-5272, RED) (38) Take plugs out and reconnect line from drain on flue gas K.O. pot F-304 back to hot pot absorber E-305, 2nd floor. (^W0-5271, RED) (39) Remove and inspect XCV-2096 above F-204B. Leaks during operation. (MWO-5273, RED) (40) Repair steam block valve downstream of FCV-3014, 3rd floor. Handle is loose. (MlVO-5274, RED) 305 APPENDIX 11-C-l (Sheet 3 of 5J (41) Remove and inspect all four posi-seal valves above F-207 A/B ash lockhoppers (MWO-5275, RED) (42) Clean sight glass on F-319. (MWO-5201, RED) (43) Slide gate on 8th floor to F-204 A/B lockhoppers is hard to open and close. Also, need some kind of cover to keep char dust blowing back up onto floor (MWO-5202, RED) (44) Repair thermocouple TE-2288 on lift line of dolomite to regenerator (MWO-5205 RED) (45) B-201-IA outlet: Take TR-2058 out of parallel with TE-2187 and repair TE-2058 thermocouple. Repair thermowell on TE-2058 and examine thermowell on TE-2187 for a hole. (MWO-5204, RED) (46) B-203 heater outlet: Take TR-2047 out of parallel with TE-2115 and repair TE-2047. MWO-5203, RED) (47) Unplug sample point S-9, 6th floor and also rotate line CD-206 to take TCV-2030 out to unplug. (MWO-5241, RED) (48) Remove, inspect and clean regenerator and gasifier dP and TE side taps and repair as necessary including thermowells. (^W0-3768, FAP) (49) Remove breeching on B-201-IA and IB heaters for inspection. (MWO-3592, JCG) (50) Remove burner on B-203 heater for inspection. (MWO-3593, JCG) (51) Rotate line CO-202 at 4th floor for inspection and cleaning. (MWO-3594, JCG) (52) Repair TE-2057 and its thermowell. The TE is broken off in the damaged thermowell. B-201-IB heater outlet, (MWO-3595, JCG) (53) Install Cameron test ball valve complete with operator in line to lignite lockhopper. A-200-11-72-2, X-30400, EWO . (54) Install C-313 in parallel with C-303. A-300-5-73-5, X-42000, EWO. (55) Replace CO-202-2"-SlC with CO-202-3"-SlC. Install 4" XCV-2004 on gasifier nozzle Utilize LCV-2000. A-200-5-73-17, X-42600, EWO. (56) Remove grid from D-101. Install 6" ring half way up in bottom cone. A-100-5-73-1 X-05700, EWO. (57) Modify the two top regenerator side tap configurations to same as the bottom three side taps. A-300-6-73-1, 01X15800, Eng. Consol request. (58) Design and install water nozzles for regenerator quench tower venturi nozzles A- 300-5-73-2, X-41700, EWO. (59) Install modified sample point S-13. P-11-72-1, X-30500, EWO. (60) Reconnect dPT-2034 and dPT-2035. Reinstall control circuit. EWO. (61) Install EOV's in purge gas to air actuated posi-seal valves above ash lockhoppers Eng. 306 APPENDIX 11-C-l (Sheet 4 of 5) (62) Relocate the source of purge to L-513 I.G. dryers from current location on 350# I.G. header inside of utility room to upstream of 350# header block valve which is upstream of 350# pressure controller. (NfWO-3654, NRK) (63) Pull graylock fitting on gasifier top head for vessel inspection. (MWO-3596, JCG) (64) Remove XCV-2085 and XCV-2086 for inspection and cleaning. Reinstall upon approval. Solids inlet to F-204 A/B lockhoppers . (MlVO-3597, JCG) (65) Open manway on F-213 dolomite out hopper for vessel inspection and cleaning. Button up upon approval. (MWO-3599, JCG) (66) Remove insulation from around B-201-IA and IB outlet headers for inspection by Alan Crockett. (MWO-3600, JCG) (67) Unplug drain from 1st floor to MH #2. (MWO-5211) (68) Open D-101 top manway for cleaning of vessel. (MlVO-5216) (69) Overlay heater tube in B-201-IB heater. (MWO-3701, JCG) (70) Remove gasifier bottom head for replacement of the 2" liner pipe in nozzle "G" with a 3" liner pipe. (MWO-3702, JCG) (71) Check and replace if necessary the following TE's: TE-2320, Skin on B-201-IB (reads ambient) TE-2327, Skin on B-201-IA (reads low) TE-2299, Process B-201-IA (reads low) TE-2037, Gasifier probe, Pt. 44 on TE-2001 (reads low) TE-2313, Regenerator Pt. 31 on TI-2001 (lost reading) (72) Add three alternates for low side of dPT-2030. EWO-0810. (73) Repair broken probe supports in the gasifier. (MWO-370S, JCG) (74) Remove cast iron plug from bottom of regenerator. (^■1WO-3706, JCG) (75) Blind air line between GA-208 and AP-509 at union near connection to AP-509 under heater deck. (MlVO-3655, NRK) (76) Remove, inspect CO-204 and reinstall F-224, char stop pot. (MWO-3656, NRK) (77) Install restriction orifices in B-201-IA and IB heater inlet passes. EWO (78) Modify steam addition system to gasifier boot. EWO (79) Install "no-block" purge fittings on gasifier. EWO (80) Pipe up CO^ from CO^ storage for use in side flow in gasifier. EWO (81) Install PCV on steam line to gasifier so steam is superheated at orifice plates. EWO 307 APPENDIX 11-C-l (Sheet 5 of 5) (82) Reinstall blind upstream of bypass valve at FCV-2013 station. (MV;0-3657, NRK) ^^'^ iTvTn'/tL'^'''^ thermowell on TE-2314, gasifier side - 4th floor, to extend 2" Deyond the end of the mside of the pressure tap. (MWO-3680, FAP) (84) Cut a 4V hole in the body of stage two of lignite preheater internal cyclone L-iib to disable cyclone - Consol request. (EWO-0110, MHV) (85) Install new G-6 sample point on 5th floor flanges on GP2-201 with a TI . EWO (86) Repair drain line on J-203 A/B blowdown pot, first floor. (MWO-3709, JCG) 308 ,0 APPENDIX ll-C-2 SHUTDOWN LIST Repairs and Revisions Between Runs llA and IIB (1) Remove 180"^ for regenerator dumping. (MlVO-3711, JCG) (2) Open F-3I9. [mO-3712, JCG) (3) Open F-321. (MWO-3713, JCG) (4J Remove spool piece upstream of regenerator quench venturi . (MWO-3714, JCG) (5) Pull basket in regenerator top head for inspection. (MIVO-371S, JCG) (6) Remove char stop pot F-224 for inspection and clearing of line CO-204. If necessary, open flange on bottom of char lift Y, 1st floor. (MlVO-3716, JCG) (7) Remove TCV-2030 for inspection and cleaning. Rotate line CD-206 if necessary (MWO-3718, JCG) c:>^cixy. (8) Remove gasifier "T" . (MlVO-3717, JCG) (9) Repair hot spot on line CD-208, 6th floor. (MWO-3719, JCG) (10) Replace section of damaged 2" inlet lines to F-207 A/B ash lockhoppers (MlVO-3720, JCG) ^^ (11) Remove LCV-3002, regenerator quench tower water outlet, for cleaning of valve and line. (mO-3721, JCG) (12) Replace TE-2311, regenerator side, PT-33 on TI-2001. (^WO-3722, JCG) (13) Repair or replace thermowell and thermocouple on TE-2187. B-201-IA outlet (MlVO-3684, FAP) (14) Repair or replace well on TE-2058. Present well has a hole in it. Also fMW? ^^^ ^^ ^"'^ replace if necessary. It was drifting during operation! (15) Check out B-203 heater and damper. Heater keeps kicking out. (MWO-3724, JCG) (16) Remove "no plug" purge fittings that were installed on FI-2280 and FI-2041 (MWO-372S, JCG) (17) Check dPR-2080 to see if the low and high sides are not reversed. (MWO-3726, JCG) (18) Clean 6th floor FI's per list. (MWO-3727, JCG) (19) Inspect J-201 and J-203 recycle compressors. (MWO-3728, JCG) (20) Repair leaks in FCV-2021 loop. Controller will not hold in seal position (MWO-3686, FAP) i • • (21) Repair hot spot in line CD-208, 3rd floor. (MWO-3729, JCG) (22) Open and clean suction lines to gasifier quench water pumps. (MWO-3730, JCG) 309 APPENDIX ll-C-2 (Sheet 2 of 2) (23) Remove, clean and repair XCV-2090 below F-204 B lockhopper. (MWO-5171, RED) (24) Remove regenerator top head for vessel cleaning. (MWO-3731, JCG) ^^^^ ?otfh-'°^'^''''°" ^^'^^^ ^"^ ^""'^^^ ^ temporary drain from XCV-2010 to tote bins for regenerator washing. (f.WO-3732, JCG) (26) Remove breeching from B-2010IA/IB heaters and burner from B-203 heater for inspection of heater tubes by Man Crockett. (fWO-3733, JCG) (27) Repair PCV-5152, 350 to 18.5 psig I.G. reducing station. (MWO-3687, FAP) (28) Drill 1/4;' diameter holes in the tops of the bubble caps on the regeneration air distributor. Holes to be drilled in the tops of the caps as cfose ?o ^L regenerator wall as possible. (MWO-3734, JCG) ''°^ ^i''\^iiitirMr'' '''-'' '" ^^^^"^-^""^ "^-^^°^ "i^h "-22 brush (31J Open regenerator overhead line GF-201-6" at flange on 6th floor at L-202 for inspection of line. (MWO-3663, NRK) '"^ r:;:ne?a?o"Leth IZf'^ i^Jl:-]Z^l^'-- ^^^ -"= -" ^"' :o::?^'i?^^:!:-1-,g„-?-« ^1-3So^=r:-e'ri^eJ"'1n:° —"^ -^^ (34) Unplug bypass valve at LCV-3002 (Regenerator Quench Tower). Plugged above top valve. (MWO-5129, EBW) ^i^ggea aoove (35) XCV-2010: Make valve operable to full range. (MWO-5175, NRK) (36) Remove top from B-201-IB heater and overlay tubes as necessary. (MlVO-3736, JCG) (37) Remove the 2'- grayloc fitting from the gasifier top head and provide a lieht for inspecting the gasifier interior. (MWO-3737, JCG) proviae a light tor ^''' Tz':\moTss'rvlh''' ''''"^''^ '^°" regenerator for removal of broken drill (39) Repair cause of hot spot on CD-208 below third floor. (MWO-3666, NRK) •CtV.S. GOVERNMENT PRINTING OFFirp. i « ^„ 1 riuiNuiNOUJ-HCE: 1979-6(^0- Qjiy ^^^^^ REGI0NN0.4 310