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A S rUDY OF rHE EXTRACTIVE ACTION 
 OF BENZENE AND XYLENE ON COAL 
 AT HIGH PRESSURES 
 
 BY 
 
 RICHARD STONER FISHER 
 
 THESIS 
 
 FOU THE 
 
 DEGKE1-: OF BACHEI.OR OF SCIENCE 
 
 IN 
 
 (HIEMISTRY 
 
 COLLEGE OF LIBERAL ARTS AND SCIENCES 
 
 UNIVERSITY OF ILLINOIS 
 
 1922 
 
Digitized by the Internet Archive 
 in 2015 
 
 https://archive.org/details/studyofextractivOOfish 
 
- A 
 
The writer wishes to acknowledge the ready advice 
 and helpful criticism of Dr . T. E. Layng in the work of which 
 this is the report. 
 
i 
 
TABLE OE CONTENTS 
 
 Page. 
 
 Introduction, 1. 
 
 The Carbonization of Coal. 2, 
 
 Historical 2. 
 
 Importance of Theory of Carbonization. 4. 
 
 Methods of Attacking the Problem. 5. 
 
 I. The Fractional Carbonization of Coal. 7. 
 
 II. The Action of Solvents on Coal. 10, 
 
 Existing Status of the Theory of Carbonization. 12. 
 The Purpose of this Investigation. 13. 
 
 Experimental. 14. 
 
 Conclusions, 17. 
 
 Data. 19. 
 
 Bibliography. 25, 
 
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-1 
 
 A STUDY OF 
 
 THE EXTRACTIVE ACTION OF BENZENE AND XYLENE 
 ON COAL AT HIGH PRESSURES. 
 
 INTRODUCTION. 
 
 The primary purpose of a study of the products obtained 
 by the action of solvents on coal is to formulate a workable the- 
 ory of coal carbonization. Of all industrial operations which are 
 carried out on such an immense scale, the manufact'ure of coke is 
 perhaps the least understood. In spite of the great advance the 
 industry has made in substituting the by-product recovery oven for 
 the older bee-hive type, the carbonization of coal is still very 
 largely a rule of thumb process. 
 
 Why, then, a tneory of carbonizat ion? Gooa co^e is 
 made by the present methods. One - half of the world’s supply of 
 coal is in the United States . What need is there of knowing the 
 details of how coke is formed as long as plenty of good coke can 
 be made without that ^inowleage? The best answer to this query is 
 the fact tliat at the present rate of consumption, the available 
 supply of coal fit for coking will be exhausted in the next fifty 
 years. Since coal is such a very bulky substance, it is cheaper 
 to ship iron ore to the country which produces the coal than to 
 import the coal necessary for metallurgical processes. Thus no 
 country which does not have an adequate supply of coal from which 
 good metallurgical coke can be made can hope to be a great pro- 
 ducer of iron and steel goods no matter what the quantity and the 
 quality of its iron ore. 
 

 
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 It is imperative, then, if we wish to retain our pres- 
 ent position as a great steel manufacturing nation, tmt some 
 method he found to coke these coals which are at present regarded 
 as non - coking. Obviously the best way to go about finding why 
 anthracites and some of the lower grades of coal will not coke is 
 to find how and v/hy the so called "coking” coals do form coke. 
 
 To that end v?e must direct our attention to a study of the devel- 
 opment of a theory of carbonization, 
 
 THE CARBONIZATION OR COAL, 
 
 Coal carbonization aims at the production of coke. 
 According to V . B. Lewes (2)^, coxe is "the name given to the 
 solid residue left by the destructive distillation of coal and 
 many other carbonacous substances, and contains as its chief con- 
 stituent carbon, together with the mineral matter or ash of the 
 original body, such portions of the residues as the tenperature 
 employed has failed to drive out of the mass, and occluded gasesV, 
 
 HISTORICAL 
 
 The carbonization of coal to form coke grew out of the 
 necessity of finding a substitute for charcoal. Charcoal had 
 been, up to this time, the main fuel used in extracting iron from 
 its ores, but the supply of wood available for the production of 
 charcoal was rapidly being exhausted. The first attempts to coke 
 
 coal were quite naturally patterned after the methods then in 
 general use in charcoal burning. Cocil was heaped on the ground, 
 ignited, and plastered with wet coal dust to blanket combustion. 
 
 ^N. B. Numbers in parenthesis refer to bibliography. 
 

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 Later a sinall chimney was introducea in the center of the coal 
 mass to allow free escape of the ^ases . The pile of coal was ig- 
 nited hy introducing burning coal through this chimney and com- 
 bustion was checlced as before. This method of coke manufacture 
 was, of course, very wasteful. Not only the gas evolved but even 
 a part of the coal itself was consumed in heating the mass. The 
 old bee - hive coke oven grew out of this early practice, these 
 ovens, Duilt in groups of heavy masonry, had the effect of retain- 
 
 I 
 
 ing the heat better than the old ”meiler” heaps. But the ovens 
 were still heated by the destruction of all the gaseous products 
 of distillation and a part of the coal itself. Gradually we have 
 come to a realization of the ijnmense value of the by - products of 
 coal distillation, and to the conviction that we have too long 
 been wasting our natural resources. The by - product coke oven 
 has come into wide use as a direct result of this feeling, togeth- 
 er with the greater economy of operation. These ovens are fired 
 externally and the valuable products are recovered before the gas 
 is burned to heat the ovens. 
 
 At the same time has come a somewhat similar development 
 of the other of the carbonization industries - gas manufacture. 
 
 The growth of this industry has been marked by a doggeo singleness 
 of purpose which has at times overlooked the best interests of the 
 industry as a whole.. Gas production managers have been intent 
 upon obtaining the largest possible volume of gas from a ton of 
 coal. In doing this they have frequently been guilty of forgetting 
 quality in their search for quantity. They have also, up to this 
 time, steadily refused to devote any thought to a possible improve- 
 ment of the coke produced as a by - product of the industry. Coke 
 in the gas industry has always been considered more of a necessary 
 
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 evil that a possible source of profit. The result has been an 
 inferior quality of coke - porous, friable, and hard to dispose 
 of. It is to be hoped that the gas manufacturer will soon take a 
 more lively interest in fuel conservation and, by using a some- 
 what lower temperature and paying a little more attention to the 
 coke produced, give us a better quality of gas and^ample quantity 
 of coke which, if not adaptable to metallurgical uses, may be 
 used extensively for domestic purposes. Such a coke - cheap, and 
 easily ignited would be a boon to our smoke infested cities. 
 
 IMPORTANCE OE THEORY OF CARBONIZATION. 
 
 What, then, is the problem involved in the theory of 
 carbonization? Good coke is being made every day. What more do 
 we want? The problem is simply this. Only certain, rather def- 
 initely restricted classes of coal will coke. Why is this? What 
 makes coal coke? What is lacking in anthracites tnat they will 
 not coke? Why will lignites not coxe? Can these non - coking 
 coals be made to coke? These are some of the questi or.s facing 
 the carbonization industries today. Why do we want to coke these 
 coals? We have coal enough to supply us with metallurgical coke 
 for many years . Why not burn the rest raw? Because when raw 
 coal is burned in the ordinary type of domestic furnace from 60 - 
 80 % is wasted. V/orse, for this waste is also responsible for the 
 great smoke nuisance in the cities and so impairs the cheerfulness 
 
 and even the health of the inhabitants. If coke were used exclu- 
 sively for domestic and office heating, great wealth in the form 
 of dye - stuffs, medicinal basis, germicides, fertilizers, and 
 light oils for use as a substitute for gasoline, would be saved 
 
 every year 
 
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 METHODS OE ATTACKING THE PROBLEM. 
 
 Three methods have been used in attacking the problem 
 of obtaining a satisfactory theory for the carbonization of coal. 
 These are:- 
 
 1. Microscopic examination . 
 
 2. Low temperature carbonization. 
 
 3. The action of solvents on coal. 
 
 Reinhardt Thiessen (3), has done sojne very exact work 
 on the microscopic examination of coal. However, since this phc^se 
 of the work has more bearing on the ident if icat ion and examination 
 of the individual constituents of coal than on any definite theory 
 of carbonization, we will at present consider the last two means 
 of attack. A very interesting theory of the formation of coal 
 has been built up around this work of Thiessen by David V/hite . (3) 
 We will consider -White’s theory a little later in connection with 
 a preliminary study of the constitution and formation of coal. 
 
 Before starting on a review of the work that has been 
 done in the fields of low temperature carbonization and solvent 
 action it will be well to present some of the ideas and accepted 
 facts concerning the substance and origin of coal. What is coal? 
 Where did it come from? Almost any school boy will embark glibly 
 enough on an explanation of the latter question, but ask him what 
 coal is and he has no answer. Or he may say that coal is carbon 
 and class it with diamond and graphite as a form of that element. 
 
 As a matter of fact there is probably no free carbon in coal. And 
 when it comes to an attempt to enumerate the substances present in 
 coal we may as well admit that we do not know. We only know that 
 coal contains compounds of carbon, hydrogen, oxygen, nitrogen, and 
 sulpher arranged in innumerable chemical combinations and mixed 
 
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 with inert mineral matter in varying proportions. This complica- 
 ted structure of coal together with the fact that coals from the 
 same neighborhood may be widely different in character, is very 
 largely responsible for the altogether different results which 
 may be obtained by two independent investigators working on simi- 
 lar problems. In 1878, Green defined coal as "a compact stratified 
 mass of mumified plants subjected to arrested decay in various 
 stages of completeness and free from all except a very low percent- 
 age of foreign material". 
 
 White ( 3) claims that all coal was laid do’vn in beds an- 
 alagous to our peat beds of today. All kinds of vegetation from 
 the largest club mosses to the smallest fungi went into the depos- 
 its. Hence the wide divergence in the characters of different 
 coals . The climatic conditions existing at the time were very 
 largely responsible for the formation and burial of these peat beds 
 The warm atmosphere led to a quick luxuriant growth which, because 
 of the coarse structure due to such rapid growth, was easily at- 
 tacked by decay. According to White, one foot of surface peat was 
 laid down in ten years. Because of dehydration and densif icat ion 
 caused by the increased pressure and temperature, it would take 
 about one hundred years to get a one foot stratum of peat twenty 
 feet below the surface of the ground. Three feet of this compress- 
 ed peat would be required to produce a one foot stratum of coal. 
 
 The change from the original vegetable matter to coal is divided 
 into two parts. First, the dead vegetable matter is subjected to 
 biochemical reactions to give peat. Then the peat is buried and 
 subjected to dynamo chemical processes to form coal. Plant mater- 
 ials are composed chiefly of celluloses and proteins. The cellu- 
 losic part makes up the large bulk to form a framework. The pro- 
 

 
 
 
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- 7 - 
 
 teins are concerned in the vital functions of the plant. These 
 compounds differ widely in their resistance to various agencies. 
 The proteins are relatively unstable while the celluloses are 
 attacked with more difficulty. 
 
 At the death of the plant, governed by conditions in 
 the bog, a partial decomposition, elimination, and chemical re- 
 duction sets in. This biochemical change is brought about chief- 
 ly by organic agencies - fungi at first and bacteria later. The 
 most volatile parts of t plant constituents are removed first, 
 the next follow, etc., until the most resistant parts are left in 
 a residue called peat. This process of decomposition and reduct- 
 ion, begian in the peat cniefly by biochemical means, is taken up 
 and continued by dynamo chemi cal agencies into and through succes- 
 sive stages of de coiiposition into the various grades of coal. 
 
 So much for the composition and formation of coal. We will now 
 turn our attention to the most common methods of studying coal 
 carboni zati on, 
 
 THE FRACTIONAL CARBONIZATION OP COAL. 
 
 The classic example of carbonizati on work is that done 
 in England by Burgess and Wheeler (4). Similar work has been 
 more recently attempted in this country by Porter and Tlaylor (5), 
 The results and conclusions drawn by Porter and Taylor differ 
 widely from those of Burgess and Wheeler. This does not mean at 
 all that the results of one or tne other were in error,, for the 
 experiments were both carried out with great care, but it does 
 show the effect of a different grade of coal studied under slight 
 ly different conditions by different men. The personal equation 
 plays an important part in such studies of coal. 
 
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- 8 - 
 
 Studying the gaseous products obtained from 200 grams 
 of powdered South Yorks, Silkstone bituminous coal at temperatures 
 of 100’, 200’, 300*, 3t0*, 400’, and 450’C, Burgess ana Wheeler 
 reached the following conclusions: 
 
 Coal contains two types of compounds of different de- 
 grees of ease of decomposition; the one, the least stable, yield- 
 ing the paraffin hydrocarbons and no hydrogen; the other, decom- 
 posing with greater difficulty and yielding hydrogen alone or hy- 
 drogen and the oxides of carbon. Probably the difference between 
 one coal and another is determined mainly by the proportions in 
 which these two types of compounds exist, anthracite, for example, 
 containing but little of the more unstable constituent. The pres- 
 ence of carbon monoxide is more probably due to the liberation of 
 water from hydroxy compounds and the subsequent reaction of the 
 steam thus formed with carbon. In a later paper Wheeler states 
 that he believes that the hydrogen yielding constituent is what 
 he calls the "cellulosic" and the paraffin yielding the ’’resinic” 
 part of the coal. The experimental work of Burgess and Wheeler 
 has been confirmed by similar work carried out by Vignon on some 
 French coals. Vignon’ s discovery of a critical temperature be- 
 tween 700’ and 800’C., at which there is a marked increase in 
 the evolution of hydrogen. 
 
 The conclusions drav/n by Burgess and V/heeler have, how- 
 ever, been severely criticised by Porter and Taylor(5). These 
 investigatorsaob j ect to the statement that after all the less 
 stable paraffin yielding ’’resinic” constituent has been decom- 
 posed, tne decomposition of tne more stable hydrogen yielding 
 
 ’’cellulosic" part sets in about 700’C. Wheeler’s statement that 
 water of decomposition begins to be evolved about 200’C., shov/s 
 
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-9- 
 
 that a partial decomposition of the "cellulosic” constituent has 
 "begun at that early point. Porter and Taylor found that: 
 
 1. More tiian two - thirds of the organic su’Dstance of 
 coal is decomposed "below bOO’C., but there is a variation among 
 different kinds of coal in their ease of decomposition. 
 
 2. The first decomposition occurring in any type of coal 
 
 as the temperature is raised is the breaking dov/n of certain oxy- 
 gen - bearing substances related to cellulose, from which chiefly 
 water of decomposition, COj?* CO. are produced, 
 
 3. Other decompositions, producing paraffins both liq- 
 uid a/h. gaseous, begin at an early stage. Vlliether or not such de- 
 compositions become the predominating type below 500’C. depends on 
 the character of the coal, and, as a general rule, the higher the 
 oxygen in the coal, the less will be the proportion of hydrocar- 
 bons and tax in the volatile matter. 
 
 4. Secondary decompositions of the primary volatile pro- 
 ducts occur quickly and easily at temperatures of 730’C., and 
 above. 
 
 The theoretical conclusions which Porter and Taylor 
 have drawn from these results are as follows: 
 
 "All kinds of coal consist of cellulosic degradation 
 products more or less altered by the processes of aging, together 
 with derivatives of resinous substances, vegetable waxes, etc., in 
 different proportions more or less altered. They all undergo de- 
 composition by a moderate degree of heat, some, however, decom- 
 posing more rapidly than others at the lower temperatures. The 
 less altered cellulosic derivatives decompose more easily than 
 
 the more alteied derivatives and also more easily tiisn the resin- 
 ous derivatives. The cellulosic derivatives decompose so as to 
 
A 
 
- 10 - 
 
 yield water, caroon monoxide, carbon dioxide, and hydrocarbons, 
 giving less of the first three products the more matured and alt- 
 ered they are. The resinous derivatives, on the other hand, de-e 
 compose on moderate heating so as to yield principally the par- 
 affin hydrocarbons, with probably hydrogen as a direct decomposi- 
 tion product. The more mature bituminous coals, having good cok- 
 ing properties, contain a large percentage of resinous derivatives, 
 and their cellulosic . constituents have been highly altered. The 
 younger bituminous or sub - bituminous coals are constituted of 
 cellulosic derivatives much less altered than those in the older 
 coals. They undergo a large amount of decomposition below their 
 fusion point and possibly for that reason many of them do not coke! 
 
 THE ACTION OF SOLVENTS ON COAL. 
 
 parts: 
 
 The study of solvent action should be divided into two 
 
 1. The action of reagents which separates out some of 
 the constituents of coal in an altered form. Under this head come 
 sulphuric and nitric acids, potassium and sodium hydroxides, py- 
 ridine, aniline, quinoline, phenol, bromine, and oxygen. 
 
 2. True solvent action which is believed to extract 
 from the coal substance some of the unchanged coal constituents. 
 Some of the substances which are supposed to exert only a solvent 
 action on coal are benzene, chloroform, alcohol, ether, petroleum, 
 ether, acetone, toluene, xylene, and di - phenyl ether. 
 
 The action of reagents we must pass over without much 
 
 discussion. No results obtained from a study of bodies extracted 
 
 from coal by such reagents ceui carry much weight because the ex- 
 istance of such bodies as such in coal cannot be definitely proved 
 

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- 11 - 
 
 For instance, it has heen found that the substarice obtained from 
 coal by extraction with pyridine usually contains almost twice tne 
 amount of nitrogen as was originally present in the coal . This 
 shows that the pyridine oase has entered into combination with 
 some of the acidic substances of the coal maicing any further study 
 of the products obtained useless. 
 
 In regard to solvent action, Bone (l) says: 
 
 » The difficulty is to find solvents that will differen- 
 tiate sufficiently between the main constituents of the coal and 
 extract a large proportion of some one of them, without at the 
 same time having some depolymerising or other sinilar action upon 
 the whole structure". Most of the solvents which, without much 
 question, do extract the coal constituents unchanged do so in 
 such minute quantities as to make the task of obtaining sufficient 
 amounts of the substances for experimental purposes almost hope- 
 less, J. A. Smythe (1) found that ethyl ether and petroleum e- 
 ther had very little effect on the coal while benzene, chloro- 
 form, and alcohol extracted quantities varying between 1.8 and 
 3.0 percent of the coal. Similar experiments have been more re- 
 cently carries out by many v/orkers with practically the seone re- 
 sults , 
 
 Interesting possibilities are disclosed in some recent 
 work by Fischer and Gluud (1) in Berlin on the action of benzene 
 on coals at pressures of some 50 atmospheres. By using a temper- 
 ature of 270’ C,, and a pressure of 55 atmospheres, 6.7 % of ex- 
 tract was obtained from a coal which had previously yielded only 
 0.1 % on extraction with boiling benzene. No study of the pro- 
 ducts obtained was made aside from the determination of their 
 physical properties. No proof was offered that, at the temper- 
 
- 12 - 
 
 atures employed, decomposition did occur except that no gas was 
 noticed on opening the cooled homb. In one of the experiments, 
 hydrogen sulphide- gas was noticed on opening the bomb. This was 
 taken as an indication that some decomposition had occurred. This 
 work of Pischer and Gluud, however, undoubtedly opens up great 
 possibilities of finding a means of obtaining sufficient quanti- 
 ties of such extracts from coal for farther experimental work. 
 
 EXISTING STATUS OF THE THEORY OF CARBONIZATION. 
 
 The existing theories of coal carbonization have been 
 very well crystallized in the following statement of Lewes’ opin- 
 ion: 
 
 "Many theories have been put forward as to the nature 
 of the binding material in coke. Some declare tl^iat it is the re- 
 siduum of the semi - fused constituents in coal, whilst Wedding 
 and others consider that it is carbon deposited by the decomposi- 
 tion of heavy hydrocarbon vapors, v;hich is undoubtedly the cause 
 of the carbon hairs found in coking. It seems most probable, how- 
 ever, that the cementing material is due to liquid products, the 
 most volatile of which are driven off as vapors, leaving pitch, 
 which carbonizes and binds the mass into coke". 
 
 A somewhat different theory has been recently aavanced 
 by Dr. T. E. Layn^ of the University of Illinois, 
 
 For the formation of good coke three conditions must 
 be fulfilled. 
 
 1. There must be a bond forming material present. 
 
 2. The material to be bonded must have delivered all 
 
 of the adsorbed oxygen and oxides of carbon before the decorapo- 
 ^This theory was presented in class room discussion. 
 

 
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-13 
 
 sition of the bond forming material. 
 
 3. The bond forming material must not distil without 
 decomposition. 
 
 As may be readily seen, this theory conforms well to a 
 number of well known facts about the coking of coal. Anthracites 
 will not coke because they lack the bond forming material. The 
 better grades of bituminous coals conform to all three conditions 
 and therefore give good coke . The lower grades of bituminous 
 coals and lignites are easily oxidizable. Oxygen is adsorbed and 
 the oxiaes of carbon are formed. These gases are liberated at 
 the time of the decomposition of the bond forming material and 
 prevent good contact of the bonding material with the material to 
 be bonded. 
 
 THE PURPOSE OF THIS INVESTIGATION. 
 
 The purpose of this investigation is two - fold: 
 
 First, to find, if possible some method of extracting 
 the coking constituent from coal in satisfactory quantities and 
 with as little change as possible. 
 
 Second, to investigate, with the aid of the substances 
 obtained from the coal, the above theories of carbonization. 
 

 
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- 14 - 
 
 exp ERIMENTAL ^ 
 
 Extraction of Coal with Benzene under Pressure. 
 
 Various forms of bomhs were t.ried in the heginning of 
 this work. The first type used was a small model of the steel 
 tomb used by Fischer and Gluud. A seven inch length of four inch 
 steel pipe was threaded at both ends and fitted with caps. A 
 mixture of litharge and glycerine was used as a cementing agent 
 and later lead was melted into tne caps in an attempt to make the 
 bomb leak - proof, but tne pressure desired could not be main- 
 tained. In the second attempt several ten inch lengths of one 
 inch pipe welded at one end and fitted with a cap at the other 
 were used. This type was also discarded because the capacity was 
 too small and leaks still developed. The most satisfactory re- 
 sults obtained were with tne use of an empty mercury container. 
 100 grams of coal powdered to pass a sixty mesh sieve and about 
 two liters of benzene were charged into the bomb and the plug 
 screwed in tightly and sealed with a smoothly mixed paste of 
 litharge and glycerine. This bomb was found to be almost entire- 
 ly leak - proof at the pressures used. The analysis of the coal 
 used which was from Franklin County, Illinois, is given in Table 
 ' 1 , of the section devoted to data. The bomb was placed in an 
 electric furnace and kept at a temperature of from 210’ to 240’C. 
 for 24 - 48 hours, (see table 2). At the end of this time the 
 bomb was opened and tne solvent was decanted off rapidly through 
 a suction filter leaving as much of tne coal as possible in the 
 bomb. Any coal on the filtor was returned to the bomb and fresh 
 solvent was added as before. The benzene solution of the third 
 
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of these extractions was practically colorless showing that all 
 of the material extractable with benzene was reirioved in the first 
 two extractions. The benzene solution of the extract was strongly 
 fluorescent. This solution was again filtered to remove the last 
 traces of suspended coal and evaporated to dryness in a current of 
 nitrogen. The residual coal after the last extr section was W8.shed 
 on the filter with alcohol, then with ether and dried in a cur- 
 rent of nitrogen. The proceedure in the case of the extractions 
 with xylene was exactly the same excepting that seven extractions 
 were necessary to completely exhaust the coal of extractable ma- 
 terial. The results (see table 3), show that in the case of the 
 xylene extractions approximately one - fourth of the coal sub- 
 stance was disolved out of the coal under conditions of temper- 
 ature and pressure which preclude any possibility of decomposi- 
 tion of either the coal or the solvent. 
 
 The comparison between the ultimate analysis of the 
 coal, extract, a.nd residue shows a close agreement in the values 
 obtained for the analysis of the coal by actual experiment and 
 by calculation from the corresponding values of the extract and 
 residue. The value obtained for sulpher is too low. This may 
 be ascribed to a loss of some of the more volatile organic sul- 
 pher compounds due to exposure to the temperature necessary to 
 drive off the last traces of the xylene from the extract. The 
 values for oxygen and hydrogen reflect the high heat value caused 
 by some of the solvent not removed from the residue and possibly 
 from the extract. The analysis of the residue was corrected for 
 an ash value which was too high, due to extraneous material from 
 the bcanb and the litharge glycerine mixture used to seal it. 
 

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 ■j r i 
 
 .•. 4 V *>. ;■ i .' ' . ■■ 
 
 I 
 
 ■; 5 1 
 
 ,f J- 
 
 ‘ x ',‘ 
 
 • • 1 . •J U'’i* n/» 
 
 
 « / i • j ‘ 
 
 / ,..n 
 
 Tt^: 
 
 
 .•^AT. 
 
 I'i'A, 
 
16 
 
 The carbonization data (see Tables 5 and 6) is of 
 interest both as a support of Dr. Layng’s tneory of carbonization 
 and as farther evidence in the controversy between Burgess and 
 Wheeler on the one hand, and Porter and Taylor on the other. The 
 main constituents of the gases obtained from a carbonization of 
 the residue up to 350* C,. are oxygen and carbon dioxide. Between 
 350’ and 450’C., the residue, which corresponds to what Wheeler 
 calls the ” cellulosic" part of coal, yields mainly hydrogen, oxy- 
 gen, and the oxides of carbon together with quite a large percent- 
 age of hydrocarbons of the marsh gas series. In the carboniza- 
 tion of the residue, the evolution of hydrogen sulphide was first 
 noticed at 420’C. No tar was noticed in the distillation of the 
 residue. 
 
 The fraction of gases collected from the extract up to 
 350’C., contained mainly hydrocarbons of the marsh gas series 
 with appreciable quantities of hydrogen, carbon monoxide and oxy- 
 gen. The fraction from 350’ - 450’C., consisted mainly of hydro- 
 gen with some hydrocarbons. Hydrogen sulphide evolution began aL 
 240’ C. A large quantity of tar of specific gravity less tnan one 
 was collected. 
 
 Various coking tests were made and are tabuleb od after 
 Table 6 in the data. 
 

 ■’ 
 
 
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 ■ ■ ■'■ ' ■ , ' ■ ^ . ' ' -. V' \ ^r^Tir ,. ..^ 
 
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-17 
 
 CONCLUSIONS, 
 
 1. In the opinion of the writer, the most important 
 result obtained in this investigation was the discovery of a new 
 method of extracting the coking constituent of coal in quantities 
 large enough for experimental purposes. The coking tests made 
 were all upon one gram samples and as such are possibly not en- 
 tirely indicative of the results which may be obtained on larger 
 samples. The writer believes that work along the line herein ex- 
 plained will go on in these laboratories and that extractions will 
 probably be made on several kilos of coal at a time in autoclaves 
 using xylene as a solvent. In this way enough of the coking con- 
 stituent could be obtained in the course of several weeks to per- 
 mit more exhaustive investigations, 
 
 2. The results obtained from the fractional carboniza- 
 tion of the extract and residue seem to indicate tJriat both sides 
 are right in the controversy between Burgess and Wlieeler, end 
 Porter and Taylor. The main constituents of the gas obtained 
 from the residue up to 3fcO*C., are oxygen and the oxides of car- 
 bon. The largest single constituent of the gas from the residue 
 between 350 and 450* C., is hydrogen, in accordance with the claims 
 of Burgess and Wheeler. The extract, in the lower fraction, yields 
 mainly the paraffin hydrocarbons as is agreed by both factions, 
 but in the fraction from 350* - 450*0., the main constituent is 
 again hydrogen which agrees with the results of Porter and Taylor, 
 but is contradictory to those of Burgess and Wheeler. 
 
 The sharp distribution of organic and pyritic sulpher 
 
 between the extract and the residue is shown by the fact that the 
 evolution of hydrogen sulphide from the extract begins at 240*0., 
 
-18- 
 
 while in the case of the residue it is not apparent until 420’ C,, 
 is reached. 
 
 The coking tests which were made tend to substantiate 
 the theory of carbonization which has already been attributea to 
 Dr. Layng of this University. The residue from the xylene extract 
 ion showed no coking tendency whatever. This shows the effect 
 produced when the bond forming niateris.1 is removed. When the 
 extract and residue were mixed in the correct proportions, a good 
 hard coke was obtained. Oxidized residue mixed with the correct m 
 amount of extract gave a very soft sooty coke. After carboniza- 
 tion some of this ixidized residue was again mixed with extract a 
 and yielded a good, hard coke. This test show’s the effect of oxy- 
 gen on the residue where it is unprotected by the extractable por- 
 tion. Oxygen is adsorbed and combines with the coal substance. 
 Oxygen and the oxides of carbon are liberated at the temperature 
 of decomposition of the bond forming material and tend to pre- 
 vent the formation of a suitable bond. 
 
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 -19- 
 
 
 
 DATA 
 
 
 
 Table 1, 
 
 
 The Proximate 
 
 and Ultimate Analysis 
 
 of the Coal Used. 
 
 Co al 
 
 from Franklin County, 
 
 Illinois. 
 
 
 As received 
 
 Moisture and ash free. 
 
 Moisture 
 
 .9 .48 
 
 - 
 
 Ash 
 
 9 .45 
 
 - 
 
 Volatile matter 
 
 38.58 
 
 47.63 
 
 Fixed carbon 
 
 42.49 
 
 52.37 
 
 B. T. XT. 
 
 11,701. 
 
 14,446. 
 
 Carbon 
 
 63.70 
 
 78.64 
 
 Hydrogen 
 
 4.96 
 
 6.02 
 
 Oxygen 
 
 9.42 
 
 11.64 
 
 Nitrogen 
 
 .97 
 
 1.21 
 
 Sulpher 
 
 2.02 
 
 2.49 
 
k I I'jV, 'll ^ ,» m- i n?f- ■'•- — 
 
 
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 * «• * ♦ 
 
 . .7 
 
 1 
 
 
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 ^ >. ■'* ', I 
 
 A# 4 : 
 
 
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 t 
 
 .fi;p affix' 
 
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 » 
 
 a. 
 
 . :.• zt ’id ri^.i'i £)J I- :. © « i J *a X O' ' 
 
 
 y. 
 
 do:^ 
 
 ;. . II 
 
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 i 
 
 l^viV‘r.5^ AA • 
 
 ■y 
 
 ■' ’ T' > 
 
 r ,V. ^ 
 
 
 ^ : ',ic 
 
 ' -i’' 
 
 ^ ■''* 
 
 • W .XV ? ' ;- -i 
 
- 20 - 
 
 Table 2. 
 
 Extraction Data. 
 
 Extraction 
 with Benzene 
 
 Extraction 
 with Xylene, 
 
 210 - 240»C. 210 - 240»C. 
 
 250-37 b #/sq.in. 180-200 #/sq.in. 
 
 lOOgm. 
 
 lOOgm. 
 
 Temperatin’es used 
 Pressure 
 
 Weight of coal used 
 Humber of charges of solvent 
 for each extraction 
 Volume of solvent used in each charge 
 Extraction time for each charge 
 
 (■♦ A third charge of benzene was introduced into the bomb 
 in an attempt to make a more complete extraction but after 
 extraction the solvent was only slightly discolored.) 
 
 2 liters 
 24-48 hrs . 
 
 2 litei-s 
 24-48 hrs. 
 
 Table 3. 
 
 Comparative Yield of Extracts obtained 
 from Benzene and Xylene. 
 
 Percentage original coal obtained 
 as extract , 
 
 Benzene Xylene. 
 
 
 
 As r * c *d . 
 
 M . & A. free 
 
 As r’c’ 
 
 First 
 
 Extraction 
 
 4.8 
 
 6.0 
 
 
 Second 
 
 Extrtict ion 
 
 5.3 
 
 6.6 
 
 
 Third 
 
 Extraction 
 
 
 
 22.91 
 
 Fourth 
 
 Extract! on 
 
 
 
 24.85 
 
 M & A 
 free 
 
 28.2 
 
 30.7 
 
■ry ^ 
 
 
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21 
 
 Table 4, 
 
 A Comparison of the Ultimate analysis of Coal, 
 Extract, and Residue, 
 
 
 Xylene 
 
 Residue 
 
 Coal 
 
 
 
 extract 
 
 As r* c’d 
 
 Corrected 
 ash basis 
 
 calculated 
 from extract 
 and residue 
 
 Coal by 
 analysis 
 
 c 
 
 85.96 
 
 54.42 
 
 57.28 
 
 63.90 
 
 63.70 
 
 H 
 
 7.13. 
 
 - 
 
 5.99 
 
 6.20 
 
 4.96 
 
 0 
 
 5.42 
 
 - 
 
 13.29 
 
 11.43 
 
 9.42 
 
 N 
 
 .42 
 
 .98 
 
 1.04 
 
 .89 
 
 .97 
 
 S 
 
 .95 
 
 1 .50 
 
 1.58 
 
 1.44 
 
 2.02 
 
 Moist . 
 
 .07 
 
 6.96 
 
 7.33 
 
 - 
 
 9.48 
 
 Ash 
 
 ol5 
 
 17.53 
 
 13.50 
 
 - 
 
 9.45 
 
 B. T. U. 
 
 16,499, 
 
 10,667, 
 
 11,229. 
 
 12,387. 
 
 11,701*. 
 

 : ./ • 
 
 
 i 
 
 ' 2 
 
 r T 
 
 I 
 
 I 
 
 t 
 
 ?♦ 
 
 •::n 
 
 \ 
 
 f 
 
 
-22 
 
 Fractional Carbonization of Extract, 
 
 Five gram sample of xylene extract. 
 
 Sulpher begins to decompose at 240’ C. 
 
 Heavy yield of light tar from 200 - 220'C, 
 
 TabUe 5, 
 
 Analysis of Gaseous Products of the Carbonization of Extract, 
 
 
 Gases up 
 
 to 350’C. 
 
 350 - 450’ 
 
 C. 
 
 
 Nitrogen free 
 
 Vol . in e . c . 
 from 100 gm .ext . 
 
 Nitrogen 
 
 free 
 
 Vol. in cc 
 from lOOgm 
 
 C02 
 
 4.9 
 
 94 
 
 4.1 
 
 177 
 
 °2 
 
 12.6 
 
 237 
 
 - 2.6 
 
 110 
 
 Unsat . 
 
 4.7 
 
 86 
 
 .7 
 
 31 
 
 Aromatics 
 
 .8 
 
 14 
 
 .4 
 
 18 
 
 
 20.3 
 
 382 
 
 53.3 
 
 2275 
 
 CO 
 
 10.8 
 
 202 
 
 4.7 
 
 201 
 
 CH 4 
 
 19.6 
 
 367 
 
 23.6 
 
 1007 
 
 
 26.3 
 
 497 
 
 10.5 
 
 433 
 
■V 
 
 r 
 
 I 
 
 x.c- 
 
 t 
 
 
 
 [I 
 
 
 
 » 
 
-23- 
 
 Fractional Carbonization of Residue. 
 
 Sulpher begins to decompose at 420* C. 
 
 Table 6. 
 
 Analysis of Gaseous Products of Carbonization of tbe Residue, 
 
 
 Gases 
 
 up to 350*C. 
 
 350 - 
 
 450*C. 
 
 
 Nitrogen 
 
 free 
 
 % 
 
 Vol . in e .c . 
 
 from 100 gm. 
 of extract. 
 
 Nitrogen 
 
 free 
 
 % 
 
 Vol , in c. c 
 from 100 gm 
 of extract. 
 
 o 
 
 o 
 
 60.7 
 
 646 
 
 16.1 
 
 540 
 
 ^2 
 
 30.8 
 
 277 
 
 15.5 
 
 518 
 
 Unsat , 
 
 .5 
 
 4 
 
 2.8 
 
 92 
 
 Aromatics 
 
 .0 
 
 0 
 
 .5 
 
 14 
 
 «2 
 
 1.8 
 
 17 
 
 38.4 
 
 1285 
 
 CO 
 
 3.7 
 
 34 
 
 5.9 
 
 199 
 
 CH 
 
 4 
 
 .9 
 
 8 
 
 13.3 
 
 447 
 
 2 6 
 
 1.6 
 
 13 
 
 7.5 
 
 249 
 

 9 
 
 
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 *•''*•' I ^ 
 
 
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 '<;K 
 
 01 ' 
 
 >t-X 
 
 !\ , 
 
 
 
 V' > 
 
 1 
 
 
 '> ■' 
 
 
-24- 
 
 Coking Tests, 
 
 A. With "benzene extract and residue. 
 
 Extraction with benzene did not visibly impair 
 the coking qualities of the residue. 
 
 Benzene extract melts from 115 - 130*C. 
 
 B. With xylene extract and residue. 
 
 Residue from xylene extraction shows no coking 
 tendency . 
 
 100 % extract softens quickly and swells to a very 
 great extent. Much of a one gram sample will be lost by 
 this swelling. A light, porous, fluffy coke remains. 
 
 15 % extract 85 % residue gives a rather poor, 
 soft coke. 
 
 30 % extract 70 % residue gives a hard, black, 
 porous coke. 
 
 Compares favorably with coke of original coal 
 except that some of the silvery luster is lacking. 
 
 A portion of the residue was set aside and exposed 
 to the action of the air and moderate heat. After sev- 
 eral weeks of this atmospheric oxidation a coke test was 
 made with 70 % of this oxidized residue and 30 % ex- 
 tract. The mixture shov/ed only a very slight caking 
 tendency. The coke obtained was very soft and sooty. 
 
 Some of this oxidized residue was then heated in a cov- 
 ered crucible to coking temperature and a portion mixed 
 with extracts as before. Again a coke sample of good 
 quality and texture was obtained. 
 
-25- 
 
 BIBLIOGRAPHY. 
 
 1, Wm. A. Bone. Coal and its Scientific Uses. 
 
 2. V. B. Lewes. The Carhonizat ion of Coal. 
 
 5. White and Thiessen. The Origin of Coal. Bulletin 
 
 38 Bureau of Mines.. 
 
 4. Burgess and Wheeler. The Volatile Constituents of 
 
 I 
 
 Coal. Journ. Chem. Soc. V. 97, p. 1917; V. 99, 
 p. 649; V. 105, p. 131/. 
 
 5. Porter and Taylor. The Primary Volatile Products 
 
 of Coal. Tech. Paper 140, Bureau of Mines. 
 
 6. Porter and Ovitz. The Volatile Matter of Coal. 
 
 Bulletin 1, Bureau of Mines. 
 
 7. Parr and Hadley. The Analysis of Coal with Phenol 
 
 as a Solvent. Journ. Soc. Chem. Ind. 1915, p. 213 
 U. of I. Engineering Experiment Station, Bulletin 76 
 
 8. Lavid White. Effect of Oxygen in Coal. 
 
 Bulletin 29, Bureau of Mines. 
 
 9. Parr and Olin. The Coking of Coal at Low Temperatures 
 
 Engineering Experiment Station, Bulletin 79,