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They sem tobe tee Frcturefssures caus by tectonic movements o¢ misag, or funn’ een ge ut which abound in all vegetable tse, although mos of thse dca hae be “stroyed by crusting or by abtreton wah mineral epee, Rhos tha ed ‘dus can een be som unde a micoscoe The macroporoiy volume is determined by mercury injstion, Under a pressure of | br 100 KP), or example, mereary wl penetrate pares paving a ameter pete thn 15 un, whereas narrower pres are barred toby cpilary frees By ane he Cure of valume introduced aginst pressure, for extmpl upto sb hoop (G00 MP), he dssibution of maeropers of dxmetergrecter than 1Seem (13D Ayis ‘btined as shown in Figure |, Tis tmacroporsty eperentssovrl peach Volume ofthe vitae, bu ste toal urace wea sony oft oat Grass Tes thought tat eine ses macroporous thas wnt: ad tat fete on 'n grea "aetonors er considered to be thot stroner han about 2 nm (20 A), and"intemediat pores those af a niae betwen micro: nnd Macroponer The olune ofthe fine porosity i determined by eomparson between tre density see below) and density wing meray under high prewure The delored Sone ee ofthese micropores haben evauated by dierent methods say of avons ‘on-derorpion isotherms of gases und rapoucs (Fgure 13 heat ese aoe iguid pensation Figure 1.6) and sahangis Keay difacion, 8) sess ih-thin aes unde an tron microns, it spose to vey the canton his micropores, ough st to make auaniatve mesurencnts ‘re iicalty es he fac tht thse easine pore ane moe oles accesible, ‘en othe amie molecules usd, depending onthe experimental eoitons and ts tat certain Haul which havea strong chemical afi) for coal increase the porsiy trough wbich hey Bow by epurating the mills Neverthe cece Fas gradual bon reached bout the odes of magica of surface ares Sod ot Volumes. 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When a coal begins to oxidize, the maximum plasticity decreases very the plastic zone narrows, mainly from the lower end. Fixation of 0.1% oxygen (cstimated by interpolation) is enough to reduce the plasticity appreciably though still ‘without visible effect on the material balance of carboniza Lengthier oxidation, correspond be obtained with a gras coal in 4h. is fine enough, greatly reduces the coking properties and for some coals suppresses ly. The plastic zone is reduced from both ends and a decrease in tar ‘be noticed. It appears that with 2% oxygen the coking properties has reacted with the coal is released in the form of CO, CO, elf; another part remains attached to the luring carbonization, some around 300- fect of oxidation on the coking ofa few coals, ion of a high-volatile coal (a coal close to $36 Volatile matter over a greater temperature interval and thus decreases its maximum rate. ‘ad vse Te oF wh nse) 2 708 300 Figue 210 Rate of weightloss ofcoa $36 of 7.5% onypen, before and alter oxidation C The phsticsate ofeua scones 1 Ww i | u : is ce us a 02} cea 10 ao : 2 Belin mo 25 teeta) Figure 211 Changes ia ASTorraie ‘Sembeat ty of three coals as a function of time of oxidation VM and 83% carbon, C= Coal of type €35, = t when a coal is very plastic, slight oxidation which reduces its plasticity a litle can increase the swelling index by half a point. 2.2.54.2 Interpretation ‘The efect on coking properties is explained in the first place by dehydrogenation of the coal, the overall reaction during heating as far as the beginning of the pyrolysis zone being capable of schematization as: Coal + oxygen-+water-+ dehydrogenated coal The formation of metaplast is very sensitive to the amount of available hydrogen Next, part of the oxygen fixed on the coal is apparently fot hydroxyl groups, -OH, which are preferential sites for condensa which are responsible f explains the inerease also lead to.a redu Consequence is a reduction in smoke during com 22543 01 Several oxidizing agents have an action somewhat analoy and perbenzoie acids and ferric oxide, Fe,O,, may be mé produced with additions of blast furnace dust or 0 ‘oxides beforehand, to reduce the trivalent oxide c oxidants One interesting case to be considered is that of free sulphur, because its action ‘greatly resembles that of oxygen and because it has sometimes been used to reduce the tendency of briquettes to swell 12). The sulphur is fixed on the coal and is partly12 Pandan of eoniaon C ed during carbonization, produces dehydrogenation and al he form of hydrogen sulphide. Like oxygen,there- c ing which is not without ing sulphur is much more 1a8 practically the same quantitative eflect as oxygen: 1% sulphur reduces the plasticity as much as 0.5% oxygen, lity s a consequence of the plastic s 3. Reduce the production of Industrial oxidation can be performed of the ease of temperature control. 2.2.5.5 Hydrogenating agents There is a remarkable symmetry between the action of hydrogenating agents and that of oxidants, Very careful hydrogenation of low-rank coals results limination of oxygen yeen modified in a manner temperature, a large jerease in the temperature at which transforms coals of more than 15% lable sticty and @ relatively sme plasticity ceases. More extended hydrogenat Volatile matter into @ kind of bitumen and finally, by perseverance, into dis hydrocarbons. ‘The formation of metaplast is considerably increased relative to unhydrogenated verified by solvent extraction of the products in course of carboniza- ‘The reduction in fusion temperature is due forces before any pyrolysis. 2.2.56 Addition of bituminous products ‘These may be coal tar pitch (low- or high-temperature) or even an ai petroleum bitumen, the inv the role of metaplast ex: ‘Many laboratory tests and some industrial operations have been made with additions of the order of 2-6% of coke oven pitch. Interdissolution of the pitch and the molten coal occurs. As happens after hydrogenation, the plasticity is considerably increased and the plastic zone is slightly extended, For example, for a certain flambant coal, the maximum rate of rotation of the Gieseler plastometer increased of 5% of pitch and 1060 after ad ym 50 degrees of are per minute to 235 after addition of 10%. The effect is even more positive for demi-gras coals which are at the limit of fusibility and which form insufficient quantities of metaplast. A demi-gras of 16% volatile matter, which does not agglomerate in laboratory tests at 3*Cmin~! and which does not cause any rotation ¢ The plastic state of coub and i oneness 83 of the plastometer, begins to swell and to show appreciable plasticity, with the mation of a very good coke, after addition of 5% pitch. More generally, adi of 2% appreciably increases the fluidity ofall coke oven charges, with an almost linear between the quantity of pitch and the logarithm of the maximum rate of However, we have seen (see section 2.2.5 quality of the coke to only a where the shortcoming in qualit e additions can improve the in the not very frequent cases of fluidity. 2.25.7 Metaplast-destroying agents ‘The effect is exactly opposite ion of bituminous produets, ‘Oxidant are agents that destroy the metaplast, but other products have an effect of this nature. They appear to act by accelerating the condensation reactions. In point of fact, these are catalysts which in organic chemistry are known to produce reactions of Friedel-Crafts type which can crosslink aromatic molecules. ‘These are strong acids (sulphuric and phosphoric) or acid chlorides (of zine and aluminium, for example). It is as ifthe metaplast is destroyed by cross-linking as itis formed. The mechanism can be verified by heating a low-temperature tar (very similar st) at 400°C in the presence of these substances, which very rapidly into coke. Another category of substances inactivates the metaplast not by che sation but by a physical adsorption phenomenon. jon temperature in plasticity. Five per cent by weight of activated carbon or adsorbent totally destroys the coking properties, and even 1% has a noticeable effect, shown that they adsorb the metaplast, often wei! latter can no longer play its rl ‘There have been proposals to smoke during the combustion of briquet strongly. The result isa little analogous of calorific value, Clays in washery water may be deposited on coking fines and unfavourably affect their coking properties. 5 lay almost 2.2.6 Consequences of the fusion of coals Coals that can be coked undergo plastic fusion when they are heated to around 400~ 500°C, and they simultaneously evolve a large amount of gascous products at this temperature. The present section examines the consequences, mainly of a mechanical nature, of the juxtaposition of these two phenomena. 2261 Swelling (a) Description The start of swelling has been studied by the following two techniques: 1. Microscopic observation of thin layers of coal during coking, with the aid of ‘ecelerated| microcinematography to follow the relatively slow process better.Fito ot ctoiaoe C 2. Coking of coal particles with rapid quenching at different stages, and microscopic ‘observation of the particles after cooling. In this way it is observed that almost simultaneously: Within the particles, principally the largest, bubbles of more or ess spheroidal form arise and grow because the gases that form at the centre of the material do not have an easy exit; the larger the particle, the more difficult it becomes. ‘The external outline of the particles is deformed, though of course in a manner that depends greatly on the pressure applied. This pressure may be, for example, the weight of the particles themselves: they will be weaker in a laborato, small amount of coal and the deformation of the extern ata temperature higher than if the height of coal above the pe areater. les therefore become closer together, though sti 1g some voids 1em ~ intergranular pores ~ they al spe and are regular shape than the intragranular voids formed by a gas bubble within a plastic particle If the coal is not very plastic at the heating rate used, that particles are more or less swelled by the bubbles and fused in places. After ion the coke is not very coherent and the swelling of the whole will remain ifthe coal is more plastic, or if the particles swell oF finally ifthe coal has b osure of the intergranular The pyrolysis gases can no longer freely escape and the pressure increases in these intergranular pores, giving rise to swelling of the whole mass of coal and hence closure of new intergranular pores. The result of this is a renewed increase in pressure, and the phenomenon becomes selfexciting as it were, until the large bubbles of imprisoned gas burst. The overall expansion can attain several times the initial volume of coal, (b) Role of surface properties Clearly, within certain limits an increase in plasti- city can thus facilitate swelling, But this is not the only factor, and it can happen that at the same plasticity and coking conditions (particle size, packing, heating rats) particles of certain coals swell more than others. The reason is not to be sought rate of release of the volatiles, as docs matter) that are the least swelling at constant pl In our of the cause ty. rather ina class of properties that are fairly difficult to measure, which one could call ‘film-forming’ or ‘surface 0 detail 0} poorly understood rank coals have a at the intragranular they re-form more tension’ properties. phenomena, let ‘surface tens and intergranular bubbles grow more before but easily after bursting. However that may be, when the coal is sulficiently fuid, the whole takes on the appearance of a pasty mass swollen with gas bubbles which expand and then burst, the porosity that they form no longer bears virtually any relation to the voids initially present between the particles. ¢ “he piste foals iu concerns 85 Towards the end of the plastic stage the Muidity decreases and bubbles that have burst no longer close again. A new network established for the escape of gas, ‘ough the bubbles and the channels between them. If this network is formed while wappens when the ‘surface tension’ is 1. Intragranular, which depends only on the coal, its particle size and the heating rate. 2. Intergranular, which depends also on packing and the forces on the solid phase. However, the distinction no longer has any point when there is suficient pl because the boundaries between the particles are obliterated by agel city, (c) Factors favouring swelling In accordance wit late the factors that favour swelling. is description, let us recapitu- not very favourable, however, e mass of coal, “film-forming” properties Not too fine a particle size, since the gases can escape from fine particles by diffusion and hence without causing intragranular sweling, ‘A high charge density and even, paradoxically, a degree of pressure, which will favour the closure of the intergranular pores i the case of coals at the limit of Remember finaly that, si ‘Phenomenon, a minor modi therefore be taken in measuring sw results are to be obtained, (4) Numerical relationships between plas tendency, in monitoring coals for co} swelling are almost equivalent characteristics and that coking properties can be assessed with a plastometer just as well as with a dilatometer. This is not grossly untrue, indeed, since coals that are sufficiently plastic also have good si ‘ood correlation bet ire was obtained+ maigres x Ukgras #1292 Dhgras #9735 3coked oar ScokeB xflanbant gras 8 ‘ flambentsee igure 2.12, Corcelaton between maximus fuidity and Arnu iatation coking coal of 20% volatile matter having a fluidity of 20 divisions per minute in the Giescler plastometer as with a coal of 38% volatile matter giving 2000 divisions per though the rate of release of volatiles at the moment of maximum 1ost double for the latter. swelling is alm 2.2.62 Caking ‘Two coal particles in the plastic state stick to one another when they come into contact even at low pressure. But in all blends used for coke production there are or even inert: general ‘and sometimes maigre coals, coke breeze and accident ‘eration between plastic coal and an inert particle is ood plasticity and a degree of contact pressure. 10rs have expressed the opinion that caking could be inadequate between oals whose pl exceptional to find two coals whose plastic ranges are as much out of step as in that example. Moreover, such a blend of flambant gras and demi-gras is unsuitable for coke ovens because both constituents have too little The plastic sate of coals and its consequences 87 the presence of tarry sgins ata temperature rather the fact that one or both of the cor imum plas In practice the capacity for good caking coincides with the existence of intergrai lar swelling, because on the one hand this swelling occurs when the particles fuse inder the escape of gas, and on the other hand the local pressure which aids agglomeration of the inert are therefore mutually reinforcing phenom example given 1g in the dilatometer implies in fact that intergranular swelling has occurred freely. If the criterion of plasticity were to be taken, however, a rate of rotation of 20 divisions per minute would correspond to a ‘matter, whereas with a flambant coal ‘When two coals that can be converted to coke are carbonized in a blend, do they really mix to form a homogeneous plastic phase, or do the two phases preserve & certain individuality? It is surprising to find that a question so basic to a theot understanding of coking phenomena should have attracted the interest of rela few research workers, ‘The indispensable tool for this study is a high-magnification polarized-light microscope, used for examining polished sections of coke, which must be very carefully prepared, like optical surfaces. In this way the cokes formed from the ‘igure 213 Causal chain of phenomena in coke formation88 Fundamentals of carbonization C ty be recognized (see section 2.3.5.2). For example, there is ween the coke from a coal such as $36, ly black when observed with cross ; very texture (Figure 2.14), The two coals are sufficiently plastic to fused coke. in the laboratory or in a coke oven from blends of coals arly shows black and granitic areas originating from the one individuality unde However, if we examine - tion, we perceive a transi ness: 0.01-0.05mm under conditions, but a little more for cokes from industrial ovens. The ‘of this zone show continuous and progressive passage from one type of coke cr. Itis noted, for example, that the e-grained in places, which is the appearance of eoke from gras co le matter. Here then we have ‘ mixed phase resulting ftom local blending of the two original coals, probably by diffusion during the plastic state If one of the constituents is realy infusible, there is no longer any trans and the boundary is very clear. If one of the constituents is almost inf ple, a flat ti F side, but the texture ofthe coke from D is slightly bourhood of the flambant coke frm, has become ‘degraded! This e metaplast of coal D25 has dissolved a small amount of coal F40 or of its metaplast and that the mixture sn an intermediate coke. int for those in the coking industry to consider is the thieleness of the transition zones. They are a than in laboratory cokes iff a blend of industrial zones none the less Is, n the laboratory, however, the coal is often erushed to ‘mm to obtain a represes Under these conditions the mixed phase can extend to the majority of the coke. This ter in plastometers, where the agitation caused by rotation of the moving part favou fore necessary to realize that a laboratory jends of finely crushed particularly” the plas information on a mixed phase which ven. If we may be ‘much difference as between sample of 3 mi is nevessary to carbonize samples of more than 100 g, impossible to achieve isothermal heating. This problem can be resolved only by ‘compromise: it appears to the authors that a sizeof under 0.4 mm or 0.5 mm gives a -xtent of mixed phase in the laboratory and allows samples of 5 g or90. Funda of xbotaton G 10g to be handled, which oxidation in air compared be heated isothermally, while reducing spontaneous the usual size of under 0.16 mm, 2.3 Resolidification and formation of texture 2.3:1 Description of the phenomenon; concept of resolidification temperature observed experimentally that a coal cannot be kept for an extended time ‘At the heating rate in a coke oven, ie. 2-4°C min” ‘coals can be made into coke is maintained from around 350-500! an hour. If the heating rate is lower, terval lastic state becomes narrower (sce section 2.2.5.3) and the pl jecreas end of some hours in the most favourable case the plas ceases and solidifies into coke irreversibly. If carbonization is prematurely interrupted mas have had take place, an-apparent but not permanent resol ved on cooling; the coal retains the capacity to soften again during further heating to a higher In any case, resolidifica- tion will be permanent when no more than 11-15% volatile matter remains in the coal The resolidification temperature is rather better defined than the softening temper- ature, since plasticity decreases more rapidly than it appears (Figure 24, curve 1), In the whole course of thermal treatment of the coal, there is no temperature zone where the phenomena have twenty or so degrees that precede resol © crystalline order of the coke begins to form. relative disposition of the carbon atoms nor the porous structure can be profoundly modified at a later stage. The mechanical stresses that cause fissuring of the coke during further carbonization depend by 10°C, a mediocre coking coal could be transformed into a good one or vice versa. 2.3.2 Measurement of resolidifcation temperature Instruments that allow the softening of coal to be studied, especially plastometers, permit resolidification to be observed by the disappearance of plasticity ha ‘measurement is not precise. Plastometers are in fact intended for studying plasticities that may be high and therefore use low torques; they stop rotating before actual tion, because the viscosity has become too great. CHAR has constructed a speci eter for a precise stu cation (references {43} and [44] of Chapter 1). It indicates temperatures re to about 3°C and higher than those given by the Gieseler or Brabender pl Itincorporates a trident-shaped rotor which turns very slowly (50 as not to iixing phenomena in the coals in the plastic state). The opposing torque is recorded, stage and inereases more and more rapidly until the coke shatters (Figure is recorded, denoted 0,. Two success fends of two coals of sufficiently different rank and no! (see section 2.3.6). a fey a = iable-torque pastomete, showing the rsoidifcation tempera Figure 215 Curves recorded by a te) 2.3.3 Resolidification kinetics The resolidification temperature of a coal increases with the heating rate. To a first it may be considered that resolidifcation takes place at a well-defined. level of progress ofthe pyrolysis reactions, characterized by the fact that there remain 0,=8,+ Klog (a9/a) which in a general manner gives the temperatures at which chemically id are found at different heating rates. Now this is indeed ‘experimentally. Kis of the order of 60 for a coal of high volatile matter and 70 for coking coal. This means in practice that 0, increases by 15-20°C when the heating rate doubles (cf. Figure 2.8) 2.3.4 Mechanism of resolidification, Segregation phenomenon We have put forward (see section 2.2.4) a theory of fusion by formation of a ‘metaplast’ which causes a kind of solvolysis similar manner, it can be said that the cracking reactions (see section 2 / when the temperature increases, through a deficiency of hydrogen and through the disappearance of the weakest C-C bonds, while the condenser 23.5.1 The anisotropic phase foreshadows the erystalline order of the graphite tis composed, as we have said, of stacked planar aromatic molecules perpendicular to a given direction (practically the same throughout the globule, but varying randomly from one globule to another). The carbon atoms occupy selative positions ‘very close to those the hhave in the crystal (see section 2.4.2), the pl Certain technological properties of coke depend on its eraphitizability. 2.5.2 The coke texture remains as it was atthe moment of resoidification To every globule of the anisotropic phase there corresponds an “anisotropic domain’ in the coke (whatever its further thermal treatment), that is, a region in which there is direction of graphitic planes, independent domains. This explains the characteristic appearance of cokes examined by pol light (Figure 2.14), which exactly reproduces the arrangement of the two insoluble id phases at the moment of resoliification that we have just described. ff more than about 35% volatile matter and more than about 6% oxygen When rank inereases and when the this 35% level, a ‘granular’ appearance these domains grow to 5-10 um and give the ‘coarse-grained appearance of granite to the coke. When the domains extend, the coke takes on a ‘fibrous’ appearance around 20-22% volatile matter and shows wide sinuous ‘bands’ around 18-20% volatile matter or in a high-temperature pitch coke. ‘These fibres ar ‘materialize the orientation of the planar aromatic molecules in “oke petrography is based on the quite characteristic features listed in Table 4.13 Gee section 4.6), 23.5.3 When coalescence really occurs, the coke may display macroscopic anisotropic properties -okes, but it forms an essential feature in the pitch pie domains reach 1 mm or more, the coke breaks ce those of graphite. If carbons are manufactured by or extrusion, the needles or flakes, and consequently the graphitic planes, are ed relative fo the direction of displaying overall anisotropy of propert sion and electrical resistivity will differ depending on direction. ‘This is desirable in certain applications but completely unwanted in others. This is why easi srge anisotropic domains (needle coke) or om the other hand with small domains (gilsonite coke, for example) are often sought 2.3.6 Resoliification of coal blends Consider blends of two fusible coals A and B of very different ication temperatures quite far apart. For example, A .nd therefore with a gras d coke A le eon and fomaton of textte 95 similar to D25 and B a high-volatie coal of $36 type. Then plot on a graph (Figures 2.17 and 2.18) the resolidification temperatures of the blends as a function of the proportions of the components (reference [44] of Chapter 1). If the particle size of the two coals is fine, the resolidification temperature is well torque plastometer and the variation of @, with concentra- ear. If the particle size is slightly coarser (depending on the mn irregularity is observed at around 35-40% of component A (Figure 2.17), the significance of which is apparent from the experiments below. With an even coarser size, e.g. 1 mm, 0, is well defined for blends with less than 20% ‘and more than 50% of A. However, for blends with 20% and 30% of A, two rupture $90 ¢§ deso X20 i ol | set +450! oo 0 2 40 60 8 m0 Figure 217 Reso Partelesze <0.2 mu fon temperature ofa bend of two fusible cols as function of composition. f Tapert 1°) (ote 20) gee) co teeca) Figure 218, Resoliication temperature of the sme blends tutte industslly nin Figure 2.17, but with partislesize96 Pundametl of carbonation ¢ -scan be observed on the curve of resistance torque (see Fi jought to be an irregularity of no significance, but systematic study showed that the phenomenon was reproducible. If the two rupture temperatures are plotted, sd, where the continuity of the curve sections leaves no is observation, In the theoretical ig case in which the two components A and B would form coke independently of one another, there could be only two possible values of @, that of A alone and that of B alone. At what concentration would the value pass from one to the other? As rimuous phase, ion of the blend will coincide with that of phase B. But when the y A added 10 that occupied by the bubbles forms @ continuous phas forms only a discontinuous phase and resolidification of the whole will coincide 3 A. Not unexpectedly, the transition is found in the region of 40% of ‘component A in the blend, taking into consideration that this is more highly swelling than B, When there is less phase Bis observed at plastometer continues t phase A has resolidified of B passes unnoticed. Th phase A playing the role somewhat of ‘plastic resins to reduce their stiffness. ‘The other theoretical limiting case is that in which mutual dissolution of the two ‘components is complete and they would form only one homogeneous mixed phase, the properties of which would vary re ‘composition. Itis probably through the fact that @, varies a little with ‘concentration above 40% of A must be explained. The res re of blends of the type 70% B+30% A may ry with particle size. From this it follows that the maximum coefficient of contraction (see section 2.4.5.4), which is located just after resolidification, depends on particle si rhese considerations will allow us in section 3.2 to offer the most probable lanation of the variation of the M40 index (see section 4.3 for definition) of blend ‘of a flambant coal with an auxiliary coal as a function of their proportions. nd retains a certain plasticity on the macroscopic scale, .corporated in synthetic also. 2.4 Carbonization beyond 500°C. Fundamental properties of coke a solid residue is obtained that is often called i transform progressively into high-tempera- development of this solid by examining in around 1000°C, since this is what corresponds to coke s limited to phenomena that occur during homogeneous smal conditions. Compared with what occurs in the range 350-S00"C, the coking conditions — heating rate, pressure, particle size are of less importance above 500°C. Most of the characteristics of the coke are determined by the state at 500°C, by the maximum temperature reached and to a secondary extent by the residence time at that temperature, ‘We shall very often again come across the fundamental difference betwen the two C— caroniation ont 0° Fundamental pope ofcke 97 types of carbon ~ graphitizable and non-graphitizable ~ depending on whether the plastic state is maintained to a temperature high enough to allow development of the anisotropic phase or whether on the other hand this does not form. 24.1 Chemical changes Tables 23-28 show how the volatile matter and elementary composition vary ‘The analyses were carried out on In an extreme case, the 800°C can adsorb 2% of oxyger inated to a large extent by heating For various reasons the determinations of carbon in the carbonizat ie imprecise and have been rounded to the nearest 0.5% or ‘volatile matter varies considerably from one coal to anoths ly higher for parent coals richer is explained by the relatively high mass contribution of CO and H,O volatile matter. More precisely, Figure 2.19(a) shows the rate of release (by volume) of the principal tion of temperature for a heating rate in the region of 2°C min and ite of a coal little different from $36 (after Fitzgerald and van Krevelen 16). At 500°C mainly methane is released, but this proportion rapidly decreases as the temperature rises, Carbon monoxide remains an important const tuent between 600°C and 800°C, while hydrogen passes through a very characteristic maximum around 750°C, almost independent of the type of cot hydrocarbons other than ically ceases after 550° a for a coal of 19% vol igure 2.19(c) gives this release rate for a semicoke also from a but pre heated to $80°C, after Rennhack (17]. The prior heating has modified the ki erat low 700°C, but this graph provides data that are probably valid for devolatilization above 700°C and thus complements Figure 2.19(a). Here the heating rate is S'Cmin-', which of course increases the rate of release tis noteworthy that the sulphur content of the solid residues should ‘equal to or a little below that of the parent coal up to 1000% sulphur in the coal is found in the 1000°C coke, whether itis organic or pyri has proposed the following average relation for American cokemaking co: Sulphur content of coke=0.084-+ 0.759 (sulphur content of coal) ‘Thermal desulphurization of coke occurs only at high temperatures, inthe region of 1500-1800°C. However, desulphurization can be performed at much lower tempera~ ‘ares, from 700°C for example, if carbonization is carried out ina stream of hydrogen ‘or water vapour and if the lumps are small enough for the carrier gas to diffuse into the interior. So far, no practical and economic process has really been found for desulphurizing coke in 60 or 90mm lumps. It appears easier to reduce the sulphur ‘content of coke from initially 3% to 1% than to obtain a coke of 0.2% sulphur from‘Table 23 10) 96 opeztogis Jo semourepeeg rods cro a 2) Ror 400 450 050 aaa Vole eaverat yen 95929987 hima ons c ii 20 2 oy 2 os 925 BS 94.0 955 60 ” f ate acectmeeAiteet isin ct eecss Mace | auscneuis he misasetc: 8 uo oo i 6 ek x B 6 2 2 1 tT 03 we : 06 SS CSsStswaes tS Den ime st orc is eas ae kes ey OM Pen Tale 24 (025 Frotercronad ar Ce Rovcoat 400 450) 555 arama Woe manera Yoni us) aiaasuc med seals no eves fees sae see cee Una an 0) e er i st So SSS seen ee 6 a 35 i 04 x lee Oo ameeg saeco see ee A ceca ee ccc : 06. 06 sek Dens: Twist ioc 1s 28a) Thao ie a tt eeepmeniommmens sas non senmam ——>) \‘Table 25 (C25) Product carbonized at ce) Rav coal 40 45088008 Volatie mater at 2Cmin“" mo m2 kas 90 66 3s 1s os ° ‘Umate analysis %6- c By ty ete bn eon 9s 960 970 H 32 52 48 40 3a 20 12 a8 ° 3 “a a 40 30 09 04 N ts 16 7 a7 17 1 16 ls s 04 04 04 08 as 04 04 03 Density Tnwatcrat 0'C 128 128.3036 Inhelom t Le 137 198 Table 26 (C35) Product carbonised at co) Raw coal 00 48050058000 ‘Vola matter at 2Cmin" nts moa 90 1» 38 6 a ° ‘Utimate analysis 6) c ws SOT sows 80 H 34 32 44 39 35 29 22 13 19 07 ° 56 53 45 3s 2a 0 u as 02 N i 8 os as os os os os os os os o4 Density were ao ety ee 206 ede te eee i el Inbal i ey te 3 vonesyuagies o seromepany got ‘00 9 sedond eoumpun 2,095 paokeg voRsqORIRD ) 101Table 27 (836) FN pope 408mm ww ‘ota ne ist aa) fi Cr ee i se TEE ge 8 uo Oo UBM x @ @ 6 § h wf ob ow wy 3 a 8 8 0 & 38 @ 8 8 Deni Tntrat OC 13a oe essa hate ih Tae 28 4 Feder extender 2) Hovew! 49 ww oe panera remo Ms mo skew ‘it say é mss os Ms moos 5 see Egg Ss 8 memo ko SB S 3 ee ee ee 3 Oe es Deny tie tore ag) Ms aay Eka i is i mo soneeagae jo smmaurepung 2409 0 sopindoxd jmurepun “2,005 puOK wopETIIOGED > sor104 Fundamentals of carbonization one containing 1%. Reference may be made to [18] and to [8a] on these questions of ‘the behaviour of sulphur during carbonization and the dé Electron paramagnetic resonance studies have shown that all coals contain unpaired electrons (equivalent to unsaturated valencies, otherwise called free radi. varies somewhat with coal rank around 10" radicals per gram and increases with carbonization temperature to a maximum of about 10% Teached around 600-700°C. Beyond thi Ithas been possible to estab attached to one particular carbon atom but can freely wander Aromatic groups’ of carbon atoms that were referred to in section 1.1.43. Though interesting from a theoretical point of view, this existence of free radicals has not se far been related of coal or coke, 100°C; the main observations are the trons begin to disappear. ese are “delocalized” electrons which are not Or al properties of coke 10! 8a result of the reduction of iron oxides, ind some of Its calorific value correspondingly rises by i somewhat surprising that all these reactions occur as low a explained by the formation of a liquid phase composed of a mixture of metal sulphides and carbides, in which the n of the metals reduces their chemical heat of combustion of a combustion of 33.50-33.80 MJ kg", which is therefore nearer to th ‘amorphous’ carbons (34 MJ kg™') than that of graphite (32.9 MJ ke") 24.2 Graphitization References (1) and (19) in particular may be consulted on this topic. We call graphitization the totality of the structural transformations that occur rogressively as a graphitizable coke is heated to high temperature. There is no question here of the surface deposition of shiny pyrolytic carbon to be mentioned in section 3.4 Graphitization is customarily begun around 1000-1500°C, since so far the physical methods used to study it are difficult to use for cokes carbonized below this temperature. Transformation to graphite ends onl ‘around 2500-3000°C. This isa temperature re for industrial coke production, but cokes used itera faily long residence time lurgical may ms of use, and this considerably influences their quality. For other materials that may be produced by the carbonisy, tion industries (calcined anthracite, pitch and pitch coke), graphitization behaviour is Of quite prime importance, Between S00°C and 1000°C there is already some rearrangement of carbon atoms; ‘his is less well understood than that at high temperature because of the difculty of studying poorly ordered structures with X rays, that just before resolidification the majority of the carbon atoms formed roughly planar, highly polycondensed aromatic hydrocarbons of high mole cular mass, and that these molecules were arranged parallel to one another. When such an arrangement isc a sulci occur, Xray ex: arrangement of planar aromatic molecules is st nanomet In cach planar molecule, the disposition of the carbon atoms is already very much the same as in an elementary graphite layer, but the average distance between the lanes is greater than the 0.335nm of a graphite erystal because there is significant amount of hydrogen present. To get an idea of the structure of a semicoke from a gras coal, imagine graphite crystals about 10um in size. Separate the clementary planes, turn them slightly in r icular axis and finally bend these planes little. The picture woul iple for cokes fromC flambant coals, but the crystallites are much smaller - only a few nanometres ~ and parallelism of the planes of carbon atoms probably occurs only in part of the structure. Around 700-800°C the evolution of most of the hydrogen in the semicoke allows the graphitic planes to begin to approach one another. Numerous stu the thermal development of coke structure have involved examination of the following phenomena during progressive heating: 105 Fundamentals of carbonization |. Growth in area of the clementary layers (graphitic planes) and internal reorganiza- tion in each layer. 2. Displacement of the layers in their plane and expulsion of crystallographic defects 3. Mutual approach of the layers to their limiting distance of 0.3351m to form a three-dimensionally ordered crystal. ‘These studies have also considered the relation between these rearrangements and. coke properties; cf. especially reference [1]. Here it suffices to say that: through three states usually from the three graph ned above. F, is the final state and corresponds to the graphite The three phases F,, F, and F, coexist in a single carbon particle, their temperature until F, and F, have disappeared, when ‘transformation is complete 1 ing, the carbon passes succes ‘ofa carbon sample can be indicated either by lementary layers are mutually ordered as they intty g which represents the fraction of the path covered by the wy layers when they approach from the distance of 0.344 nm in non-graphitized carbon to the final distance of 0.335 the crystal. If their average distance apart is d, o3s—a 8° Y34a= 0335 P and g can be deduced from an X-ray diffraction diagram, mas are effected with a very smi tial position, which approximately It should be said again that these transform Ig Ly ‘The hot face has therefore contracted less than the other. Consequently, the slice bends like a bimetallic strip. This eur if'for cxample segments AB and CD of the thin slice ~ ie. in practice less than 1 em — such an approximation is stresses are reduced suflicently to avoid fisuring, The fin of curvature B may be calculated approximately. At the end of ‘carbonization the points representin practically complet difference in contre ‘The expression ( 0), is called the coefficient of contraction at temperature @,Figure 37 Curvatore of th ‘The thickness of the slice is: = 46) ‘where (04/2x), is the thermal gradient in the resolidification zone, Approximating the slice to a bimetallic sheet formed by the two faces, we obtain: De nee et eee RL e L @ ‘The final radius of curvature is inversely proportional to the coefficient of contraction at resolidification and to the thermal gradient. 3.3.2.3 Calculation of stresses and fissuring This first approximation, which has been presented only to provide an idea of the phenomenon under study, was set out by Soulé [6], whose work was developed by Chagnon and Boyer (reference [27] of Chapter 2) For a given coal, the following are determined: the as a function of temperat te of contraction of the coke fairly good approximation. The Poisson ratio y of coke is assumed to be equal to which will not introduce great error. The principal hypothesis is thatthe layer of coke jis mechanically fre, ie. that the external mechanical stresses, such as the weight of the coke and the pressure exerted by the plastic layer, are negligible compared with the internal stresses set up by contraction. The general equations of equilibrium in a solid are then written, which have been solved numerically and which thus give ata given instant the distribution of stresses in Distance from heating val (ma) 22 ° 10 20 30 40 50. ‘igure 38 Mechanical stresses inthe absence of fase in coke from coal S36 at diferent periods from the start of coke formation ese stresses are always parallel to of coke at every point and are much higher than the external stresses, which justifies a the hypot of the phenomenon can be pursued further. The appearance of the first fissures reduces the stresses in their immediate vicinity, and fissures are formed unt the stresses are everywhere reduced below the fracture calculate a value of D (average distance between parallel fissures) correct to a factor of about 2. Computer calculation programs exist and are ready for more accurate numerical values of ereep. However, the main interest of this theory for the coke oven operator is not this between calculated and observed values of D. carbonization process determine D, as ‘This process of fissuring due to inequ a result of a thermal gradient is not an fracture the example most remarkable for flows that have resolidified in a vert homogeneity of the mate separation, exactly par 3.33 Factors associated with fissuring ‘Ths above mechanical theory reveals thre principal factors which control the average distance between fissures, which we have cal