Liquefaction co-processing of coal shale oil at - Argonne National ...

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ecame aware of an evolutionary trend in coal liquefaction processing. The major factors contributing to this novel trend were: 1) the better understanding of the very sensitive interdependency between the stages of coal extraction, of the coal extract upgrading and hydrogen donor recycle solvent requirements. which emerged only from the data produced in a continuous, integrated recycle mode of operations, and 2) the more favorable results of low-severity operations, practically solving, in an easy and elegant manner, most if not all the problems encountered by using high-severity operations which were practiced in earlier processes. i.e. German, H-Coal, SRC-11, etc. But perhaps more important to the fundamental research community is the fact that the large set of ITSL data under scrutiny for process development, lacks the fundamental data to support the profound changes in the mechanism and kinetics occurring at low-severity coal liquefaction. Some of the concepts and technology needs are outlined below. Preservation of highly reactive, small fragments in the coal extract is of utmost importance in producing an excellent donor solvent and high quality distillate fuel products. For this purpose, the fragments should be withdrawn from the extraction reactor as soon as they are formed. The unconverted coal can be further converted by recycling it with the preasphaltenes as part of the recycle solvent. Better preservation of the reactive small fragments can be achieved by increasing the donatable hydrogen level and decreasing the heteroatom content of the recycle solvent. It i s important for the superior hydrogen donor solvent to penetrate the less reactive macerals. Consequently, it is advisable to allow for a thermal soaking treatment. i .e., at 250-350°C temperature range for 10-30 minutes, prior to the short contact time (SCT) reaction of rapid heating (two minutes) to the 45OoC exit temperature. It is evident that all the above activities are interdependent and the improvements maximized in an integrated recyle process. It is extremely difficult to capture in research bench scale units the essence of the results produced in the integrated recycle process, because most of the key benefits, i.e., coal conversion and enhanced donor solvent quality, are obtained only after several cycles of the integrated staged operations. Bench scale researchers could avoid the long and tedious recycle operations by applying the aforementioned kinetic model for coal extract hydroprocessing (12) and using proton-NMR data of the coal extract to predict solvent donor capability and yield structure of the upgraded products. Proton-NMR analysis is' rapid, requires small samples, is highly reliable and has excellent reproducibility. Removal of the heteroatoms in the early stage of coal extraction is desirable and ought to be sequential, removing first the more abundant oxygen and thus making easier the subsequent nitrogen removal. 297
Complementary fundamental studies on C-0 and C-N bond scission should be emphasized over the current C-C bond cracking effort. Most of the sulfur is converted to hydrogen sulfide during the two above sequences, and the H S must be kept in the system as catalyst itself and as "activa?or" of transition metal catalysts. It is essential that the ITSL technology be pursued to the completion of the evolutionary trend which became almost dormant with the termination of most of the ITSL projects. It is up to the fundamental research community to fill-up the gap of supportive fundamental research through studies of thermodynamics, kinetics and reaction mechanisms involved in low-severity operations which are part of the ITSL process. Of particular interest would be the matching of reaction kinetics of dehydrogenation of the hydrogen donor solvent with the hydrogen acceptancy of coal extracts. Those of us involved in these efforts are optimistic about the future of low-severity direct coal liquefaction and the quite similar coal/oil co-processing as the practical approaches in helping to alleviate an increasingly energy-deficient world. REFERENCES 1. 2. 3. 4. 5. 6. 7. 8. S. Zaczepinski, Exxon ER&E Co., Private communication, April 1983. A.G. Comolli, E. J. Hippo and E. S. Johanson, "Two-Stage Direct Liquefaction," McGraw-Hill Science and Technology of Synfuels 11, New York City, NY. February 2-4, 1983. E. C. Moroni. F. B. Burke. R. A. Winschel and B. W. Wilson. "Inteqrated Two-Stage Liquefaction Process--Sol Meeting, Seattle, WA, March 20-25, M. Peluso, A. N. Schiffer and H. D. Liquefaction Process (ITSL)". Coal Texas, November 1981. H. D. Schindler, J. M. Chen. M. Pel "The Integrated Two-Stage Liquefact Meeting, New Orleans, LA, November ent Quality Effects," ACS National 983. Schindl er, "The Two-Stage Technology '81 Meeting, Houston, so, E. C. Moroni and J. D. Potts, on Process (ITSL) ," A1Ch.E Annual 981. M. 8. Neuworth, "Advanced in Two-Stage Liquefaction" 9th Energy Technology Conference, Washington, D.C., March 1982. E. C. Moroni, "Future Development for the ITSL Concept," 7th Annual EPRI Contractors' Conference on Coal Liquefaction, Palo Alto, CA. May 11-13, 1983. M. B. Neuworth and E. C. Moroni, "Development of an Integrated Two-Stage Coal Liquefaction Process ," Fuel Processing Technology, 8, (1984) 231-239. Elsevier Science Pub1 ishers. 298
Page 1 and 2:
ABSTRACT LIQUEFACTION CO-PROCESSING
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eaction temperature, 1000-1500 psig
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6. 7. 8. 9. 10. 11. 12. 13. 14. 15
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I 0" 100- I I I WyO-3 P 3: 1500 psi
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11.3 A-6 yJ 600 OF, 1500 psig CO, 3
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Experimental UDqradinq and Cooroces
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catalytic to the thermal hydrogenat
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the reaction with oil production re
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TET did not promote the production
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MICROAUTOCLAVE DESCRIPTION AND PROC
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FEEDSTOCK PROPERTIES Some propertie
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CONCLUSIONS HRI's microautoclave ha
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176
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100. 2 8%. M = ?8. 38. .... . . . .
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CATALYTIC CO-PROCESSINS OF OHIO NO.
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CATALYST COMPARISON STUDY The premi
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fractions and a decrease of heavier
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TABLE 2 Coal Analyses I1 1 i noi s
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Temperature WHSV, G/hr/cc TABLE 6 C
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z FIGURE 3 COAL REACTIVITY SCREENIN
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COPROCESSING USING HzS AS A PROMOTE
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- 3 - that product yields depend on
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- 5 - occurs in the yields of aspha
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Table 1 Analysis of Feedstocks Fore
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THO-STAGE COPROCESSING OF SUBBITUMI
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esult in retrogressive reactions ta
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8. 6. Ignasiak, L. Lewkowicz, G. Ko
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Table 4 OVERALL MASS BALANCE FOR TH
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BACKGROUND COAL LIQUEFACTION/RESID
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system, which could be operated wit
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TABLE 1 EFFECT OF LC-FINING~"' TEMP
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Figure 1. SCHEMATIC OF LCI CO-PROCE
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SIMULATION OF A COAL/PETROLEuII RES
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20 pseudocomponents was developed t
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ottoms is less sensitive to the num
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Low Pressure Separator A temperatur
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7. Gallier, P.W., Boston, J.F., Wu,
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I I I I I I I I I 100- --- Experime
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Coprocessing Schemes The coprocessi
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processing 25,000 and 150,000 bbl/d
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FIGURE 1 I DISTRIBUTION OF REFINERI
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Table 1. Samples Analyzed PNLNumber
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the coal itself. The chemical compo
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- - ITSL PAH Fraction PAH Fraction
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PROCESS DEVELOPMENT STUDIES OF TWO-
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SUMMARY e The major effect of close
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omw '??h 4NO WNID ?N? 000 wmm c9'1'
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Page 99 and 100: qkCqQ r! o! 0 0 0 0 0 0 0 I-UH ')I
Page 101 and 102: Materials The catalyst was shell 32
Page 103 and 104: CONCLUSIONS Separation of a light h
Page 105 and 106: Table 3. Results of activity testin
Page 107 and 108: feed coal and plant configuration a
Page 109 and 110: P1 #2 #3 114 115 #6 ITSL subbitumin
Page 111 and 112: temperature, time and solvent power
Page 113 and 114: TABLE 1 EXPERIMENTAL CONDITIONS AND
Page 115 and 116: la Figure 1. lH-NMR spectra of samp
Page 117 and 118: PERFORMANCE OF THE LOW TEMPERATURE
Page 119 and 120: BENCH UNIT DESCRIPTION Process deve
Page 121 and 122: Recycle Residuum Hydrogenati On Res
Page 123 and 124: FIRST STAGE HRI'S CATALYTIC TWO STA
Page 125 and 126: FIRST-STAQ COAL CONVERSION (W I IIA
Page 127 and 128: REACTOR SOLIOS HTOROGEN/CARBON ATOl
Page 129 and 130: TRANSPORTATION FUELS FROM TWO-STAGE
Page 131 and 132: Process Identification LV% Of AS- R
Page 133 and 134: Table I11 HYDROTREATING TESTS WITH
Page 135 and 136: Table IV HYDROTREATING TO 0.2 PPM N
Page 137 and 138: Table VI EFFECT OF BOILING RANGE ON
Page 139 and 140: (4) In all cases studied, the jet f
Page 141 and 142: 292
Page 143 and 144: INTEGRATED TWO-STAGE LIQUEFACTION:
Page 145: are over-riding features in its fav
Page 149 and 150: Comparative Economics of Two-Stage
Page 151 and 152: The variation in hydrotreating cost
Page 153 and 154: FIGURE 1: COMPARISONS OF ILLINOIS N
Page 155 and 156: Process TABLE 1: TWO-STAGE PROCESSE
Page 157 and 158: Abstract Temperature-Staged Catalyt
Page 159 and 160: Results and Discussion Reactions in
Page 161 and 162: 2. 3. 4. 5. 6. Derbyshire, F. J. an
Page 163 and 164: I LL a rJJW ., .. ;> 0 i s W 8 a 31
Page 165 and 166: Materials Feeds to the WGS-solvent
Page 167 and 168: products. Thus, coupling the WGS an
Page 169 and 170: 5. R. J. Xottenstette, Sandia Natio
Page 171 and 172: ENHANCED COAL LIQUEFACTION WITH STE
Page 173 and 174: change in weight being compared to
Page 175 and 176: I I aromatic ring. The group of sig
Page 177 and 178: T,\llI.l< I ASAI,YSIS OP \\YOl)Al\:
Page 179 and 180: 00 3000 2000 le00 1600 1400 1200 IO
Page 181 and 182: THE EFFECT OF REACTION CONDITIONS O
Page 183 and 184: and may ultiontely form methyl-subs
Page 185 and 186: ! 5. Narain, N.K., Utz, B.R., Appel
Page 187: 4 (u I t + 9 (u I 337 - Q 0
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