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

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un also resulted in more particle disintegration than was observed in the other residues. The microscopic studies of the liquefaction residues reflect the trends shown by the yield data in confirming that the staged catalytic liquefaction produced the Conditions most conducive to coal hydrogenation and liquefaction. From the residue analysis for the subbituminous coal, it appears that the temperature selected for the low-temperature stage was too high as shown by the increase in reflectance of the vitrinite-derived materials in the residues relative to the vitrinite (huminite) in the untreated coal. In contrast, the residues from catalysed bituminous coal hydrogenation display the predominance of hydrogenation reactions as evidenced by the lower vitrinite reflectance compared to the parent coal. Without catalyst, the very obvious development of plasticity indicates the dominating effect of thermal treatment. Effect of Other Reaction Conditions The data presented above have illustrated the potential advantages to be derived by liquefying coals in stages of increasing temperature and in the presence of a catalyst. Verification of these phenomena has been demonstrated more comprehensively and on a larger scale by Hydrocarbon Research Inc. (3). In the laboratory scale studies, no systematic attempt has yet been made to investigate how independent variables such as the reaction conditions in the first and second stages, the solvent composition and the catalyst type and concentration affect the performance attainable in such a reaction sequence. Some preliminary data sre presented in Figure 1 which show the comparative affects on the product distribution for the subbituminous coal (PSOC-1401) due to (i) increasing the high temperature residence time from 10 to 45 min while employing naphthalene as solvent and (ii) using the more reactive process solvent and the 45 min high-temperature residence time. With naphthalene, increasing the reaction time at high-temperature is evidently advantageous in promoting further interconversion of oils to asphaltenes (the oil to asphaltene ratio increased from 0.8 to 2:l) with some simultaneous increase in gas make; the CO yield increased from 7.9 to 9.8% and the yield of C -C hydrocarbons increased frh 0.8 to 3.0%. As in the other experiments using nabhthalene as solvent, there was no significant conversion of naphthalene to tetralin. A much more dramatic change in product selectivity was achieved by using the process solvent when the oil to asphaltene ratio increased to approximately 14:l. To offset this gain there was a more significant increase in gas make; the CO and C -c yields being 12.2 and 4.7%. respectively. Quite evidently, the composition of 4 the solvent is an important parameter even in the presence of an active catalyst. Acknowledgements Three of the authors, Derbyshire, Epstein. and Stansberry, wish to acknowledge the financial support of the Department of Energy, Grant No. DE-FE22-83PC60811 and Contract No. DE-FG-22-84PC7003. Frank Derbyshire wishes to scknowledge Dr. Frank Burke of Conoco Coal Research for his helpful discussions and contributions and Dr. Eneo Moroni for his steadfast support. References 1. Derbyshire, F. J., Davis, A., Lin. R., Stansberry. P. G., and Terrer, 14.-T., Accepted for publication in Fuel Proc. Tech. 310 A
2. 3. 4. 5. 6. Derbyshire, F. J. and Luckie, P. T.. Quarterly Report to U.S. DOE for the Period July 1st-September 30th, 1985, Contract No. DE-FG-22-84-PC7003. Comolli, A. G., MacArthur, J. B., and McLean, J. B.. Proc. Tenth Annual EPRI Contractors' Conference on Clean Liquid and Solid Fuels, 1985, p. 2-1. Derbyshire, F. J., Davis, A., Lin, R., Stansberry, P. G., and Terrer, M.-T.. ACS Fuel Division Preprints, 1985, 30. No. 4, 326. Mitchell, G. D., Davis, A.. and Spackman, W., in R. T. Ellington, ed., "Liquid Fuels from Coal." pp. 245-270. Academic Press, 1977. Shibaoka. M., Fuel, 60. 240-246, 1981. 311 al a e Y u 0 4 I( s i: 3 ij a Q Y U n t .I m 4 Q P) a Y 9 al a al Y 8 4 x t"
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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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tl f 246
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248
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qkCqQ r! o! 0 0 0 0 0 0 0 I-UH ')I
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Materials The catalyst was shell 32
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CONCLUSIONS Separation of a light h
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Table 3. Results of activity testin
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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 and 146: are over-riding features in its fav
Page 147 and 148: Complementary fundamental studies o
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: Results and Discussion Reactions in
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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