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

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Table 5 Elemental Composition of PS and BS Fractions from Coprocessing Temperature ps BS Reactants QC Catal vst % C %H % C %H Maya TLR 400 None 84.5 11.4 + Coal 84.0 11.3 82.8 Maya TLR 400 Ni Mo/A12O3 84.8 10.9 84.6 + Coal 84.8 10.9 86.8 Maya TLR 400 + Coal Maya TLR 425 + Coal Maya TLR 400 + Coal + TET Maya-TLR 400 + Coal + TET Maya TLR 425 + Coal t TET Mo Naphthenate 84.3 10.8 83.6 84.3 10.8 84.1 Mo Naphthenate 85.7 11.0 84.6 10.6 86.3 84.9 10.7 85.1 85.1 10.6 None 86.3 10.1 83.8 86.4 10.1 83.5 NiMo/A1203 87.8 10.5 87.1 10.5 86.0 85.7 10.3 84.7 87.4 10.5 Mo Naphthenate 86.9 10.5 85.6 86.5 10.3 85.7 The presence of TET in the coal/resid/Mo naphthenate system did not substantially change the product slate. Coal conversion, hydrogen consumption and oil production were the same as the reaction without TET. The total amount of NAPH formed during the reaction was 1.5 mmoles which fell between that for the thermal and NiMo/Al 03 reactions. Ten times as much NAPH was formed as DEC. The H2 utilized by the 60 naphthenate systems, 57.5 mmoles without TET and 52.5 mmoles with TET, was high compared to the other reactions performed. The product slates from these Mo naphthenate reactions show the effective utilization of H2 in terms of coal conversion and oil production. 1The addition of catalyst in the residuum upgrading reactions increased the amount of oil production achieved and, in the case of NiMo/Al 03, substantially increased the IOM formed. The presence of TET had varying effect; but only in the reaction with NiMo/AlzOj did TET improve the oil production. In all upgrading reactions, the BS fraction was reduced during the reaction forming both 1 ighter and heavier products. The catalytic reactions with NiMo/A1203 and Mo naphthenate at 425OC reduced the BS fraction the most. The combination of TET plus NiMo/A120 resulted in the greatest reduction of the BS fraction and subsequent increase in $he PS fraction. In the coprocessing experiments, both the addition of catalyst and the addition of tetralin promoted coal conversion. For the NiMo/Al2Og reactions, the combination of catalyst and tetra1 in synergetical ly promoted coal conversion. With Mo naphthenate, coal conversion was high (89.5%) without TET addition and no change was observed with the addition of TET. Thus, with a highly accessible and active catalyst, additional hydrogen donation from the solvent had 1 ittle influence on coal conversion. Therefore, coal conversion in coprocessing appears to be dependent upon both catalyst and hydrogen donation except in the case of a highly active catalyst where catalytic activity predominates. 167 7.1 7.4 7.3 7.2 7.2 6.4 6.8 6.9 7.0 7.0 7.1 6.6 6.6
TET did not promote the production of PS materials in either the thermal or catalytic reactions. In fact, in the thermal reactions the presence of TET was detrimental to oil production. The effect of TET and catalytic treatment on BS production is also instructive in examining the roles and relative importance of these two factors in coprocessing. BS production is defined as the difference between the final BS and the initial BS divided by the upgradeable material which is maf coal. Compared to the thermal reaction at 4OO0C, the addition of TET increased the amount of BS production (Table 3). Catalytic treatment at 4OO0C did not increase the BS production; however, the addition of TET to reaction system with NiMo/A120j at 4OO0C did enhance BS production. At 425OC, the presence of NiMo/Al 03 and Mo naphthenate increased the 8s production as shown in Table 4. The aidition of TET to the Mo naphthenate reaction again increased the BS production. Since all of these reactions showed positive oil production, the increases observed in the BS production were directly related to the upgrading of liquefied coal to BS products. Thus, the presence of TET assisted in the production of BS but not in the production of PS. The presence of a hydrotreating catalyst was required for oil production in the coprocessing reactions. References 1. Monnier, J. CANMET Report 84-5E, "Review of the Coprocessing of Coals and Heavy Oils of Petroleum Origin", March 1984. 2. Curtis, C.W., Tsai, K.J., Guin, J.A., Ind. Enq. Chem. Proc. Des. Dev., 1985, - 24, 1259. 3. Curtis, C.W., Tsai, K.J., Guin, J.A., submitted to Ind. Ena. Prod. Res. and Dev., 1986. 4. Kottensette, R.J., Sandia Report SANDB2-2495, March 1983. 5. Bearden, R. and Aldridge, C.L., U.S. Patent 4,134,824, 1979. 6. 7. Curtis, C.W., Tsai, K.J., and Guin, J.A., in press, Fuel Proc. Tech., 1986. Moody, T. Master's Thesis, Auburn University, 1985. Acknowledgments The authors gratefully acknowledge the Department of Energy for support of this work under Contract Nos. DEFG2282PC50793 and DEFG2285PC80502. 168 j
Page 1 and 2: ABSTRACT LIQUEFACTION CO-PROCESSING
Page 3 and 4: eaction temperature, 1000-1500 psig
Page 5 and 6: 6. 7. 8. 9. 10. 11. 12. 13. 14. 15
Page 7 and 8: I 0" 100- I I I WyO-3 P 3: 1500 psi
Page 9 and 10: 11.3 A-6 yJ 600 OF, 1500 psig CO, 3
Page 11 and 12: Experimental UDqradinq and Cooroces
Page 13 and 14: catalytic to the thermal hydrogenat
Page 15: the reaction with oil production re
Page 19 and 20: MICROAUTOCLAVE DESCRIPTION AND PROC
Page 21 and 22: FEEDSTOCK PROPERTIES Some propertie
Page 23 and 24: CONCLUSIONS HRI's microautoclave ha
Page 25 and 26: 176
Page 27 and 28: 100. 2 8%. M = ?8. 38. .... . . . .
Page 29 and 30: CATALYTIC CO-PROCESSINS OF OHIO NO.
Page 31 and 32: CATALYST COMPARISON STUDY The premi
Page 33 and 34: fractions and a decrease of heavier
Page 35 and 36: TABLE 2 Coal Analyses I1 1 i noi s
Page 37 and 38: Temperature WHSV, G/hr/cc TABLE 6 C
Page 39 and 40: z FIGURE 3 COAL REACTIVITY SCREENIN
Page 41 and 42: COPROCESSING USING HzS AS A PROMOTE
Page 43 and 44: - 3 - that product yields depend on
Page 45 and 46: - 5 - occurs in the yields of aspha
Page 47 and 48: Table 1 Analysis of Feedstocks Fore
Page 49 and 50: THO-STAGE COPROCESSING OF SUBBITUMI
Page 51 and 52: esult in retrogressive reactions ta
Page 53 and 54: 8. 6. Ignasiak, L. Lewkowicz, G. Ko
Page 55 and 56: Table 4 OVERALL MASS BALANCE FOR TH
Page 57 and 58: BACKGROUND COAL LIQUEFACTION/RESID
Page 59 and 60: system, which could be operated wit
Page 61 and 62: TABLE 1 EFFECT OF LC-FINING~"' TEMP
Page 63 and 64: Figure 1. SCHEMATIC OF LCI CO-PROCE
Page 65 and 66: SIMULATION OF A COAL/PETROLEuII RES
Page 67 and 68:
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
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P1 #2 #3 114 115 #6 ITSL subbitumin
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temperature, time and solvent power
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TABLE 1 EXPERIMENTAL CONDITIONS AND
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la Figure 1. lH-NMR spectra of samp
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PERFORMANCE OF THE LOW TEMPERATURE
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BENCH UNIT DESCRIPTION Process deve
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Recycle Residuum Hydrogenati On Res
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FIRST STAGE HRI'S CATALYTIC TWO STA
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FIRST-STAQ COAL CONVERSION (W I IIA
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REACTOR SOLIOS HTOROGEN/CARBON ATOl
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TRANSPORTATION FUELS FROM TWO-STAGE
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Process Identification LV% Of AS- R
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Table I11 HYDROTREATING TESTS WITH
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Table IV HYDROTREATING TO 0.2 PPM N
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Table VI EFFECT OF BOILING RANGE ON
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(4) In all cases studied, the jet f
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292
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INTEGRATED TWO-STAGE LIQUEFACTION:
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are over-riding features in its fav
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Complementary fundamental studies o
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Comparative Economics of Two-Stage
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The variation in hydrotreating cost
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FIGURE 1: COMPARISONS OF ILLINOIS N
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Process TABLE 1: TWO-STAGE PROCESSE
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Abstract Temperature-Staged Catalyt
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Results and Discussion Reactions in
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2. 3. 4. 5. 6. Derbyshire, F. J. an
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I LL a rJJW ., .. ;> 0 i s W 8 a 31
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Materials Feeds to the WGS-solvent
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products. Thus, coupling the WGS an
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5. R. J. Xottenstette, Sandia Natio
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ENHANCED COAL LIQUEFACTION WITH STE
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change in weight being compared to
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I I aromatic ring. The group of sig
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T,\llI.l< I ASAI,YSIS OP \\YOl)Al\:
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00 3000 2000 le00 1600 1400 1200 IO
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THE EFFECT OF REACTION CONDITIONS O
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and may ultiontely form methyl-subs
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! 5. Narain, N.K., Utz, B.R., Appel
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4 (u I t + 9 (u I 337 - Q 0
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