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

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i 2a t . 5 10 15 20 15 n I5 UI 45 0 Irtentlo" TI-. .I". Figure 2. Gas chromatograms of samples from experiment 5. (a) feed oil, (b) wax, (c) dewaxed oil. (internal standard, n-decane) c 267
PERFORMANCE OF THE LOW TEMPERATURE FIRST STAGE OF HRI 'S CATALYTIC TWO-STAGE LIQUEFACTION PROCESS J. B. McLean, A. G. Comolli and T. 0. Smith Hydrocarbon Research, Inc. (A Subsidiary of Dynalectron Corporation) P. 0. Box 6047 Lawrenceville, New Jersey 08648 ABSTRACT Hydrocarbon Research, Inc. (HRI), under the sponsorship of the U. S. Department of Energy (DOE), is developing a catalytic two-stage coal liquefaction process. The process consists of two direct-coupled ebullated-bed reactors in series, with the first stage operated at lower temperatures (t800'F) than typically used in direct liquefaction. Studies of both bituminous and sub-bituminous coals in a nominal 50 lb/day continuous, integrated recycle bench unit have shown con- siderable improvements in both distillate yield and product quality over other processes. In order to better understand the chemistry of the unique first-stage reactor conditions, a special on-line sampling system was added to the bench unit. Samples obtained over a wide range of operating conditions indicate that the first stage is an efficient hydrogenation system, achieving balanced rates of coal conversion and dissolution. solvent to coal hydrogen transfer, solvent regeneration, and liquefaction product upgrading and stabilization. Differences in responses of the two coals studied are noted and discussed. INTRODUCTION Hydrocarbon Research, Inc. (HRI) has long been actively involved in the development of coal liquefaction process technology. The H-Coal@ Process, featuring a single-stage ebul lated-bed catalytic reactor, was successfully developed and demonstrated through operation of a 200 ton per day pilot plant at Catlettsburg. Kentucky, in the early 1980's.(l) In 1981-1982, HRI conducted a series of laboratory investigations to evaluate various two-stage liquefaction concepts which featured a thermal first-stage re ctor followed by a closely coupled, ebullated bed, catalytic second stage.(2-6f The results of these programs formed the basis for the ctirrent Catalytic Two-Stage Liquefaction (CTSL) concept, which features two direct-coupled, ebullated-bed reactors in series. Under OOE sponsorship, HRI has been conducting a development rogram for the CTSL Process Since 1983. Program results have been re~orted(7-~~) with C4-975OF distil late yields of 65 W I MAF coal achieved for both Illinois No. 6 and Wyodak coals. The process economics have been shown to be favorable in c parison with other twostage approaches by an independent contractor's study(12?for both coals. 268 i
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
Page 65 and 66: SIMULATION OF A COAL/PETROLEuII RES
Page 67 and 68: 20 pseudocomponents was developed t
Page 69 and 70: ottoms is less sensitive to the num
Page 71 and 72: Low Pressure Separator A temperatur
Page 73 and 74: 7. Gallier, P.W., Boston, J.F., Wu,
Page 75 and 76: I I I I I I I I I 100- --- Experime
Page 77 and 78: Coprocessing Schemes The coprocessi
Page 79 and 80: processing 25,000 and 150,000 bbl/d
Page 81 and 82: FIGURE 1 I DISTRIBUTION OF REFINERI
Page 83 and 84: Table 1. Samples Analyzed PNLNumber
Page 85 and 86: the coal itself. The chemical compo
Page 87 and 88: - - ITSL PAH Fraction PAH Fraction
Page 89 and 90: PROCESS DEVELOPMENT STUDIES OF TWO-
Page 91 and 92: SUMMARY e The major effect of close
Page 93 and 94: omw '??h 4NO WNID ?N? 000 wmm c9'1'
Page 95 and 96: tl f 246
Page 97 and 98: 248
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: la Figure 1. lH-NMR spectra of samp
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 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
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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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