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

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- TABLE 2: CONCEPTUAL COMMERCIAL PLANT SUMMARIES Rouu: input Slam hi. TPD (UF) Garifl~r Cod. TPD (MF) TOW PIml W, TPD (MF) - OUlpUl SNQ, MMSCFD Raw 4 + Uguld, BPSD Total Llquld Vkld aflw Hydrolnatmenl, BPSD Process: ILLINOIS NO. 6 COAL FEED WYOMING COAL FEED Lummus Wilsonville Wilsonville ITSL ITSL DIEL CTSL ---- - Input Steam Coal, TPD (MF) Gaslfier Coal, TPD (MF) 3,000 0 2,000 3.000 2,000 4.000 4,000 s,m Total Plant Coal, TPD (MF) 33,000 36.000 36,OOO 43,OOO Output SNG, MMSCFD Raw C4 + Liquld, BPSD 33 70,000 26 00.000 6 97,000 3 114,000 Total Liquid Yield after Hydrotreatment. BPSD 80,OOO 94,OOO 96,OOO 119,OOO 307
Abstract Temperature-Staged Catalytic Coal Liquefaction Frank Derbyshire, Alan Davis, Mike Epstein, and Peter Stansberry College of Earth and Mineral Sciences The Pennsylvania State University University Park, PA 16802, USA Coal liquefaction has been investigated under conditions where reaction is conducted in successive stages of increasing temperature and in the presence of a dispersed sulfided Mo catalyst. This sequence leads not only to high conversions but also greatly increases the selectivity of the products to oils at the expense of asphaltenes, with only marginal increase in gas make. The product distribution is strongly influenced by the solvent composition and the reaction conditions in the two stages. Examination of the liquefaction residues from the liquefaction of a bituminous and a subbituminous coal has provided supporting evidence to show that the temperature-staged reaction sequence favors hydrogenative processes. Moreover, the choice of reaction conditions for optimum performance is rank-dependent; for example, low-rank coals appear to require a lower first stage temperature than bituminous coals in order to minimize the potential for regressive reactions. Introduction In some earlier reported research (1,2) a bituminous and a subbituminous coal were pretreated by dry catalytic hydrogenation, using a molybdenum catalyst at 35OoC for 1 h, following which they were mixed with naphthalene (2:l solvent to coal ratio) and reacted at 425OC for 10 min. The results showed that the low-temperature pretreatment improved both the net coal conversion, based upon solubility in tetrahydrofuran, and the product distribution. Notably, the oil to asphaltene ratio was substantially increased with only marginal additional gas make. Based upon these findings, further research has been directed to investigating the chemistry and the potential of temperature-staged coal liquefaction. The results of this research are presented in this paper. Similar studies are being conducted on a larger scale by Hydrocarbon Research Inc. (3). Experimental Coal Preparation Samples of bituminous and subbituminous coal were provided by the Penn State Coal Sample Bank for use in this research. The coals were obtained undried and in lump form about 12 mm size and were crushed in a glove box under oxygen-free nitrogen to 0.8 mm top size. The crushed coals were subdivided by riffling into a number of 10 g representative samples and sealed in vials under nitrogen. Properties of the coals are shown in Table 1. The coals were impregnated with Mo catalyst by slurrying with an aqueous solution of ammonium tetrathiomolybdate in the concentration necessary to attain a loading of 1% wt Mo on a dmmf basis. The quantity of coal impregnated was sufficient for a complete series of experiments. After slurrying, the excess water was removed by vacuum freeze-drying. Liquefaction The impregnated coal was mixed in a ratio of 1:2 with liquefaction solvent. In most of the experiments, naphthalene was selected as the solvent because, at least 308 I ' I 1
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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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
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 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: Process TABLE 1: TWO-STAGE PROCESSE
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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