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

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Figure 2. Schematic flow diagram for a two-stage liquefaction process via WGS-solvent production. TABLE 1 Results of Coal Liquefaction Experiments a Exp. Solvent: Conversions (% dmmf basis) No. Coal THF C, C,- C, ----- l b 3:l 30 17 1.6 2c 2:l 91 21 2.9 3' 3:l 97 42 3.1 4' 4:l 98 48 3.1 a) b) C) Performed with WGS-produced solvent. Products Solvent Hydrogen Balance (X donatable hydrogen) To Coal To Gas Remaining -- 90 9 1 04 11 5 69 11 20 Reaction conditions for all experiments: 445 C, 36 min, 450 psig cold chorge nitrogen. No gas-phase hydrogen used. Performed with flow reactor feed solution. PAH's only; no donatable solvent hydrogen.
ENHANCED COAL LIQUEFACTION WITH STEAM PRETREATMENT P.R. Bienkowski, R. Narayan, R.A. Greenkorn and K.C. Chm' School of Chemical Engineering Purdue University West Lafayette, Indiana 47907 SUMMARY A two step process for the liquefaction of coal, in a semi-Eow micro reactor, was investigated. The process consisted of pretreating coal with low temperature steam, followed by treatment with supercriti- cal steam. The maximum observed conversion of a Wyodak subbituminous coal, using this two step process, was 40 wt% on a moisture and ash free basis (MAF). The 240 ' c pretreatment step resulted io a 32% increase over the conversion observed with just a 400 c treatment. The coal liquid obtained has a number average molecular weight of 325 and a mass average molecular weight of 373, with a narrow molecular weight distribution. The hydrogen and oxygen content of the extract is increased, a significant amount of the oxygen is present as dihydroxyl aromatics. A highly condensed residue of lower hydrogen and oxygen content is obtained which can be of value as a solid fuel. INTRODUCTION Recent investigations have led to the observation (1) that in its native unweathered state coal is a reactive material, far from being the inert solid that it is commonly regarded. Extensive hydrogen bonds connect the poly nuclear aromatic cluster to form a semi-permanent macro molecular structure. The structure is particularly fragile in subbituminous coals, and may le subject to rupture with mild treat ment to dissociate the hydrogen bonds. GraU and Brandes (2) found that carbon conversion to liquids in pyroiysls at 940 c was raised from 23% to over 50% if the coal was exposed to steam for times less than 30 minutes at temperatures between about 320 and 360 O c. Both pretreatment and pyrolysis were conducted in 50 atm of steam. This result suggests that coal is partially depolymerized by the steam pretreatment, perhaps by the removal of oxygen linkages. If this is indeed the case, improved yields and/or lighter liquids should result if the pretreated coal is liquefied instead of pyrolyzed. 321
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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
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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
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
Page 167 and 168: products. Thus, coupling the WGS an
Page 169: 5. R. J. Xottenstette, Sandia Natio
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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