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

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THE EFFECT OF REACTION CONDITIONS ON SOLVENT LOSS DURING COAL LIQUEFACTION Bruce R. Utz and Sidney Friedman U.S. Department of Energy Pittsburgh Energy Technology Center P.O. Box 10940 Pittsburgh, PA 15236 INTRODUCTION The fate of a coal-liquefaction recycle solvent during Integrated Two-Stage Liquefaction (ITSL) and other direct liquefaction processes is a major concern. If the solvent has an inadequate concentration of hydrogen donors or other solvent components that might enhance liquefaction, then the quality of the solvent will be degraded and conversion to liquid products will be adversely affected. Studies using the solvents phenol (l), tetrahydroquinoline (2-4), quinoline (5), and pyridine (6) have shown that these compounds are partially incorporated by covalent bonds, but a relatively large amount is h drogen bonded to coal-derived products. In other studies using pure "C- and '*C-labeled aromatic or hydro- aromatic compounds as solvents (3,6-8), the amount of adduction was determined. Although adduction and hydrogen bonding of solvent components account for solvent loss, other degradative reactions also account for loss of original solvent and solvent quality. Ring contraction of tetralin (9), and octahydrophenan- threne (8,lO) under coal-liquefaction conditions reduces the hydrogen-donor concentration and therefore the solvent quality. The use of a one-component solvent system can be misleading because reactions with coal may be occurring that normally would not occur if other components of a solvent were present. The objective of this study was to examine a multicomponent synthetic solvent and determine if solvent components are preferentially lost or degraded during short-contact-time liquefaction (SCTL) , and how solvent loss in SCTL compares with other liquefaction conditions that involve gradual heat-up. EXPERIMENTAL Experiments were performed in a microreactor assembly (11) consisting of a 316 stainless steel 1/2-in. union tee with two end caps. Five grams of a synthetic solvent and one gram of moisture-free Western Kentucky 9/14 coal were added to the microreactor, which was assembled and pressurized to 1100 psig with Hz. The synthetic solvent consisted of 4% quinoline, 13% m-cresol, 20% tetralin, 33% 1-methylnaphthalene, 20% phenanthrene, and 10% pyrene. Experiments were conducted with one- and two-component solvents and coal in order to identify unique products from each of the simple solvent systems. The two-component solvent consisted of 20% pyrene and 80% tetralin, or 20% phenanthrene and 80% tetralin. One- component solvents of 1-methylnaphthalene, tetralin, and m-cresol were also used. The microreactor assembly was attached to a wrist-action shaker that moved the reactor through a small arc for adequate mixing of the reactor contents. The shaker was positioned above a vertically moving platform that supported a fluidized sand bath (11). For SCTL experiments, the bath was heated to an initial temperature of 46OOC. When the experiment was initiated, the temperature set point was changed to 425OC and the platform (with bath) was raised, immersing the microreactor. Heat-up to 425oC took approximately 1 min. Reaction time was 3 min at 425OC. For experiments conducted under traditional or severe conditions, the reactor was immersed in the sand bath, which was at room temperature, gradually heated (55 min) to 425oC, and held at reaction temperature for 30 min or 6 hours. At the end of the 331
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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
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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
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 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: 00 3000 2000 le00 1600 1400 1200 IO
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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