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

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COllpARISON OF FIRST-STAGE OIL AND PFL PROPERTIES Bench Unit Coal Conversion, W % MAF Microautoclave Sol vent Quality Test. W % THF Conversion HRI\Il Conoco (2) * H/C Ratio - 650-850°F 850-975'F 975'F+ Proton? NMR - X Aromatics 850°F- Di sti 1 late 85OoF+ Residuum TABLE 3 ILLINOIS NO. 6 COAL YYODAK COAL Run No. 227-18-12 Run No. 227-25-16 < ___________ s T A GI s -----_------ > ---- FIRST SECOND FIRST SECOND OIL PFL OIL PFL -- -- 87.1 92;7 73.6 91.6 83.3 82.9 1.28 1.19 0.95 14.6 29.2 (1) HRI procedure uses matched coal and solvent. (2) Conoco procedure uses Indiana V coal. Data provided by CONOCO. W % 975"F+ In Oil 97iV[+H;;p;erti es X Nitrogen % Oil % Asphal tenes % Preasphaltenes Estimated Net 9750Ft Yield - W % MAF Coal Oils Asphal tenes Pre-Asphal tenes TOTAL - 975OF' RESIDUUM PROPERTIES 76.6 54.5 52.0 79.9 64.5 64 .O 1.25 1.40 1.40 1.13 1.34 1.24 0.91 1.06 0.98 15.7 11 .o 10.6 31.4 19.3 25.3 ILLINOIS NO. 6 WYOOAK Run 227-32-9 Run 227-25-16 < _______ S T A G S _______ > First Second First Second - 39.5 1.03 0.65 64.5 28.6 6.9 9.6 9.3 3.3 22.2 2 79 32.1 0.99 0.53 71.9 23.5 4.6 -3.2 -7.2 -2.9 -13.3 - 12.1 1.06 0.79 75.3 24.1 0.6 2.4 2.2 0.1 - 4.7 9.0 0.98 0.73 84.7 15.0 0.3 -0.2 -1 .R -0.1 - -2.1 TABLE 4
TRANSPORTATION FUELS FROM TWO-STAGE LIQUEFACTION PRODUCTS Richard F. Sullivan Chevron Research Company, P. 0. Box 1627 Richmond, California 94802-0627 INTRODUCTION FOK several years, Chevron Research Company under a contract with the US Department of Energy has been studying the refining of coal liquids. Detailed results are given in a series of DOE Interim Reports (1). The earlier work emphasized upgrading of products from single-stage processes: SRC-11, H-Coal, and EDS. More recently, we have been studying products from two different two-stage processes: the Integrated Two-Stage Liquefaction (ITSL) Process and the Catalytic Two-Stage Liquefaction (CTSL) Process. The purpose of this paper is to compare results for syncrudes from single-stage and two-stage processes, from different two-stage processes, from different coals [Illinois No. 6 (bituminous) and wyodak (subbituminous)], and of different boiling ranges from a given coal and process. The ITSL process, developed by Cities Service and Lummus Crest, Inc., operates with a high temperature (over 80O0F) first stage with no added catalyst. The product is then deashed, and sent to a second-stage that operates at lower temperatures (typically below 800OF) with an ebullated catalyst bed (2). The CTSL process, developed by Hydrocarbon Research, Inc. (HRI), operates with two catalytic ebullated-bed stages. In contrast to the ITSL process, the CTSL first stage operates at a lower temperature (below 8 OOOF) than the second (!which operates above 800°F) (3). Depending upon how each liquefaction process is operated, the end point (EP) of the net whole-liquid product will vary. Typically, part or all of the vacuum gas oil (VGO) made by the process is used as recycle solvent for the coal. Some or all of it is ultimately converted to lower boiling products. Thus, the net whole-liquid product can have an EP ranging from below 65OoF to over 85OOF. As we will see, the ease or difficulty of upgrading is affected to a large extent by product EP. The 650-850'F VGO is relatively difficult to upgrade, but is reported to be an excellent recycle solvent. Therefore, there may be both upstream and downstream advantages to recycling this VGO, as shown for example, by MacArthur et a1 (4). Ultimately, of course, the costs and yields of both liquefaction and upgrading must be used to determine the optimum EP. In this paper, we will use results for upgrading products from the H-Coal process (1, 5) as our primary basis for comparison with single-stage processes. FEEDSTOCKS Key factors that determine how easy or difficult a particular syncrude is to refine are EP, boiling range, hydrogen content, and heteroatom content. Also, hot-heptane insoluble compounds (low- solubility polycyclic-aromatic and polar compounds, asphaltenes, and ash) can make syncrudes difficult to processes. 280
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
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 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: REACTOR SOLIOS HTOROGEN/CARBON ATOl
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\:
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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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