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Special Equipment in the Coal-Hydrogenation Demonstration Plant

Description: Report issued by the Bureau of Mines over the equipment used in coal hydrogenation demonstration plants. Detailed descriptions of the equipment and machinery are presented. This report includes tables, illustrations, and photographs.
Date: January 1950
Creator: Markovits, J. A.; Braun, K. C.; Donovan, J. T. & Sandaker, J. H.
Partner: UNT Libraries Government Documents Department

Advanced direct coal liquefaction concepts - appendix

Description: This detailed appendix presents the results of direct coal liquefaction studies performed by the contractor. Several hundred tables summarizing the chemical compostion for runs of a bench scale reactor are presented.
Date: July 1, 1994
Creator: Berger, D. J.; Parker, R. J. & Simpson, P. L.
Partner: UNT Libraries Government Documents Department

Physical Parameters in Synthoil Process, Quarterly Report: October-December 1975

Description: This work is being done in support of the development of processes for converting coal to liquid fuel of low sulfur content, suitable for use in power production. Most of the effort is intended to produce information applicable to the SYNTHOIL Process. In the SYNTHOIL Process for converting coal to a low-sulfur fuel oil, coal is liquefied and hydro-desulfurized in a turbulent-flow, catalytic packed-bed reactor. A slurry of coal in recycled oil is reacted with hydrogen at 450 degrees C and 2,000 to 4,000 psi in the presence of Co-MoSiO2-Al2O3 catalyst. The turbulent flow of fluid prevents the coal's mineral matter from settling and plugging the reactor. The gross liquid products are centrifuged to remove the unreacted solids. The centrifuged liquid product is a low-S, low-ash fuel. The following four tasks are included: (1) heat of reaction of hydrogen with coal slurries; (2) heat transfer coefficient; (3) additives to facilitate separation of solids from liquids; and (4) catalyst testing. These are now in the planning stage of development.
Date: 1976
Creator: Fischer, J.; Lo, R.; Nandi, S.; Fredrickson, D.; Bump, T. R.; Mulcahey, T. P. et al.
Partner: UNT Libraries Government Documents Department

Advanced Direct Liquefaction Concepts for PETC Generic Units - Phase II

Description: The results of Laboratory and Bench-Scale experiments and supporting technical and economic assessments conducted under DOE Contract No. DE-AC22-91PC91040 are reported for the period July 1, 1997 to September 30, 1997. This contract is with the University of Kentucky Research Foundation which supports work with the University of Kentucky Center for Applied Energy Research, CONSOL, Inc., LDP Associates, and Hydrocarbon Technologies, Inc. This work involves the introduction into the basic two stage liquefaction process several novel concepts which include dispersed lower-cost catalysts, coal cleaning by oil agglomeration, and distillate hydrotreating and dewaxing. Results are reported from experiments in which various methods were tested to activate dispersed Mo precursors. Several oxothiomolybdates precursors having S/Mo ratios from two to six were prepared. Another having a S/Mo ratio of eleven was also prepared that contained an excess of sulfur. In the catalyst screening test, none of these precursors exhibited an activity enhancement that might suggest that adding sulfur into the structure of the Mo precursors would be beneficial to the process. In another series of experiments, AHM impregnated coal slurried in the reaction mixture was pretreated withH S/H under pressure and successively heated for 30 min at 120, 250 2 2 and 360 C. THF conversions in the catalyst screening test were not affected while resid conversions o increased such that pretreated coals impregnated with 100 ppm Mo gave conversions equivalent to untreated coals impregnated with 300 ppm fresh Mo. Cobalt, nickel and potassium phosphomolybdates were prepared and tested as bimetallic precursors. The thermal stability of these compounds was evaluated in TG/MS to determine whether the presence of the added metal would stabilize the Keggin structure at reaction temperature. Coals impregnated with these salts showed the Ni and Co salts gave the same THF conversion as PMA while the Ni salt gave higher ...
Date: December 1, 1997
Partner: UNT Libraries Government Documents Department

Low Severity Coal Liquefaction Promoted by Cyclic Olefins

Description: The development of the donor solvent technology for coal liquefaction has drawn a good deal of attention over the last three decades. The search for better hydrogen donors led investigators to a class of compounds known as cyclic olefins. Cyclic olefins are analogues of the conventional hydroaromatic donor species but do not contain aromatic rings. The cyclic olefins are highly reactive compounds which readily release their hydrogen at temperatures of 200 C or higher. Considerable effort has been o expended toward understanding the process of hydrogen donation. Most of this work was conducted in bomb reactors, with product analysis being carried out after the reaction was complete. Efforts directed towards fundamental studies of these reactions in situ are rare. The current work employs a high temperature and high pressure infrared cell to monitor in situ the concentrations of reactants and products during hydrogen release from hydrogen donor compounds.
Date: April 9, 1998
Creator: Curtis, Christine W.
Partner: UNT Libraries Government Documents Department

Free-radical kinetics of coal liquefaction

Description: A rate expression with first- and second-order terms in the concentration of extractable compounds in solid coal particles is derived from a fundamental free-radical mechanism. The expression was suggested empirically by prior experiments for coal liquefaction in the presence of a hydrogen-donor solvent. Radical reactions are considered to occur in both coal and in solvent. The long-chain approximation justifies the neglect of initiation, hydrogen abstraction, and termination rates as quantitatively insignificant relative to propagation reaction rates.
Date: July 16, 1994
Creator: Wang, M.; Smith, J.M. & McCoy, B.J.
Partner: UNT Libraries Government Documents Department

Surface Modified Coals for Enhanced Catalyst Dispersion and Liquefaction

Description: The aim of this study is to enhance catalyst loading and dispersion in coal for improved liquefaction by preadsorption of surfactants and catalysts on to the coal. During this reporting period, the effects of dodecyl dimethyl ethyl ammonium bromide (DDAB) (a cationic surfactant), sodium dodecyl sulfate (SDS) (an anionic surfactant), Triton X-100 (a neutral surfactant), and ferrous sulfate (as a catalyst precursor) on the coal surface charge at various pH values were determined. The results of the zeta potential measurements suggest that ferrous sulfate as catalyst precursor creates a distinctly different condition on the coal surface compared to that of molybdenum as reported in the previous progress reports. The effects of the adsorption of the surfactants also varied distinctly with the type of surfactant. With the adsorption of DDAB, the cationic surfactant, the surface charge was more positive. The opposite effect was observed for the SDS, the anionic surfactant. The coals treated with Triton X-100, the neutral surfactant, also showed an overall negative surface charge density. The adsorption of the catalyst precursor (ferrous sulfate) resulted in a net negative charge on the coal surface.
Date: December 4, 1998
Creator: Yeboah, Yaw D.
Partner: UNT Libraries Government Documents Department

Advanced Direct Liquefaction Concepts for PETC Generic Units - Phase II

Description: Reported here are the results of Laboratory and Bench- Scale experiments and supporting technical and economic assessments conducted under DOE Contract No. DE- AC22- 91PC91040 during the period April 1, 1997 to June 30, 1997. This contract is with the University of Kentucky Research Foundation which supports work with the University of Kentucky Center for Applied Energy Research, CONSOL, Inc., LDP Associates, and Hydrocarbon Technologies, Inc. This work involves the introduction into the basic two stage liquefaction process several novel concepts which includes dispersed lower- cost catalysts, coal cleaning by oil agglomeration, and distillate hydrotreating and dewaxing. This report includes a data analysis of the ALC- 2 run which was the second continuous run in which Wyodak Black Thunder coal was fed to a two kg/ h bench- scale unit. One of the objectives of that run was to determine the relative activity of several Mo- based coal impregnated catalyst precursors. The precursors included ammonium heptamolybdate (100 mg Mo/ kg dry coal), which was used alone as well as in combination with ferrous sulfate (1% Fe/ dry coal) and nickel sulfate (50 mg Ni/ kg dry coal). The fourth precursor that was tested was phosphomolybdic acid which was used at a level of 100 mg Mo/ kg dry coal. Because of difficulties in effectively separating solids from the product stream, considerable variation in the feed stream occurred. Although the coal feed rate was nearly constant, the amount of recycle solvent varied which resulted in wide variations of resid, unconverted coal and mineral matter in the feed stream. Unfortunately, steady state was not achieved in any of the four conditions that were run. Earlier it was reported that Ni- Mo catalyst appeared to give the best results based upon speculative steady- state yields that were developed.
Date: September 1, 1997
Partner: UNT Libraries Government Documents Department

Highly Dispersed Pseudo-Homogeneous and Heterogeneous Catalysts Synthesized via Inverse Micelle Solutions for the Liquefaction of Coal

Description: The mission of this project was to use inverse micelle solutions to synthesize nanometer sized metal particles and test the particles as catalysts in the liquefaction of coal and other related reactions. The initial focus of the project was the synthesis of iron based materials in pseudo-homogeneous form. The frost three chapters discuss the synthesis, characterization, and catalyst testing in coal liquefaction and model coal liquefaction reactions of iron based pseudo-homogeneous materials. Later, we became interested in highly dispersed catalysts for coprocessing of coal and plastic waste. Bifunctional catalysts . to hydrogenate the coal and depolymerize the plastic waste are ideal. We began studying, based on our previously devised synthesis strategies, the synthesis of heterogeneous catalysts with a bifunctional nature. In chapter 4, we discuss the fundamental principles in heterogeneous catalysis synthesis with inverse micelle solutions. In chapter 5, we extend the synthesis of chapter 4 to practical systems and use the materials in catalyst testing. Finally in chapter 6, we return to iron and coal liquefaction now studied with the heterogeneous catalysts.
Date: January 5, 1999
Creator: Hampden-Smith, M.; Kawola, J.S.; Martino, A.; Sault, A.G. & Yamanaka, S.A.
Partner: UNT Libraries Government Documents Department

STUDY OF SOLVENT AND CATALYST INTERACTIONS IN DIRECT COAL LIQUEFACTION

Description: In our previous direct coal liquefaction work using the Short Contact Time Batch Reactor (SCTBR) we have had recovery of product of approximately 75 to 85% due to hold up of the reaction mixture in the preheater, precooler and also in the blow case. This has forced us to determine conversion by use of aliquots and using an ash balance. This has worked out quite well when we were running coal liquefaction reactions without catalyst or were using small amounts of soluble catalyst which did not leave significant amounts of mineral matter in the product. Now however, we are interested in running catalyzed liquefactions with solid and often supported catalysts which contribute significant amounts of mineral matter to the reaction system, thereby reducing the precision of the conversion determination. It therefore has been important to develop a method of determining conversion by other means. To do this, we have redesigned the reactor system to increase the recovery by reducing the hold up of material in the system. This was done by redesigning the blow case so there is little or no bypassing of the compressed gas used to drive the reaction mixture into the reactor, by changing the condenser system so that there is less hold up of material there, and to reduce the length of the tubing in the preheater and precooler. With these changes, we have been able to increase our recovery to over 90 to 95%. This should permit a more accurate determination of conversion by product material balance provided one determines the amount of tetralin solvent in the recovered liquid product and the solids content in that product. The solids content is determined by filtration and weighing of the insoluble material. For the tetralin content, a gas chromatographic method on the liquid portion of the reaction ...
Date: April 1, 1998
Partner: UNT Libraries Government Documents Department

Overview of catalyst testing and coprocessing studies at Sandia National Laboratories

Description: Prior to the initiation of Sandia`s fine particle size catalyst testing project, it was not feasible to compare the activities of the many direct coal liquefaction catalysts developed in various laboratories. This was due to the wide variety of testing methods used by the different catalyst developers. Sandia developed a procedure that uses a bituminous coal (DECS-17 Blind Canyon coal), phenathrene as the reaction solvent, and a factorial experimental design with three variables: temperature, time, and catalyst loading. Numerous catalysts have been evaluated. Pacific Northwest National Laboratories` (PNNL) 6-line ferrihydrite catalyst is the most active among the particulate catalysts. West Virginia University`s (WVU) iron catalyst impregnated on Blind Canyon coal is the best iron catalyst evaluated to date. Because this catalyst was prepared by impregnation, which involves several preparation steps, it cannot be directly compared to particulate catalysts. In an effort to enable this comparison, WVU produced a particulate iron catalyst that has been tested at Sandia. In addition, Sandia has also evaluated several of Argonne National Laboratory`s molybdenum and iron catalysts that were impregnated on Wyodak subbituminous coal from the Argonne Premium Coal Sample Program. Current activities are focused on developing capabilities for performing coprocessing experiments to support FETC`s coprocessing thrust and a new project aimed at helping Puerto Rico solve its waste disposal problems.
Date: October 1, 1997
Creator: Stohl, F.V.; Goodnow, D.C.; Diegert, K.V. & Andujar, L.
Partner: UNT Libraries Government Documents Department

EXPLORATORY RESEARCH ON NOVEL COAL LIQUEFACTION CONCEPT

Description: All first-stage experimental tests were completed for Task 4 (and the Contract). The first-stage one-liter autoclave tests that were made were duplicates of Run 41-LA. The conditions used were chosen last quarter to reduce the cost of the first-stage of the process from those used at the conclusion of Task 3. Filtration and second-stage tests were made using the products of the first-stage tests. Post-second-stage filtration, tested as an alternative to interstage (pre-second- stage) filtration, resulted in low filtration rates. Different catalyst loadings and type and residence time for second-stage hydrotreating were explored. Longer residence times did not result in significantly more resid conversion. Higher catalyst loadings were more effective in converting the resid at the same residence time. The material and elemental balances for the first-stage were completed. The material and elemental balances for the second-stage were initiated.
Date: June 30, 1998
Partner: UNT Libraries Government Documents Department

DIRECT LIQUEFACTION PROOF OF CONCEPT

Description: The eighth bench scale test of POC program, Run PB-08, was successfully completed from August 8 to August 26, 1997. A total of five operating conditions were tested aiming at evaluating the reactivity of different pyrolysis oils in liquefaction of a Wyoming sub-bituminous coal (Black Thunder coal). For the first time, water soluble promoters were incorporated into the iron-based GelCat to improve the dispersion of the promoter metals in the feed blend. The concentration of the active metals, Mo and Fe, was 100 and 1000 ppm of moisture-free coal, respectively. Black Thunder coal used in this run was the same batch as tested in HTI�s Run POC-02. Similar to Runs PB-01 through 7, this run employed two back mixed slurry reactors, an interstage gas/slurry separator and a direct-coupled hydrotreater. In addition to the hot vapor from the second stage separator, the first stage separator overhead liquid was also fed to the hydrotreater, which was packed with Criterion C-411 hydrotreating catalyst. Pyrolysis oil was produced off-line from a pyrolysis unit acquired from University of Wyoming. Solids rejection was achieved by purging out pressure filter solid. The recycle solvents consisted of O-6 separator bottoms and pressure filter liquid (PFL). The Run PB-08 proceeded very smoothly without any interruptions. Coal conversion consistently above 90W% was achieved. High resid conversion and distillate yield have been obtained from co-processing of coal and 343&deg;C+ (650&deg;F+) pyrolysis oil. Light gas (C<sub>1</sub>-C<sub>3</sub> ) yield was minimized and hydrogen consumption was reduced due to the introduction of pyrolysis oil, compared with conventional coal-derived solvent. Catalytic activity was improved by incorporating a promoter metal into the iron-based GelCat. It seemed that lowering the first stage temperature to 435&deg;C might increase the hydrogenation function of the promoter metal. In comparison with previous coal-waste coprocessing run (PB-06), significant improvements in the process ...
Date: September 1, 1998
Partner: UNT Libraries Government Documents Department

Exploratory Research on Novel Coal Liquefaction Concept

Description: Task 3 experimental tests were concluded this quarter. Second-stage testing of first-stage distilled filtrates and of a Wilsonville resid from Run 263 were completed. The first-stage filtrates were found to have higher reactivity than the Wilsonville material. Task 4 experimental testing was initiated. First-stage microautoclave tests were made at reduced catalyst loading and reduced solvent to coal ratio without negatively affecting coal conversion. Lower severity second-stage catalytic upgrading tests were begun. The single-pass resid conversion obtained in the first completed second-stage test was high (67-69 %).
Date: December 12, 1997
Creator: Winschel, R. A. & Brandes, S. D.
Partner: UNT Libraries Government Documents Department

A Characterization and Evaluation of Coal Liquefaction Process Streams The Kinetics of Coal Liquefaction Distillation Resid Conversion

Description: Under subcontract from CONSOL Inc. (DOE Contract N o. DE- AC22- 94PC93054), the University of Delaware studied the mechanism and kinetics of coal liquefaction resid conversion. Th e program at Delaware was conducted be tween August 15, 1994, and April 30, 1997. It consisted of two primary tasks. The first task was to develop an empirical test to measure the reactivit y toward hydrocracking of coal- derived distillation resids. The second task was to formulate a computer model to represent the structure of the resids and a kinetic and mechanistic model of resid reactivity based on the structural representations. An Introduction and Summary of th e project authored by CONSOL and a report of the program findings authored by the University of Delaware researchers are presented here. INTRODUCTION Resid hydrocracking is a key reaction of modern (i. e., distillate- producing) coal liquefactio n processes. Coals are readily converted to resid a nd lighter products in the liquefaction process. The resid is combined with fr esh coal in a ratio often greater than 1: 1, and some vacuum gas oil and is recycled to be further converted. Understanding the chemistry of resids and resi d reactivity is important to improve direct liquefaction process design and to achieve economi c objectives for direct coal liquefaction. Computational models that predict resid conversion from the chemical characteristics of the resids and reaction conditions would be a cost- efficient way to explore process variables. Implementation of such models could aid in the design an d operation of liquefaction facilities.
Date: June 4, 1998
Creator: D.Campbell; Nichols, D.G.; Pazuchanics, D.J.; H.Huang; M.T.Klein; Winschel, R.A. et al.
Partner: UNT Libraries Government Documents Department

Slurry Phase Iron Catalysts for Indirect Coal Liquefaction

Description: This report describes research conducted to support the DOE program in indirect coal liquefaction. Specifically, we have studied the attrition behavior of Iron Fischer-Tropsch catalysts, their interaction with the silica binder and the evolution of iron phases in a synthesis gas conversion process. The results provide significant insight into factors that should be considered in the design of catalysts for the conversion of coal-derived synthesis gas into liquid fuels.
Date: September 10, 1998
Creator: Datye, Abhaya K.
Partner: UNT Libraries Government Documents Department

A Characterization and Evaluation of Coal Liquefaction Process Streams

Description: CONSOL characterized 38 process strea m samples from HTI Run PB- 04, in which Black Thunder Mine Coal, Hondo vacuum resid, autom obile shredder residue (ASR), and virgin plastics were used as liquefaction feedstocks with dispersed catalyst. A paper on kinetic modeling of resid reactivity was presented at the DOE Coal Lique -faction and Solid Fuels Contractors Review Conference, September 3- 4, 1997, i n Pittsburgh, PA. The paper, "The Reactivity of Direct Coal Liquefaction Resids", i s appended (Appendix 1). Three papers on characterization of samples from coal/ resid/ waste p lastics co- liquefaction were presented or submitted for presen tation at conferences. Because of their similarity, only one of the papers is appended to this report. The paper, "Characterization o f Process Samples From Co- Liquefaction of Coal and Waste Polymers", (Appendix 2) was presented at the DOE Coal Liquefaction and Solid Fuels C ontractors Review Conference, September 3- 4, 1997, in Pittsburgh, PA. The paper, "Characterization of Process Stream Samples From Bench- Scale Co -Liquefaction Runs That Utilized Waste Polymers as Feedstocks" was presented at the 214th National Meeting of the Ameri can Chemical Society, September 7- 11, 1997, in Las Vegas, NV. The paper, "Characterization of Process Oils from Coal/ Waste Co- Liquefaction" wa s submitted for presentation at the 14th Japan/ U. S. Joint Technical Meeting on Coa l Liquefaction and Materials for Coal Liquefaction on October 28, 1997, in Tokyo, Japan. A joint Burns and Roe Services Corp. and CONSOL pap er on crude oil assays of product oils from HTI Run PB- 03 was presented at the DOE Coal Liquefaction and Solid Fuel s Contractors Review Conference, September 3- 4, 1997, in Pittsburgh, PA. The paper , "Characterization of Liquid Products from All- Slurry Mode Liquefaction", is appende d (Appendix 3).
Date: June 9, 1998
Creator: Robbins, G. A.; Winschel, R. A. & Brandes, S. D.
Partner: UNT Libraries Government Documents Department

Fundamental Kinetics of Supercritical Coal Liquefaction: Effect of Catalysts and Hydrogen-Donor Solvents

Description: This is the quarterly report on our recent progress toward the overall objective to understand the supercritical fluid extraction of hydrocarbons from coal. Our strategy is to simulate coal as a high molecular-weight polymeric material by studying the degradation of polymers under various conditions. The hypothesis we are testing is that degradation of such macromolecules is applicable to the decomposition (depolymerization) of the coal network. Polymer degradation and coal liquefaction are influenced strongly by the solvent in the reaction. This motivated our investigation of the effect of hydrogen donor solvents on polymer degradation. In particular, we obtained new experimental data to show how a hydrogen donor, 6-hydroxy tetralin, influences the degradation rate of polystyrene. We also developed a detailed radical mechanism for hydrogen donation based on the Rice-Herzfeld chain reaction concept with the elementary steps of initiation, depropagation, hydrogen abstraction, and termination. Expressions for the degradation rate parameters were obtained by applying continuous distribution kinetics to the MWD of the reacting polymer. The theory explains the different influences of the hydrogen donor solvent on the degradation rate coefficients for different polymers. Though developed for the degradation of polymers, the mechanism and the theory are potentially applicable for chain scission and addition reactions among distributions of paraffins, olefins, and radicals of all chain lengths. The concepts can, in principle, be extended to examine the effect of hydrogen donors on coal liquefaction and on the complex mixture of liquefaction compounds. Based on this work, a research paper titled �Effect of Hydrogen Donors on Polymer Degradation,� has been submitted for publication. Our research paper entitled, �Molecular weight effect on the dynamics of polystyrene degradation,� has been accepted for publication by the journal, Industrial and Engineering Chemistry Research.
Date: April 16, 1997
Creator: McCoy, Ben J.; Madras, Girodhar; Smith, J. M. & Kodera, Yoichi
Partner: UNT Libraries Government Documents Department

Advanced Direct Liquefaction Concepts for PETC Generic Units - Phase II

Description: Reported here are the results of Laboratory and Bench-Scale experiments and supporting technical and economic assessments conducted under DOE Contract No. DE-AC22-91PC9104O during the period October 1, 1996 to December 31, 1996. This contract is with the University of Kentucky Research Foundation which supports work with the University of Kentucky Center for Applied Energy Research, CONSOI+ Inc., LDP Associates, and Hydrocarbon Technologies, Inc. This work invoives the introduction into the basic two stage liquefaction process several novel concepts which include dispersed lower-cost catalysts, coal cleaning by oil agglomeration, and distillate hydrotreating and dewaxing.
Date: February 1, 1997
Partner: UNT Libraries Government Documents Department

Refining and End Use Study of Coal Liquids

Description: This report summarizes revisions to the design basis for the linear programing refining model that is being used in the Refining and End Use Study of Coal Liquids. This revision primarily reflects the addition of data for the upgrading of direct coal liquids.
Date: October 1, 1997
Partner: UNT Libraries Government Documents Department

Laboratory Studies for Separation of Solids from Synthoil Gross Product : Parts 1 and 2

Description: PART 1. A variety of surfactants and agglomerating agents have been added to coal-liquefaction product (from the SYNTHOIL process) to determine the effectiveness of these agents in decreasing the viscosity of the product or inducing agglomeration of suspended solids in the product (and consequently facilitating the removal of solids from the product). More than two dozen additives were tested; however, only two of the additives caused a small reduction in the viscosity of the coal-liquefaction product. PART 2. A variety of organic solvents have been added to coal-liquefaction product (from the SYNTHOIL process) to determine the effectiveness in promoting the precipitation of suspended solids in the product. High-temperature settling of the product in the absence of foreign solvent does not appear to be a promising mechanism for solids removal from this product. However, the promoter-solvent de-ashing scheme has been demonstrated to be a potentially attractive solids-liquid separation method, and kerosene has been found to be an effective promoter solvent for the SYNTHOIL gross product.
Date: November 1976
Creator: Huang, H. & Fischer, J.
Partner: UNT Libraries Government Documents Department