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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

Solvent tailoring in coal liquefaction. Quarterly report, April-June 1984

Description: Although the numerous functions of the solvent during liquefaction are not completely understood, the provision for (and the maintenance of) an effective process solvent is necessary for effective coal liquefaction. In this project, the function of the process solvent regarding vapor-liquid equilibrium, hydrogen donation, and catalyst activity has been explored. In previously reported work, a number of donor compounds were evaluated for their relative efficiency in converting coal to cresol solubles. Attempts to correlate the relative efficiency of the various donor compounds were made on the basis of thermodynamic stability and structural features of the molecules. Currently, work is underway with selected donor compounds to determine if the chemical nature of the compound influences the product distribution obtained during coal liquefaction as well as affecting the amount of conversion obtained. The product distribution, which is being used to evaluate the liquefaction products, is based upon extraction of the products into different solvents. The products are divided into oil, pentane soluble material; asphaltenes, pentane insoluble, benzene soluble material; preasphaltenes, benzene insoluble, methylene chloride/methanol soluble material; and insoluble organic matter, methylene chloride/methanol insoluble material. The effectiveness of the hydrogen donor solvent will be measured by the amount of higher quality material (oil and asphaltenes) obtained as well as by the amount of coal converted.
Date: July 1, 1984
Creator: Tarrer, A.R.; Curtis, C.W.; Guin, J.A. & Williams, D.C.
Partner: UNT Libraries Government Documents Department

Production of Gasoline and Diesel from Biomass via Fast Pyrolysis, Hydrotreating and Hydrocracking: 2012 State of Technology and Projections to 2017

Description: This report summarizes the economic impact of the work performed at PNNL during FY12 to improve fast pyrolysis oil upgrading via hydrotreating. A comparison is made between the projected economic outcome and the actual results based on experimental data. Sustainability metrics are also included.
Date: August 27, 2013
Creator: Jones, Susanne B. & Snowden-Swan, Lesley J.
Partner: UNT Libraries Government Documents Department

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

Report on the Investigation of the Fire at the Liquefaction, Storage, and Regasification Plant of the East Ohio Gas Co., Cleveland Ohio, October 20, 1944

Description: Report issued by the Bureau of Mines over investigations conducted on the 1944 fire at the East Ohio Gas Company. Descriptions of the plant, and construction of the gas tanks are listed. A detailed description of the disaster, and its aftermath are also presented. This report includes tables, maps, illustrations, and photographs.
Date: February 1946
Creator: Elliott, M. A.; Seibel, C. W.; Brown, F. W.; Artz, R. T. & Berger, L. B.
Partner: UNT Libraries Government Documents Department

Power recovery system for coal-liquefaction process. [Patent application]

Description: Method and apparatus for minimizing energy required to inject reactant such as coal-oil slurry into a reaction vessel, using high pressure effluent from the latter to displace the reactant from a containment vessel into the reaction vessel with assistance of low pressure pump. Effluent is degassed in the containment vessel, and a heel of the degassed effluent is maintained between incoming effluent and reactant in the containment vessel.
Date: April 24, 1981
Creator: Horton, J.R.
Partner: UNT Libraries Government Documents Department

Microbial recovery of metals from spent coal liquefaction catalysts. Quarterly report, October 1993--December 1993

Description: The project objectives outlined in the previous reports involved defining conditions and cultures best suited to achieve the most effective metal release from spent coal liquefaction catalysts by microbial processes. The continuity of the research program was maintained during the period of principal investigator replacement. This transition period allowed the project data to be reviewed and research plans were formulated to gain new insights into the mechanisms involved in metals release. Various microbiological and physiochemical parameters which may be important in microbial release of metals from spent coal liquefaction catalysts continue to be investigated so that this technology can be optimized. Mo release from spent coal liquefaction catalysts has been shown to be dependent upon many parameters, but release is dominated by microbial growth. The microbial Mo release is a rapid process requiring less than one week for 90% of the releasable Mo to be solubilized from whole washed (THF) catalyst. It could be expected that the rates would be even greater with crushed catalyst. Efforts are now centering on optimizing the parameters that stimulate microbial growth and action.
Date: December 31, 1993
Creator: Sandbeck, K. A. & Joffe, P. M.
Partner: UNT Libraries Government Documents Department

Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, July--September 1993

Description: In this quarter, progress has been made in the following two aspects: (1) spectroscopic and chemical reaction studies on the effects of drying and mild oxidation of a Wyodak subbituminous coal on its structure and pretreatment/liquefaction at 350{degrees}C; and (2) effects of dispersed catalyst and solvent on conversion and structural changes of a North Dakota lignite. Drying and oxidation of Wyodak subbituminous coal at 100-150{degrees}C have been shown to have significant effects on its structure and on its catalytic and non-catalytic low-severity liquefaction at 350{degrees}C for 30 min under 6.9 MPa H{sub 2}. Spectroscopic analyses using solid-state {sup 13}C NMR, Pyrolysis-GC-MS, and FT-IR revealed that oxidative drying at 100-150{degrees}C causes the transformation of phenolics and catechol into other related structures (presumably via condensation) and high-severity air drying at 150{degrees}C for 20 h leads to disappearance of catechol-like structure. Increasing air drying time or temperature increases oxidation to form more oxygen functional groups at the expense of aliphatic carbons. Such a clearly negative impact of severe oxidation is considered to arise from significantly increased oxygen functionality which enhances the cross-link formation in the early stage of coal liquefaction. Physical, chemical, and surface physicochemical aspects of drying and oxidation and the role of water are also discussed. A North Dakota lignite (DECS-1) coal was studied for its behaviors in non-catalytic and catalytic liquefaction. Reactions were carried out at temperatures between 250 and 450{degrees}C. Regardless the reaction solvents and the catalyst being used, the optimum temperature was found to be 400{degrees}C. The donor solvent has a significant effect over the conversion especially at temperatures higher than 350{degrees}C.
Date: January 1, 1994
Creator: Song, C.; Saini, A. K.; Huang, L.; Schobert, H. H. & Hatcher, P. G.
Partner: UNT Libraries Government Documents Department

Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Technical progress report, October 1993--December 1993

Description: In this quarter, progress has been made in the following two aspects: The influences of temperature, dispersed Mo catalyst, and solvent on the liquefaction conversion and composition of products from low-rank coals; and the hydrous pyrolysis of a lignite and spectroscopic characterization of its structural transformation during the hydrous pyrolysis. The analytical work described in this quarter also represents molecular-level characterization of products. The purpose of the first part of the work described in this quarter is to study the influences of temperature, solvent and dispersed Mo catalyst on the liquefaction conversion and chemical composition of the products. Many specialty chemicals, including one- to four-ring aromatics, could potentially be produced by liquefying coal. To achieve this goal, not only a high coal conversion but also a desirable product distribution is necessary. Therefore, it is of great importance to understand the structural changes of the coal during reaction and to investigate the conditions under which the aliphatics or aromatics can be removed from the macromolecular structure of coal. This quarterly report also describes the hydrous pyrolysis of Potapsco lignite and spectroscopic characterization of its structural transformation during the hydrous pyrolysis. This work has some implications both on the structural changes of low-rank coals during pretreatment and on the geochemical reactions during coalification stage. Vitrinite, a major component of most coals, is derived from degraded wood in ancient peat swamps. Organic geochemical studies conducted on a series of coalified wood samples derived mostly from gymnosperms have allowed the development of a chemical reaction series to characterize the major coalification reactions which lignin, the major coal-producing component of wood, undergoes.
Date: February 1, 1994
Creator: Song, C.; Huang, L.; Wenzel, K. A.; Hatcher, P. G. & Schobert, H. H.
Partner: UNT Libraries Government Documents Department

Bench-scale demonstration of biological production of ethanol from coal synthesis gas. Quarterly report, October 1, 1993--December 31, 1993

Description: This project describes a new approach to coal liquefaction, the biological conversion of coal synthesis gas into a liquid fuel, ethanol. A new bacterium, Clostridium Ijungdahlii, strain PETC, has been discovered and developed for this conversion, which also produces acetate as a by-product. Based upon the results of an exhaustive literature search and experimental data collected in the ERI laboratories, secondary and/or branched alcohols have been selected for ethanol extraction from the fermentation broth. 2,6 Methyl 4-heptanol has a measured distribution coefficient of 0.44 and a separation factor of 47. Methods to improve the results from extraction by removing water prior to distillation are under consideration. Several runs were performed in the two-stage CSTR system with Clostridium Ijungdahlii, strain PETC, with and without cell recycle between stages. Reduced gas flow rate, trypticase limitation and ammonia limitation as methods of maximizing ethanol production were the focus of the studies. With ammonia limitation, the ethanol:acetate product ratio reached 4.0.
Date: December 31, 1993
Partner: UNT Libraries Government Documents Department

Fundamental studies of coal liquefaction. Quarterly report No. 8, July 1, 1993--October 1, 1993

Description: In the last report the effects of water, tetralin, and argon were discussed as media during the heating of Illinois No. 6 coal. In studies in which the temperature was ramped from ambient to 460{degrees}C at 30{degrees}C/min particles were observed to shrink in the case of both water and tetralin, and first swell and then collapse back to particles with their starting shapes in the case of argon. The result with tetralin was expected, but that for water was not. Similarly, the results in argon were not in accord with some models of coal pyrolysis which suggest that coals fully liquefy when heated (Solomon, et al.). The work described here includes discussion of additional work with Illinois No. 6 coal with argon and water, and new work with n-undecane as medium.
Date: October 14, 1993
Creator: Ross, D. S.
Partner: UNT Libraries Government Documents Department

Coal liquefaction process streams characterization and evaluation. Gold tube carbonization and reflectance microscopy

Description: This study demonstrated the use of the gold tube carbonization technique and reflectance microscopy analysis for the examination of process-derived materials from direct coal liquefaction. The carbonization technique, which was applied to coal liquefaction distillation resids, yields information on the amounts of gas plus distillate, pyridine-soluble resid, and pyridine-insoluble material formed when a coal liquid sample is heated to 450{degree}C for one hour at 5000 psi in an inert atmosphere. The pyridine-insolubles then are examined by reflectance microscopy to determine the type, amount, and optical texture of isotropic and anisotropic carbon formed upon carbonization. Further development of these analytical methods as process development tools may be justified on the basis of these results.
Date: December 1, 1991
Creator: Mitchell, G.; Davis, A.; Burke, F. P.; Winschel, R. A. & Brandes, S. D.
Partner: UNT Libraries Government Documents Department

Coal liquefaction process streams characterization and evaluation. Quarterly technical progress report, July 1--September 30, 1992

Description: This is the twelfth Quarterly Technical Progress Report under DOE Contract DE-AC22-89PC89883. Major topics reported are: Summaries of the final reports produced by Lehigh University, West Virginia University, and Vander Sande Associates under the Participants Program are presented. Analytical data produced by CONSOL are provided in Appendix I for all samples employed in the Participants Program and issued with the samples to research groups in the Participants Program. A paper was presented at the 1992 US Department of Energy Pittsburgh Energy Technology Center Liquefaction Contractors` Review Conference, held in Pittsburgh September 23--24, 1992, entitled ``The Chemical Nature of Coal Liquid Resids and the Implications for Process Development``. It appears as Appendix 2 in this report.
Date: November 1, 1992
Creator: Brandes, S. D.; Winschel, R. A. & Burke, F. P.
Partner: UNT Libraries Government Documents Department

Initial study of coal pretreatment and coprocessing

Description: This document describes research performed in accordance with task 3.3.1 in the 1989--1990 annual research plan under cooperative agreement number DE-FC21-86MC11076. The objective of this study was to determine the potential for enhancing liquid yields by integrating coal pretreatment and coprocessing technologies. The process tested involved pretreatment of coal to a very low moisture content and partial decarboxylation in an inclined fluidized-bed reactor by contact with hot C0{sub 2} or a C0{sub 2} and superheated steam mixture. The pretreated coal was then coprocessed with a heavy, coal-derived oil in a 2-inch screw pyrolysis reactor to produce dried coal with a higher calorific value and an upgraded oil. Six pretreatment tests and seven coprocessing tests were conducted independently with two separate systems being utilized: one system for the pretreatment tests and the other system for the coprocessing tests. The test program included evaluating alternative pretreatment gases, temperatures, and residence times in combination with different coprocessing temperatures and residence times. Pretreatment and coprocessing studies were performed on Herrin Results of the integrated pretreatment and coprocessing operations were evaluated and compared with the coprocessing of raw coal. The results indicate that a solid product is formed with a higher calorific content than the starting coal and that an upgraded oil is generated.
Date: September 1, 1991
Creator: Vaillancourt, M.; Turner, T. F. & Fahy, L. J.
Partner: UNT Libraries Government Documents Department

Optimization of reactor configuration in coal liquefaction. Ninth quarterly report, 1 October 1993--31 December 1993

Description: This quarterly report covers the activities of Optimization of Reactor Configuration in Coal Liquefaction during the Period October 1 to December 31, 1993, at Hydrocarbon Research, Inc. in Lawrenceville and Princeton, New Jersey. This DOE Contract Period was from October 1, 1991 to September 30, 1993 and has recently been extended to March 31, 1994. The overall objective of this program is to achieve a new approach to liquefaction that generates an all distillate product slate at a reduced cost of about $25 per barrel of crude oil equivalent. This quarterly report covers work on laboratory Support, Laboratory-scale Studies and Project Management.
Date: January 1, 1994
Creator: Lee, L. K.; Pradhan, V. R.; Johanson, E. S.; Comolli, A. G. & Stalzer, R. H.
Partner: UNT Libraries Government Documents Department

Advanced liquefaction using coal swelling and catalyst dispersion techniques. Report No. Q-01, Quarterly technical progress report, October--December 1991

Description: Research in this project centers upon developing a new approach to the direct liquefaction of coal to produce an all-distillate product slate at a sizable cost reduction over current technology. The approach integrates all aspects of the coal liquefaction process including coal selection, pretreatment, coal swelling with catalyst impregnation, coal liquefaction experimentation, product recovery with characterization, alternate bottoms processing, and a technical assessment including an economic evaluation. Work has centered upon obtaining bulk samples of feedstocks for the project, up-dating the background literature, and preparing and testing a computer program to perform material balance calculations for the continuous flow liquefaction unit.
Date: December 31, 1991
Creator: Curtis, C. W.; Gutterman, C. & Chander, S.
Partner: UNT Libraries Government Documents Department

Studies of coupled chemical and catalytic coal conversion methods. Eleventh quarterly report, April--June 1990

Description: The objective of our work is coal liquefaction under relatively mild conditions. Our attempts were to depolymerize the coal macromolecule to smaller fragments which could be more easily solubilized in conventional organic solvents. During the last few months we have been working on nonreductive C-alkylation procedures. The effectiveness of the newly introduced alkyl groups for the disruption of intemolecular hydrogen bonds and pi-pi interactions between the aromatic sheets in the coal mdcromolecule had been recognized. During the present quarter, a new approach for the depolymerization of the coal macromolecule was tried. This was aimed towards carbon-carbon bond cleavage in the presence of strong bases. Such bond cleavage reactions are well known with the alkali metals. Electron transfer reactions take place from the metals to the aromatic nuclei resulting in the formation of anion radicals (or dianions) which subsequently undergo carbon-carbon bond cleavage. In our work, instead of using the alkali metals, we have used bases to cleave the carbon-carbon bonds by base catalyzed hydrocarbon elimination reactions.Such anionic fragmentation reactions involving strong bases are not very well established. The only discrete evidence of carbon-carbon bond cleavage with bases were obtained from some earlier works of Grovenstein.
Date: December 31, 1990
Creator: Stock, L. M.
Partner: UNT Libraries Government Documents Department

Low severity coal liquefaction promoted by cyclic olefins. Quarterly report, April--June 1992

Description: Low severity coal liquefaction allows for solubilization of coal with reduced gas make. These lower severity conditions may result in some selective bond rupture. Promotion of coal solubilization through hydrogen transfer using highly active and effective hydrogen donors is the objective of this study. The highly effective donors being tested are cyclic olefins. Representative cyclic olefins are isotetralin, which is 1,4,5,8-tetrahydronaphthalene, and 1,4,5,8,9,10-hexahydroanthracene. These compounds are hydroaromatics without aromatic rings and have been shown to be highly effective donors. The objective of the work performed in this study during this quarter was to evaluate reaction parameters for low severity liquefaction reactions using the cyclic olefin, hexahydroanthracene, and the aromatic, anthracene. These model compounds were reacted under a variety of conditions to evaluate their reactivity without coal. The reactions were performed under both thermal and catalytic conditions. Finely divided catalysts from different molybdenum precursors were used to determine their activity in promoting hydrogenation and hydrogen transfer at low severity conditions. The catalysts used were Molyvan L, sulfurized oxymolybdenum dithiocarbamate, molybdenum naphthenate, and Molyvan 822, organo molybdenum dithiocarbamate.
Date: July 27, 1992
Creator: Curtis, C. W.
Partner: UNT Libraries Government Documents Department

Thermolysis of silica-immobilized 1-(4{prime}-hydroxyphenyl)-2-phenylethane under D{sub 2}. A hydroliquefaction model

Description: Important conclusions of this study are: Presence of D{sub 2}at 2000 psi does not alter the tendency of surface-attached radicals to rearrange. Hydrocracking is observed for hydropyrolysis of surface-attached materials. Radical D/H exchange is more efficient in the gas phase. Reaction of benzylic radicals with phenols has been documented. Phenoxyl radicals catalyze exchange between D{sub 2} and SiOH groups on silic which in turn promotes exchange at ortho and para ring positions in phenolic compounds.
Date: September 1, 1994
Creator: Guthrie, R. D.; Ramakrishnan, S.; Davis, B. H.; Britt, P. F. & Buchanan, A. C. III
Partner: UNT Libraries Government Documents Department

Highly dispresed catalysts for coal liquefaction. Quarterly report No. 10, November 23, 1993--February 22, 1994

Description: The objectives of this project are to study the effect of pretreatment methods on the two-stage liquefaction process. In particular, the effects of dispersed catalysts and carbon monoxide atmospheres on a coal liquefaction process. The project is divided into three technical tasks. Task 1 and 2 deal with the analyses and liquefaction experiments, respectively, whereas Task 3 deals with the economic impact of utilizing the pretreatment methods. This quarter the authors concentrated on Tasks 1 and 2, which are summarized below.
Date: April 15, 1994
Creator: Hirschon, A. S. & Wilson, R. B.
Partner: UNT Libraries Government Documents Department

Use of hydropyrolysis-MS to probe the hydrocracking of diphenylalkane linkages in the solid state

Description: Results have indicated increasing the hydrogen pressure reduces the extent of retrogressive chemistry for all the model substrates investigated. The primary pyrolytic event at high hydrogen pressure, as characterized by the evolution of benzene, toluene and ethylbenzene/styrene, occurs at virtually the same temperature for a given alkane linkage in the different substrates used. The C{sub 2} and C{sub 3} linkages investigated are cleaved at ca 50-100{degrees}C lower than their C{sub 1} counterparts. The pyrolysis of immobilized diphenylmethane appears to be largely unaffected by the co-attachment of tetralin.
Date: September 1, 1994
Creator: Brown, S. D.; Sirkecioglu, O.; Ismail, K.; Andersen, J.; Snape, C. E.; Buchanan, A. C. III et al.
Partner: UNT Libraries Government Documents Department

Separation of solids from coal liquefaction products using sonic waves

Description: Product streams containing solids are generated in both direct and indirect coal liquefaction processes. This project seeks to improve the effectiveness of coal liquefaction by novel application of sonic and ultrasonic energy to separation of solids from coal liquefaction streams.
Date: October 1, 1994
Creator: Slomka, B. J.
Partner: UNT Libraries Government Documents Department