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Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

Description: An investigation aimed at devising a procedure for preparing alkyl-or aryl-capped iron sulfide particles continues. An initial attempt to prepare fine-particle, aryl-capped iron sulfides (S-31) involved the competitive reaction of thiophenol (PhSH) and sodium sulfide (Na{sub 2}S) with Fe(II). However, SEM examination of the particles formed by this procedure indicated that no size control had been attained. It was thought that the phenyl group of thiophenol was not bulky enough to prevent thiolate bridging and consequent particle size growth of the metal sulfide. So the bulkier thiol 1-adamantanethiol was synthesized and used in synthesis S-33 in the next attempt to prepare fine-particle, capped iron sulfides.
Date: May 22, 1992
Creator: Klein, M.T.
Partner: UNT Libraries Government Documents Department

Design of a high activity and selectivity alcohol catalyst

Description: As specified in our original DOE grant proposal, the objective of this research is to design a new alumina-supported bimetallic catalyst for the selective hydrogenation of carbon monoxide to produce methanol and higher alcohols. A key feature of our research program is our intention to rationally design this catalyst based upon fundamental information about the structure, composition and reactivity of preliminary catalysts synthesized throughout the course of this work. During our first year, we have put in place many of the tools needed to synthesize and characterize our catalyst samples. Experimentation has focused on both the synthesis of catalysts designed for high oxygenate activity and the suppression of the secondary dehydration of methanol to dimethyl ether on both native gamma-alumina and a bimetallic catalyst supported on gamma-alumina. 2 refs., 1 tab.
Date: September 27, 1991
Creator: Foley, H.C. & Mills, G.A.
Partner: UNT Libraries Government Documents Department

Short contact time direct coal liquefaction using a novel batch reactor. Quarterly report, May 15, 1995--September 15, 1995

Description: The objective of this research is to optimize the design and operation of the bench scale batch reactor for coal liquefaction at short contact times (0.01 to 10 minutes or longer). Additional objectives are to study the kinetics of direct coal liquefaction, particularly at short reaction times, and to investigate the role of the organic oxygen components of coal and their reaction pathways during liquefaction. This quarterly report covers the status of progress toward these objectives. 3 refs., 14 figs., 2 tabs.
Date: October 5, 1995
Creator: Klein, M.T.; Calkins, W.H. & Huang, He
Partner: UNT Libraries Government Documents Department

Short contact time direct coal liquefaction using a novel batch reactor. Quarterly progress report, January 1--May 15, 1995

Description: The objective of this research is to optimize the design and operation of the bench scale batch reactor for coal liquefaction at short contact times (0.01 to 10 minutes or longer). Additional objectives are to study the kinetics of direct coal liquefaction particularly at short reaction times, and to investigate the role of the organic oxygen components of coal and their reaction pathways during liquefaction. Experimental progress is reported for uncatalyzed liquefactions, catalyzed liquefactions, liquefaction in the presence of solvents other than tetralin, and kinetics of gas formation during coal liquefaction. Analytical methods were developed for the determination of the boiling range of coal liquids by thermogravimetric analysis and the determination of phenolic hydroxyl in coal, coal liquids, and coal residues.
Date: May 31, 1995
Creator: Klein, M.T. & Calkins, W.H.
Partner: UNT Libraries Government Documents Department

Low temperature SO sub 2 removal with solid sorbents in a Circulating Fluidized Bed Absorber

Description: The construction of a bench-scale Circulating Fluidized Bed Absorber (CFBA) unit has been completed, and system calibrations have already been performed. In addition, as a novel method injecting water into CFBA, a toroidal-shaped nozzle was designed and installed in a bed reactor to increase the wetting efficiency of solid sorbents. The experimental set up for low temperature SO{sub 2} removal consists of a bed reactor of 3 inches in diameter and 10 feet in length, two high efficiency cyclones for gas/solid separation, sorbent injection and recycling system, water injection system, gas heating system, and gas flow, concentration, temperature and pressure monitoring system. The toroidal shaped nozzle located at the base of the bed has 12 holes placed symmetrically around the ring at an angle of 50{degrees} with the horizontal, and is made of copper tube.
Date: January 1, 1992
Creator: Lee, S.K. & Keener, T.C.
Partner: UNT Libraries Government Documents Department

Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

Description: The first task in our proposed study of catalysts for coal liquefaction was to prepare ultrafine dispersed metal sulfide particles by reactive precipitation from solutions of appropriate metal precursors. At this point, equipment to allow us to prepare these air-sensitive materials in an anaerobic environment has been acquired and assembled. Initial experiments aimed at synthesizing iron sulfide particles have been initiated. As part of the investigation of short contact time catalytic coal liquefaction, initial efforts focused on the noncatalytic pyrolysis reactions of coal and a model compound, Dibenzyl ether (DBE). Two different reactor configurations were examined; catalytic experiments are planned for the coming month.
Date: February 22, 1991
Creator: Klein, M.T.
Partner: UNT Libraries Government Documents Department

Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

Description: A series of carbonyl-based homogeneous catalyst precursors has been prepared. These species include: Fe(CO){sub 4}PPh{sub 3}, Fe(CO){sub 3}(PPh{sub 3}){sub 2}, Fe(CO){sub 2}(PPh{sub 3}){sub 2}CS{sub 2}, S{sub 2}Fe{sub 2}(CO){sub 6}, S{sub 2}Fe{sub 3}(CO){sub 9}. Fe(CO){sub 4}PPh{sub 3} was prepared by a combined photochemical and thermal route from triphenylphosphine (PPh{sub 3}) in iron pentacarbonyl (Fe(CO){sub 5}). This preparation procedure, which is selective to the monosubstituted product, is outlined herein. Currently these compounds are being tested as catalysts/catalyst precursors with coal or model compounds in the tubing bomb reactors to provide information relating catalytic activity to catalyst structure and properties. (VC)
Date: September 11, 1991
Creator: Klein, M.T.
Partner: UNT Libraries Government Documents Department

Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

Description: The purpose of this work is to investigate the kinetics-assisted design, synthesis and characterization of fme-pardcle, unsupported catalysts for coal liquefaction. The goal is to develop a fundamental understanding of coal catalysis and catalysts that will, in turn, allow for the specification of a novel optimal catalyst for coal liquefaction.
Date: December 30, 1991
Creator: Klein, M.T.
Partner: UNT Libraries Government Documents Department