Chemical studies on SYNTHOIL process. Sixth quarterly report, December 1, 1976--March 1, 1977. [Catalyst improvement; mineral matter effects; preheated studies; 8 refs; Co molybdate]

doi:10.2172/7109238

Title: Chemical studies on SYNTHOIL process. Sixth quarterly report, December 1, 1976--March 1, 1977. [Catalyst improvement; mineral matter effects; preheated studies; 8 refs; Co molybdate]

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Abstract

In support of the Pittsburgh Energy Research Center's SYNTHOIL Process for coal liquefaction, Sandia Laboratories has undertaken three tasks: Catalyst Improvement, Mineral Matter Effects, and Preheater Studies. In the last quarter, the catalyst improvement studies focused on the effects of nitrogen-containing compounds on the activity of presulfided cobalt molybdate catalyst pellets. Data from pulsed microreactor experiments have shown that pyridine, aniline, and pyrrole cause a decrease in the hydrodesulfurization of thiophene. In most cases these losses in activity were, to a great extent, reversible. In the mineral matter effects studies, chemical removal of pyrite and other mineral constituents has been carried out on Kentucky, West Virginia and Indiana coals. These coals were hydroliquefied in a batch autoclave. The viscosities and preasphaltene contents of the resulting liquid products were higher than those obtained from the original, untreated coals. The continuous reactor used for the preheater studies has been completed, and preliminary pressure testing has been started. The first shakedown run is expected in April.

Authors:: Holloway, P.H.; Granoff, B.; Nowak, E.J.

Publication Date:: Fri Apr 01 00:00:00 EST 1977

Research Org.:: Sandia Labs., Albuquerque, NM (USA)

OSTI Identifier:: 7109238

Report Number(s):: SAND-77-0720

DOE Contract Number:: EY-76-C-04-0789

Resource Type:: Technical Report

Country of Publication:: United States

Language:: English

Subject:: 01 COAL, LIGNITE, AND PEAT; CATALYSTS; DEACTIVATION; RESEARCH PROGRAMS; COAL; DEMINERALIZATION; DESULFURIZATION; COAL LIQUIDS; VISCOSITY; COBALT COMPOUNDS; CATALYTIC EFFECTS; MOLYBDATES; PYRITE; REMOVAL; SYNTHOIL PROCESS; THIOPHENE; ANILINE; AUTOCLAVES; COAL LIQUEFACTION; PYRIDINES; PYRROLES; AMINES; AROMATICS; AZINES; AZOLES; CARBONACEOUS MATERIALS; CHALCOGENIDES; CHEMICAL REACTIONS; ENERGY SOURCES; FOSSIL FUELS; FUELS; HETEROCYCLIC COMPOUNDS; IRON COMPOUNDS; IRON SULFIDES; LIQUEFACTION; MINERALS; MOLYBDENUM COMPOUNDS; ORES; ORGANIC COMPOUNDS; ORGANIC NITROGEN COMPOUNDS; ORGANIC SULFUR COMPOUNDS; OXYGEN COMPOUNDS; PYRITES; SEPARATION PROCESSES; SULFIDES; SULFUR COMPOUNDS; SULFUR ORES; THERMOCHEMICAL PROCESSES; TRANSITION ELEMENT COMPOUNDS; 010405* - Coal, Lignite, & Peat- Hydrogenation & Liquefaction

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                    Holloway, P.H., Granoff, B., and Nowak, E.J. Chemical studies on SYNTHOIL process. Sixth quarterly report, December 1, 1976--March 1, 1977. [Catalyst improvement; mineral matter effects; preheated studies; 8 refs; Co molybdate].  United States: N. p., 1977. 
        Web.  doi:10.2172/7109238.

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                    Holloway, P.H., Granoff, B., & Nowak, E.J. Chemical studies on SYNTHOIL process. Sixth quarterly report, December 1, 1976--March 1, 1977. [Catalyst improvement; mineral matter effects; preheated studies; 8 refs; Co molybdate].  United States.  doi:10.2172/7109238.

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                    Holloway, P.H., Granoff, B., and Nowak, E.J. Fri .  
        "Chemical studies on SYNTHOIL process. Sixth quarterly report, December 1, 1976--March 1, 1977. [Catalyst improvement; mineral matter effects; preheated studies; 8 refs; Co molybdate]".  United States.  
        doi:10.2172/7109238.  https://www.osti.gov/servlets/purl/7109238.

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@article{osti_7109238,

  title        = {Chemical studies on SYNTHOIL process. Sixth quarterly report, December 1, 1976--March 1, 1977. [Catalyst improvement; mineral matter effects; preheated studies; 8 refs; Co molybdate]},

  author       = {Holloway, P.H. and Granoff, B. and Nowak, E.J.},

  abstractNote = {In support of the Pittsburgh Energy Research Center's SYNTHOIL Process for coal liquefaction, Sandia Laboratories has undertaken three tasks: Catalyst Improvement, Mineral Matter Effects, and Preheater Studies. In the last quarter, the catalyst improvement studies focused on the effects of nitrogen-containing compounds on the activity of presulfided cobalt molybdate catalyst pellets. Data from pulsed microreactor experiments have shown that pyridine, aniline, and pyrrole cause a decrease in the hydrodesulfurization of thiophene. In most cases these losses in activity were, to a great extent, reversible. In the mineral matter effects studies, chemical removal of pyrite and other mineral constituents has been carried out on Kentucky, West Virginia and Indiana coals. These coals were hydroliquefied in a batch autoclave. The viscosities and preasphaltene contents of the resulting liquid products were higher than those obtained from the original, untreated coals. The continuous reactor used for the preheater studies has been completed, and preliminary pressure testing has been started. The first shakedown run is expected in April.},

  doi          = {10.2172/7109238},

  journal      = {},

  number       = ,

  volume       = ,

  place        = {United States},

  year         = {Fri Apr 01 00:00:00 EST 1977},

  month        = {Fri Apr 01 00:00:00 EST 1977}

}

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DOI: 10.2172/7109238

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Chemical studies on SYNTHOIL process. Fifth quarterly report, September 1--December 1, 1976. [Catalyst deactivation; mineral matter effects; preheater studies; 14 refs. ; Co--Mo]

Holloway, P.H. ; Granoff, B. ; Nowak, E.J. ; ...

In support of the Pittsburgh Energy Research Center's SYNTHOIL process for coal liquefaction, Sandia has undertaken three tasks; Catalyst Deactivation, Mineral Matter Effects, and Preheater Studies. In the last quarter, the catalyst deactivation studies continue to indicate loss of catalytic activity early in a run. Micropulse catalyst studies indicate the cracking activity of used Co-Mo catalyst is decreased more than other catalytic effects. In the mineral matter effect studies, techniques for selective demineralization of coal have been developed by controlled removal of the mineral matter from 9.95 to 1.14 percent and of the iron in the ash from 15 tomore »« less
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Holloway, P.H. ; Granoff, B. ; Nowak, E.J. ; ...

This is the first annual report of a 2-yr program of study in support of the synthoil process for coal liquefaction. The overall program consists of three tasks: Catalyst Improvement, in which the mechanisms of catalyst deactivation will be explored; Ash Effects, in which the effect of the mineral content of coals on liquefaction will be assessed in autoclave experiments; and Kinetic Studies, in which a bench-scale reactor will be set up to study the effects of process parameters on the kinetics of hydrodesulfurization and liquefaction. Progress in each task area is reported. Extensive characterization has been completed on new,more »« less
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Granoff, B. ; Baca, P.M. ; Thomas, M.G. ; ...

Mineral matter effects in coal liquefaction were studied by means of batch autoclave experiments at temperatures of 395 to 430/sup 0/C, residence times (at temperature) of 15 to 60 min and operating pressures of 1500 to 3000 psig. All experiments were carried out in creosote oil (No. 4 cut) as the solvent. High volatile bituminous coals from Kentucky, Indiana, West Virginia, Illinois and Pennsylvania were used for most of this work. The mineral contents of these coals, as determined by low temperature ashing, ranged from 24.6 to 5.2 percent; the corresponding sulfur contents ranged from 6.7 to 0.8 percent. Amore »« less
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Crynes, B.L.

Three experimental run series were conducted to assess a Synthoil liquid for hydrotreating performance. Results from one of these experiments and from another one made previously are reported. This Synthoil liquid is rather resistant to sulfur and nitrogen removal, and the trickle bed reactors would often become plugged when conditions approached 800/sup 0/F, 3 hours space time. With most of the sulfur in the residue fraction, little desulfurization was achieved with either NiMo or CoMo on alumina catalysts until sufficient hydrocracking had occurred. Very little nitrogen could be removed under all conditions tested. At the most severe conditions assessed (800/supmore »« less
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Mullendore, A.W. ; Lieberman, M.L.

The program consists of three tasks; ''Catalyst Improvement'' in which the mechanisms of catalyst deactivation and methods of reactivation will be explored; ''Ash Effects'' in which the effect of the mineral content of coals on liquefaction will be assessed in autoclave experiments; and ''Kinetic Studies'' in which a bench scale reactor will be set up to study the effects of process parameters on the kinetics of hydrodesulfurization and liquefaction. Analysis of used catalyst from a series of SYNTHOIL reactor runs has continued. Concentration profiles of Ti and Fe in used catalysts were found to match the form of diffusion profiles.more »« less