A NOVEL APPROACH TO CATALYTIC DESULFURIZATION OF COAL Metadata

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Title

  • Main Title A NOVEL APPROACH TO CATALYTIC DESULFURIZATION OF COAL

Creator

  • Author: Verkade, John G.
    Creator Type: Personal

Contributor

  • Sponsor: United States. Department of Energy.
    Contributor Type: Organization
    Contributor Info: US Department of Energy (United States)

Publisher

  • Name: National Energy Technology Laboratory (U.S.)
    Place of Publication: Pittsburgh, Pennsylvania
    Additional Info: National Energy Technology Lab., Pittsburgh, PA (United States)
  • Name: National Energy Technology Laboratory (U.S.)
    Place of Publication: Morgantown, West Virginia
    Additional Info: National Energy Technology Lab., Morgantown, WV (United States)

Date

  • Creation: 2001-11-01

Language

  • English

Description

  • Content Description: Column chromatographic separation of the S=PBu{sub 3}/PBu{sub 3} product mixture followed by weighing the S=PBu{sub 3}, and by vacuum distillation of S=PBu{sub 3}/PBu{sub 3}mixture followed by gas chromatographic analysis are described. Effects of coal mesh size, pre-treatment with methanol Coal (S) + excess PR{sub 3} {yields} Coal + S=PR{sub 3}/PBu{sub 3} and sonication on sulfur removal by PBu{sub 3} revealed that particle size was not observed to affect desulfurization efficiency in a consistent manner. Coal pretreatment with methanol to induce swelling or the addition of a filter aid such as Celite reduced desulfurization efficiency of the PBu{sub 3} and sonication was no more effective than heating. A rationale is put forth for the lack of efficacy of methanol pretreatment of the coal in desulfurization runs with PBu{sub 3}. Coal desulfurization with PBu{sub 3} was not improved in the presence of miniscule beads of molten lithium or sodium as a desulfurizing reagent for SPBu{sub 3} in a strategy aimed at regenerating PBu{sub 3} inside coal pores. Although desulfurization of coals did occur in sodium solutions in liquid ammonia, substantial loss of coal mass was also observed. Of particular concern is the mass balance in the above reaction, a problem which is described in some detail. In an effort to solve this difficulty, a specially designed apparatus is described which we believe can solve this problem reasonably effectively. Elemental sodium was found to remove sulfur quantitatively from a variety of polycyclic organosulfur compounds including dibenzothiophene and benzothiophene under relatively mild conditions (150 C) in a hydrocarbon solvent without requiring the addition of a hydrogen donor. Lithium facilitates the same reaction at a higher temperature (254 C). Mechanistic pathways are proposed for these transformations. Curiously, dibenzothiophene and its corresponding sulfone was virtually quantitatively desulfurized in sodium solutions in liquid ammonia at -33 C, although the yield of biphenyl was only about 20 to 30%. On the other hand, benzothiophene gave a high yield of 2-ethylthiophenol under these conditions. Although our superbase P(MeNCH{sub 2}CH{sub 2}){sub 3}N, which is now commercially available, is a more effective desulfurizing agent for a variety of organophosphorus compounds than PPh{sub 3} or its acyclic analogue P(NMe){sub 3}, it does not desulfurize benzothiophene or dibenzothiophene.
  • Physical Description: 46 pages

Subject

  • STI Subject Categories: 08 Hydrogen
  • Keyword: Hydrocarbons
  • STI Subject Categories: 10 Synthetic Fuels
  • Keyword: Biphenyl
  • Keyword: Sodium
  • Keyword: Mass Balance
  • STI Subject Categories: 01 Coal, Lignite, And Peat
  • Keyword: Desulfurization
  • Keyword: Thionaphthenes
  • Keyword: Coal
  • Keyword: Sulfur
  • Keyword: Ammonia
  • Keyword: Methanol
  • Keyword: Lithium
  • Keyword: Sulfones
  • Keyword: Particle Size
  • Keyword: Hydrogen
  • Keyword: Solvents

Source

  • Other Information: PBD: 1 Nov 2001

Collection

  • Name: Office of Scientific & Technical Information Technical Reports
    Code: OSTI

Institution

  • Name: UNT Libraries Government Documents Department
    Code: UNTGD

Resource Type

  • Report

Format

  • Text

Identifier

  • Report No.: FG22-95PC95208--16
  • Grant Number: FG22-95PC95208
  • DOI: 10.2172/800760
  • Office of Scientific & Technical Information Report Number: 800760
  • Archival Resource Key: ark:/67531/metadc741026

Note

  • Display Note: OSTI as DE00800760