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A sup 95 Mo solid-state NMR study of hydrodesulfurization catalysts. 1. Formation of fresh HDS catalyst precursors by adsorption of polyoxomolybdates onto. gamma. -alumina

Journal Article · · Journal of the American Chemical Society; (United States)
DOI:https://doi.org/10.1021/ja00179a020· OSTI ID:5636738
; ;  [1]
  1. Univ. of South Carolina, Columbia (United States)
The solid-state {sup 95}Mo NMR of oxomolybdates and polyoxomolybdates adsorbed to {gamma}-alumina was utilized to characterize the molybdenum species present at circa monolayer coverages of molybdenum. This represents the first attempt at using solid-state NMR to look directly at the molybdenum species on the surface of 'fresh' hydrodesulfurization catalyst precursors. The selectively excited central {plus minus}1/2 transition line shapes were obtained, by the solid-echo technique, for several polyoxomolybdates, which are considered model compounds of the surface molybdena species, as well as for the uncalcined and calcined catalysts at various loadings. The spectra were obtained for static and magic angle spinning samples. Static sample spectra of the catalysts reveal inhomogeneously broadened lines owing to a range of surface species being present. Magic and angle spinning spectra show the presence of four possible species on the surface of the uncalcined catalysts and two possible species present on the surface of calcined catalysts. Spikelet echo spectra identified static adsorbed species (speculated to be predominantly adsorbed tetrahedral/octahedral molybdena, and perhaps Al{sub 2}(MoO{sub 4}){sub 3}), and a dynamic species (speculated to be disordered, surface-interactive tetrahedral and octahedral molybdates), in the uncalcined catalyst samples. Upon calcination the line widths of the static and MAS spectra are increased, indicating a polymerization of the surface species to form a MoO{sub 3}-like phase. 67 refs.
DOE Contract Number:
FG09-84ER13296
OSTI ID:
5636738
Journal Information:
Journal of the American Chemical Society; (United States), Journal Name: Journal of the American Chemical Society; (United States) Vol. 112:23; ISSN 0002-7863; ISSN JACSA
Country of Publication:
United States
Language:
English

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