Magnetic resonance investigation of vanadia and vanadium-molybdenum gels synthesized with peroxovanadate precursors

J. W. Wiench; C. J. Fontenot; J. F. Woodworth; G. L. Schrader; M. Pruski; S. C. Larsen

doi:10.1021/jp045848e

Magnetic resonance investigation of vanadia and vanadium-molybdenum gels synthesized with peroxovanadate precursors

J. W. Wiench, C. J. Fontenot, J. F. Woodworth, G. L. Schrader, M. Pruski, S. C. Larsen

Research output: Contribution to journal › Article › peer-review

11 Scopus citations

Abstract

Vanadia gels and vanadium-molybdenum oxide gels were investigated using the magnetic resonance techniques, EPR spectroscopy and ⁵¹V MAS NMR spectroscopy. The vanadium oxide gels were derived from the reaction of H ₂O ₂ and V ₂O ₅, and the vanadium-molybdenum oxide (VMoO) gels were derived from the reaction of peroxovanadates with an ammonium molybdate solution. EPR spectroscopy was utilized to determine quantitative information about the concentration of V ⁴⁺ paramagnetic species present in the samples and additional structural information about the V ⁴⁺ coordination environment. ⁵¹V MAS NMR spectroscopy was used to elucidate the V ⁵⁺ electronic environment and how it changes as a function of molybdenum content. The observed line broadening of the ⁵¹V NMR signal with increasing molybdenum content was correlated with an increase in the concentration of paramagnetic species as monitored by EPR spectroscopy. The evolution of various vanadium sites during thermal treatment was also investigated. This work provides further support for the hypothesis that the selectivity of VMoO catalysts in the oxidation of 1,3-butadiene to maleic anhydride is due to the presence of paramagnetic V ⁴⁺ sites.

Original language	English (US)
Pages (from-to)	1756-1762
Number of pages	7
Journal	Journal of Physical Chemistry B
Volume	109
Issue number	5
DOIs	https://doi.org/10.1021/jp045848e
State	Published - Feb 10 2005
Externally published	Yes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Surfaces, Coatings and Films
Materials Chemistry

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title = "Magnetic resonance investigation of vanadia and vanadium-molybdenum gels synthesized with peroxovanadate precursors",

abstract = "Vanadia gels and vanadium-molybdenum oxide gels were investigated using the magnetic resonance techniques, EPR spectroscopy and 51V MAS NMR spectroscopy. The vanadium oxide gels were derived from the reaction of H 2O 2 and V 2O 5, and the vanadium-molybdenum oxide (VMoO) gels were derived from the reaction of peroxovanadates with an ammonium molybdate solution. EPR spectroscopy was utilized to determine quantitative information about the concentration of V 4+ paramagnetic species present in the samples and additional structural information about the V 4+ coordination environment. 51V MAS NMR spectroscopy was used to elucidate the V 5+ electronic environment and how it changes as a function of molybdenum content. The observed line broadening of the 51V NMR signal with increasing molybdenum content was correlated with an increase in the concentration of paramagnetic species as monitored by EPR spectroscopy. The evolution of various vanadium sites during thermal treatment was also investigated. This work provides further support for the hypothesis that the selectivity of VMoO catalysts in the oxidation of 1,3-butadiene to maleic anhydride is due to the presence of paramagnetic V 4+ sites.",

author = "Wiench, {J. W.} and Fontenot, {C. J.} and Woodworth, {J. F.} and Schrader, {G. L.} and M. Pruski and Larsen, {S. C.}",

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T1 - Magnetic resonance investigation of vanadia and vanadium-molybdenum gels synthesized with peroxovanadate precursors

AU - Wiench, J. W.

AU - Fontenot, C. J.

AU - Woodworth, J. F.

AU - Schrader, G. L.

AU - Pruski, M.

AU - Larsen, S. C.

PY - 2005/2/10

Y1 - 2005/2/10

N2 - Vanadia gels and vanadium-molybdenum oxide gels were investigated using the magnetic resonance techniques, EPR spectroscopy and 51V MAS NMR spectroscopy. The vanadium oxide gels were derived from the reaction of H 2O 2 and V 2O 5, and the vanadium-molybdenum oxide (VMoO) gels were derived from the reaction of peroxovanadates with an ammonium molybdate solution. EPR spectroscopy was utilized to determine quantitative information about the concentration of V 4+ paramagnetic species present in the samples and additional structural information about the V 4+ coordination environment. 51V MAS NMR spectroscopy was used to elucidate the V 5+ electronic environment and how it changes as a function of molybdenum content. The observed line broadening of the 51V NMR signal with increasing molybdenum content was correlated with an increase in the concentration of paramagnetic species as monitored by EPR spectroscopy. The evolution of various vanadium sites during thermal treatment was also investigated. This work provides further support for the hypothesis that the selectivity of VMoO catalysts in the oxidation of 1,3-butadiene to maleic anhydride is due to the presence of paramagnetic V 4+ sites.

AB - Vanadia gels and vanadium-molybdenum oxide gels were investigated using the magnetic resonance techniques, EPR spectroscopy and 51V MAS NMR spectroscopy. The vanadium oxide gels were derived from the reaction of H 2O 2 and V 2O 5, and the vanadium-molybdenum oxide (VMoO) gels were derived from the reaction of peroxovanadates with an ammonium molybdate solution. EPR spectroscopy was utilized to determine quantitative information about the concentration of V 4+ paramagnetic species present in the samples and additional structural information about the V 4+ coordination environment. 51V MAS NMR spectroscopy was used to elucidate the V 5+ electronic environment and how it changes as a function of molybdenum content. The observed line broadening of the 51V NMR signal with increasing molybdenum content was correlated with an increase in the concentration of paramagnetic species as monitored by EPR spectroscopy. The evolution of various vanadium sites during thermal treatment was also investigated. This work provides further support for the hypothesis that the selectivity of VMoO catalysts in the oxidation of 1,3-butadiene to maleic anhydride is due to the presence of paramagnetic V 4+ sites.

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Magnetic resonance investigation of vanadia and vanadium-molybdenum gels synthesized with peroxovanadate precursors

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