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NMR Spectroscopic Studies of Interactions in Solution during the Synthesis of MoVTeNb Oxide Catalysts Full article

Journal European Journal of Inorganic Chemistry
ISSN: 1434-1948 , E-ISSN: 1099-0682
Output data Year: 2008, Number: 31, Pages: 4906-4914 Pages count : 9 DOI: 10.1002/ejic.200800500
Tags Molybdenum, NMR spectroscopy, Polyoxometalates, Tellurium, Vanadium
Authors Maksimovskaya Raisa I. 1 , Bondareva Valentina M. 1 , Aleshina Galina I. 1
Affiliations
1 Boreskov Institute of Catalysis, Russian Academy of Sciences, Lavrentiev avenue 5, Novosibirsk 630090, Russia

Funding (1)

1 Russian Foundation for Basic Research 07-03-00695

Abstract: Aqueous solutions used for the synthesis of MoVTeNb oxide catalysts have been studied with 125Te, 95Mo, 51V, and 17O NMR spectroscopy. Polyoxometalate (POM) anion V9TeO285–(I), which has the decavanadate structure, containing Te6+ in one of its two central positions, has been identified for the first time in VV-TeVI solutions. In ternary MoVI-VV-TeVI solutions, the POMs TeMo6O246– (II) (pH ca. 7.8–2) as well as previously unknown complexes of the proposed compositions TeV3Mo3O249– (III) (pH ca. 8–5) and TeMo3V5O275– (IV) (pH ca. 6–1) were observed. In the structure of IV, half of the decavanadate anion is combined with half of the octamolybdate anion, in which the central Mo atom is replaced with Te6+. There is an equilibrium, IV i I + II, in the ternary solutions. Despite its stability in solution, polyanion IV could not be isolated in the solid state. During concentration under ambient conditions, less soluble polyanion II begins to crystallize first, and the equilibrium in solution gradually shifts to I. Upon dissolving the precipitate, complex IV forms again. The distribution diagrams have been derived from the NMR spectra for a solution of the cationic composition Mo1V0.3Te0.23 with NH4+ as a counterion, acidified with HClO4 in the pH range 7.25–1. In addition to the above-mentioned complexes, VO2+ and MoO22+ oxalates form in the presence of oxalic acid. Upon adding niobium oxalate, Nb2O5 gel forms without any Nb-containing species in solution.
Cite: Maksimovskaya R.I. , Bondareva V.M. , Aleshina G.I.
NMR Spectroscopic Studies of Interactions in Solution during the Synthesis of MoVTeNb Oxide Catalysts
European Journal of Inorganic Chemistry. 2008. N31. P.4906-4914. DOI: 10.1002/ejic.200800500 WOS Scopus РИНЦ ANCAN OpenAlex
Dates:
Submitted: May 21, 2008
Published online: Sep 30, 2008
Published print: Nov 1, 2008
Identifiers:
Web of science: WOS:000261049700011
Scopus: 2-s2.0-55249096941
Elibrary: 13570498
Chemical Abstracts: 2008:1440308
Chemical Abstracts (print): 151:349232
OpenAlex: W2036072515
Citing:
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Web of science 11
Scopus 13
Elibrary 11
OpenAlex 13
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