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Materials 2010, 3(2), 897-917; doi:10.3390/ma3020897

EDTA-Reduction of Water to Molecular Hydrogen Catalyzed by Visible-Light-Response TiO2-Based Materials Sensitized by Dawson- and Keggin-Type Rhenium(V)-Containing Polyoxotungstates

1
Department of Chemistry, Faculty of Science, Shizuoka University, 836 Ohya, Suruga-ku, Shizuoka 422-8529, Japan
2
Department of Chemistry, Faculty of Science, Kanagawa University, Tsuchiya 2946, Hiratsuka, Kanagawa 259-1293, Japan
*
Author to whom correspondence should be addressed.
Received: 27 November 2009 / Revised: 12 January 2010 / Accepted: 2 February 2010 / Published: 2 February 2010
(This article belongs to the Special Issue Polyoxometalate Compounds)
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Abstract

The synthesis and characterization of a Keggin-type mono-rhenium(V)-substituted polyoxotungstate are described. The dimethylammonium salt [Me2NH2]4[PW11ReVO40] was obtained as analytically pure homogeneous black-purple crystals by reacting mono-lacunary Keggin polyoxotungstate with [ReIVCl6]2- in water, followed by crystallization from acetone at ca. 5 °C. Single-crystal X-ray structural analysis of [PW11ReVO40]4- revealed a monomeric structure with overall Td symmetry. Characterization of [Me2NH2]4[PW11ReVO40] was also accomplished by elemental analysis, magnetic susceptibility, TG/DTA, FTIR, UV-vis, diffuse reflectance (DR) UV-vis, and solution 31P-NMR spectroscopy. Furthermore, [PW11ReVO40]4- and the Dawson-type dirhenium(V)-oxido-bridged polyoxotungstate [O{ReV(OH)(α2-P2W17O61)}2]14- were supported onto anatase TiO2 surface by the precipitation methods using CsCl and Pt(NH3)4Cl2. With these materials, hydrogen evolution from water in the presence of EDTA⋅2Na (ethylenediamine tetraacetic acid disodium salt) under visible light irradiation (≥400 nm) was achieved.
Keywords: polyoxometalate; rhenium; titanium dioxide; hydrogen evolution; visible light polyoxometalate; rhenium; titanium dioxide; hydrogen evolution; visible light
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MDPI and ACS Style

Kato, C.N.; Hara, K.; Kato, M.; Amano, H.; Sato, K.; Kataoka, Y.; Mori, W. EDTA-Reduction of Water to Molecular Hydrogen Catalyzed by Visible-Light-Response TiO2-Based Materials Sensitized by Dawson- and Keggin-Type Rhenium(V)-Containing Polyoxotungstates. Materials 2010, 3, 897-917.

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