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Journal of Structural Chemistry

2009 year, number 4


G.M. Maksimov, R.I. Maksimovskaya, O.A. Kholdeeva, M.A. Fedotov, V.I. Zaikovskii, V. G. Vasil'ev, S. S. Arzumanov
Keywords: heteropoly acids, titanium complexes, NMR
Pages: 648-657


Heteropoly acid (HPA) H8(PW11TiO39)2xH2O (I) is synthesized by three different ways and studied by chemical analysis, potentiometric titration, mass-spectrometry, IR, 31P, 183W, and 17O NMR spectroscopy, thermogravimetry, and transmission electron microscopy. Anion I consists of two subparticles of the Keggin structure bridged by Ti-O-Ti. The dimeric anion exists in HPA aqueous solutions at [I] > 0.02 M. At рН > 0.6 it splits to a [PW11TiO40]5- monomer stable up to рН ~ 6. When heated (150-400)°C, I splits into H3PW12O40 and, apparently, H3PW10Ti2O38 without phase separation. Thermolysis products are soluble and when dissolved in water turn again into I. Complete decomposition of I to oxides occurs at ~450°C.