Synthesis and Physicochemical Study
of the PMo₁₁(TiO) Heteropolyanion

T. E. Svinarenko^a, A. B. Vishnikin^a, and M. N. Timofeeva^b

^a Dnipropetrovsk National University, vul. Naukova 13, Dnipropetrovsk, 49625 Ukraine

^b Boreskov Institute of Catalysis, Siberian Branch, Russian Academy of Sciences,
pr. Akademika Lavrent’eva 5, Novosibirsk, 630090 Russia

Received July 12, 2007

Abstract—Procedures were developed for the synthesis of the guanidinium (Gua) and tetrabutylammonium
(TBA) salts of 11-molybdotitano(IV)phosphate heteropolyanion (MTPH) from solutions with the stoichiomet-
ric ratio P : Mo = 1 : 11 and in excess of titanium(IV) ions, Ti : P 1.5, at pH 1.85–1.90. MTPH was isolated
as the (Gua)₅PMo₁₁(TiO)O₃₉ and (TBA)₅PMo₁₁(TiO)O₃₉ salts. The composition and formula of MTPH were
established by chemical analysis, electronic absorption spectroscopy in the visible region of the oxidized and
reduced MTPH forms, IR spectroscopy, and ³¹P NMR. H₅PMo₁₁(TiO)O₃₉, obtained by ion exchange of the Gua
salt in an aqueous–organic medium, is a strong pentabasic acid. MTPH reacts with ₂₂ to form a peroxo com-
plex with limited stability in an aqueous solution. In aqueous–organic media, the peroxo complex is more sta-
ble. In acetonitrile, MTPH persists for several days.

DOI: 10.1134/S0036023608090039

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