IV Oxy acetylacetonate

Blanch master s dissertation, The Pennsylvania State University, 1956. 

Vanadium(IV) oxy(acetylacetonate) has been prepared by direct reaction of acetylacetone (2,4-pentanedione) with either hydrous vanadium(IV) oxide or an aqueous solution of an oxovanadium(IV) salt.1-3 Procedure A is an adaptation of this approach. The facts that acetylacetone can reduce vanadium(V) oxide to vanadium(IV) oxide, react as an acid4,5 with the latter to give the desired product, and behave as a solvent for that product are combined in procedure B to give a synthesis based directly upon readily available starting materials. 

Preparation from Vanadium (V) Oxide through Prior Reduction to Oxovanadium(IV) Ion 

Submitted by Richard A. Rowe and Mark M. Jones Checked by Peter Block  

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Bi s (2,4-pentanedionato) oxovanadium (I V) [vanadium-(IV) oxy(acetylacetonate)] has been prepared by direct reaction of 2,4-pentanedione and vanadium(V) oxide. By using the same method, bis(4-imino-2-pentanonato)oxo-vanadium(IV) has been prepared by substituting acetyl-acetone imide (4-imino-2-pentanone) for acetylacetone. ... 

This general procedure is illustrated in the preparation of vanadium(IV) oxy(acetylacetonate) (synthesis 30B). 

Vanadium(IV) oxy(acetylacetonate) is a blue to blue-green compound, crystallizing in the monoclinic system with refractive indexes of a, 1.520 0, 1.676 y, 1.739.7 The compound was originally believed to be a 1-hydrate but is now known to be anhydrous. It forms addition compounds with pyridine, methylamine, and other amines.8 Vanadium(IV) oxy(acetylacetonate) decomposes at elevated temperatures and has no definite melting point. The compound is soluble in ethanol, benzene, chloroform, and acetylacetone but is only moderately soluble in acetone or ethyl ether. 

B1VO4 film preparation by the metal organic decomposition (MOD) method BiV04 films were prepared by a modified MOD method [9]. Bismuth 2-ethyl-hexanoate in acetylacetone and vanadium (IV) (oxy)acetylacetonate in acetylacetone were mixed in a stoichiometric ratio, PEG 300 was added and the solution was concentrated by evaporation of the solvent. A spin coater was used to coatFTO conducting glass with the solution, and the coated glass was fired at 400-550°C for 30 min. 

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