Synthesis and characterization of supported vanadium oxides by adsorption of the acetylacetonate complex

Supported vanadium oxide catalysts are prepared by adsorption and calcination of vanadium acetylacetonate complexes on the surfaces of silica and alumina. The interaction of the complex with the support is studied by FTIR, XRD, TGA and chemical analysis. The synthesis parameters are optimized in order to obtain a well dispersed layer on the surface. After calcination, the acetylacetonate complexes decompose and form a surface layer of VOx species. These surfaces have been studied with 51V NMR, UV–VIS diffuse reflectance and XRD spectroscopies. The method of acetylacetonate adsorption on silica enables the creation of supported VOx catalysts with a V loading of 0.5 mmol g–1(2.5 wt.% V), with all species in a strictly tetrahedral configuration and no formation of microcrystallites. On the alumina surface, vanadium loadings that are 5 times higher can be achieved without induced crystallinity.

[1]  S. Haukka,et al.  Chemisorption of chromium acetylacetonate on porous high surface area silica , 1994 .

[2]  H. Kung,et al.  The effect of loading of vanadia on silica in the oxidation of butane , 1993 .

[3]  M. White Uses of polynuclear metal complexes to develop designed dispersions of supported metal oxides , 1993 .

[4]  M. Kudo,et al.  Adsorbed structure of copper and calcium dipivaloylmethanates on SiO2 , 1992 .

[5]  G. Centi,et al.  Physicochemical characterization of V-silicalite , 1992 .

[6]  H. Eckert,et al.  Solid-state vanadium-51 NMR structural studies on supported vanadium(V) oxide catalysts: vanadium oxide surface layers on alumina and titania supports , 1989 .

[7]  Y. Nishimura,et al.  V2O5/SiO2 catalysts modified by Na+ ions: surface characterization by spectroscopic methods and photoassisted oxidation of 2-propanol and propene , 1989 .

[8]  J. Grimblot,et al.  Investigation of silica-supported vanadium oxide catalysts: preparation and characterization by vanadium-51 NMR and x-ray photoelectron spectroscopy , 1988 .

[9]  K. Fujimoto,et al.  Reduction of nitric oxide with ammonia on vanadium oxide catalysts supported on homogeneously precipitated silica-titania , 1981 .

[10]  H.‐G. Jerschkewitz,et al.  Untersuchungen an katalytisch aktiven Oberflächenverbindungen. II. Zur Existenz unterschiedlicher Vanadium(V)‐oxid‐Oberflächenphasen auf SiO2 und ihre katalytischen Eigenschaften , 1978 .

[11]  P. Voort,et al.  Preparation of supported vanadium oxide catalysts. Adsorption and thermolysis of vanadyl acetylacetonate on a silica support , 1996 .

[12]  P. Geladi,et al.  Special data handling techniques for Fourier-transform infrared photoacoustic spectra: estimation and characterization of the N contents on ammoniated trichlorosilylated silica gel, using partial least-squares regression and curve fitting on the Si-H stretching vibration , 1993 .

[13]  P. Grange,et al.  Influence of the Preparation Method On the V2o5/tio2/sio2 Catalysts in Selective Catalytic Reduction of Nitric-oxide With Ammonia , 1991 .

[14]  A. Wokaun,et al.  Spectroscopic investigation of the structure of silica-supported vanadium oxide catalysts at submonolayer coverages , 1991 .

[15]  P. Voort,et al.  Effect of porosity on the distribution and reactivity of hydroxyl groups on the surface of silica gel , 1991 .

[16]  W. Hesselink,et al.  Interaction of transition-metal acetylacetonates with γ-Al2O3 surfaces , 1989 .

[17]  R. Larsson,et al.  Activity measurements and spectroscopic studies of the catalytic oxidation of toluene over silica-supported vanadium oxides , 1988 .

[18]  A. Baiker,et al.  Selective catalytic reduction of nitric oxide with ammonia: I. Monolayer and Multilayers of Vanadia Supported on Titania , 1987 .

[19]  G. Öhlmann,et al.  Investigations of catalytically active surface compounds: XVII. Influence of size and structure of vanadium oxide clusters on selectivity in the oxidation of n-butene , 1985 .

[20]  P. Ratnasamy,et al.  Catalytic Aluminas: Surface Models and Characterization of Surface Sites , 1978 .