Characterization of Hydrocarbon Soluble Metal Oxides. Precursors to Supported Catalysts

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Abstract
The metal oxide carboxylate complexes described in the previous chapter have been characterized by infrared spectroscopy, x-ray diffraction, electron microscopy, and analytical ultracentrifugation. The molecular weights and solution particle diameters have been determined for a number of the hydrocarbon soluble particles by analytical ultracentrifugation methods, and the use of a spherical model consistent with the particulate shape observed by electron microscopy. The size of the soluble complexes has been studied as a function of: metal, metal/acid ratio, acid composition, and solvent. The molecular weights for the ultimate particles are reasonably independent of the metal employed in the synthesis and are relatively constant for materials with similar metal/acid equivalents ratios. The single particle molecular weights for the complexes studied ranged from approximately 5×104 to 1.5×106g mole−1. The solution size distribution was polydisperse in all cases, with aggregates of the ultimate particles prevalent. Weight average molecular weights in excess of 109g mole−1 have been observed. The aggregation is dependent on the surface acid composition and on the solvent in which the soluble complex is dispersed. Solubility and stability of these materials have been examined in a number of solvents. The metal oxide particles are initially soluble in octane, isooctane, cyclohexane, mineral spirits, carbon tetrachloride, benzene, and tetrahydrofuran. However, most of the complexes eventually precipitate from dilute solutions in carbon tetrachloride, benzene, and tetrahydrofuran. The stability of the particles is decreased in the presence of oxygen, or when carboxylic acids, alcohols, or ketones are present even in small amounts, and is decreased even further at temperatures above 100°C. Heterogeneous catalysts have been prepared by deposition of several of the soluble metal oxides onto supports such as alumina, silica, or kieselguhr followed by oxidation to yield supported metal oxides or reduction to yield supported metal. The application of few supported metals and metal oxides in hydrogenations of olefins, benzene, and naphthalene is described.

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