Synthesis, characterization and catalytic properties of sol–gel derived mixed oxides

• Published in: The Journal of physics and chemistry of solids Vol. 64; no. 12; pp. 2385 - 2389
• Main Authors: de Farias, Robson F, Arnold, Ulrich, Martı́nez, Leandro, Schuchardt, Ulf, Jannini, Marcelo J.D.M, Airoldi, Claudio
• Format: Journal Article
• Language: English
• Published: Oxford Elsevier Ltd 01-12-2003; Elsevier
• Subjects: Catalysis; Chemistry; Cross-disciplinary physics: materials science; rheology; Cyclooctene; Epoxidation; Exact sciences and technology; General and physical chemistry; Materials science; Materials synthesis; materials processing; Mixed oxides; Physics; Sol-gel processing, precipitation; Sol–gel process; Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry; Epoxidation; Cyclooctene; Mixed oxides; Sol–gel process; Aluminium oxide; Binary compound; Adsorption isotherm; Experimental study; X ray diffraction; Inorganic compound; Calcining; Hexagonal lattices; Zirconium oxide; Transition metal compounds; Sol gel process; Silicon oxides; Surface area; Titanium oxide; Amorphous state structure; Catalyst
• ISSN: 0022-3697; 1879-2553
• DOI: 10.1016/S0022-3697(03)00276-2

Alumina and 1:1 mixed oxides of Al
2O
3–ZrO
2, Al
2O
3–TiO
2, SiO
2–TiO
2 and ZrO
2–TiO
2 were synthesized via a sol–gel process by the so-called neutral amine route, followed by calcination at 600 °C. The mixed oxides were characterized before calcination by X-ray diffraction, revealing ordered hexagonal (Al
2O
3, Al
2O
3–ZrO
2, ZrO
2–TiO
2) and lamellar (SiO
2–TiO
2, Al
2O
3–TiO
2) structures. After calcination, all samples exhibited amorphous structures. Surface areas and pore characteristics of all materials were determined by nitrogen adsorption isotherms. The calcined oxides are active catalysts in the epoxidation of cyclooctene with
tert-butyl hydroperoxide as oxidant. Epoxide yields from 14 to 45% were found for reaction times of 24 h. The titanium oxide containing catalysts are the most active and selective ones. On the other hand, the poisoning of acidic centers yields a decreasing activity while increasing selectivity.