Postsynthesis, characterization, and catalytic properties in alkene epoxidation of hydrothermally stable mesoporous Ti-SBA-15

Mesoporous Ti-SBA-15 has been postsynthesized by the titanation of pure silica SBA-15 in glycerol with the assistance of quaternary organic ammonium hydroxides, and has been extensively characterized by various techniques to investigate the mesostructural and catalytic properties, and the chemical nature of the incorporated Ti species, in comparison with those of Ti-MCM-41. To incorporate tetrahedral Ti species into the silica walls of SAB-15, the titanation needs to be carried out at elevated temperature and using an optimum amount of organic ammonium hydroxide. Ti-SBA-15 samples with a Si/Ti ratio ranging from 376 to 16 are successfully prepared with the retention of hexagonal mesostructure by elaborately conducting the titanation. The nature of the Ti species depends greatly on the Ti loading. At Si/Ti ratios higher than 50, the Ti species are mainly tetrahedrally coordinated in isolated states, while poorly dispersed Ti species of octahedral coordination are formed at higher Ti incorporation levels; however, no anatase phase is formed in all cases. The IR band at 948 cm^-1 due to Si-O-Ti bonds can be used to characterize the tetrahedral Ti species in mesoporous materials, but the techniques of dehydration or trimethylsilylation should be adopted to get rid of the influence of silanol groups. In an actual catalytic reaction, Ti-SBA-15 exhibits not only extremely high thermal stability but also outstanding endurance against Ti leaching not observed for Ti-MCM-41. Ti-SBA-15 is thus presumed to be a promising liquid-phase oxidation catalyst.