Synthesis of TS-1 from TiO2 and Ludox Silica and Use as Catalyst for Cyclooctene Epoxidation

Abstract

The aim of this work was the synthesis of a TS-1 zeolite starting from Si and Ti precursors more adapted to scale-up than TEOS and tetra-alkyl orthotitanates. Silica and titania were used here. The resulting TS-1 material was characterized and its catalytic performance evaluated in the oxidation of cyclooctene in liquid-phase (acetonitrile) using anhydrous H₂O₂ or tert-butyl hydroperoxide (TBHP) as oxidants. The TS-1 with Ti/Si = 0.0046 (XRF) was prepared via a hydrothermal treatment and characterized by X-ray diffraction (XRD), infrared spectroscopy (FT-IR), UV-Vis. spectroscopy. A MFI structure with high crystallinity was obtained in which the titanium atoms are tetrahedrally coordinated to four oxygen atoms. Using titanosilicalite TS-1 with MFI structure in heterogeneous catalytic oxydations of cyclooctene with aqueous H₂O₂ and Tert-butyl hydroperoxide the epoxide of cyclooctene is detected to be highest among the obtained variety of compounds. The reaction progress is monitored by GC-MS.

Keywords: Zeolite, XRF, TS-1, XRD, IR, UV-Vis., catalyst, cyclooctene, epoxidation