Synthesis of Ti-MCM-41 directly from silatrane and titanium glycolate and its catalytic activity1

Abstract

Titanium is successfully incorporated in hexagonal mesoporous silica to form Ti-MCM41 at low temperature. Silatrane and titanium glycolate synthesized from the oxide one-pot synthesis process are used as the precursors. Using the cationic surfactant cetyltrimethylammonium bromide as a template, the resulting meso-structure mimics the liquid-crystal phase. The percentage of titanium loading is varied in the range 1–35%. The temperatures used in the preparation are 60 °C and 80 °C. After heat treatment, very high surface area mesoporous silica was obtained and characterized using diffuse reflectance UV (DRUV) spectroscopy, X-ray diffraction (XRD), BET surface area, X-ray fluorescence, energy dispersive spectroscopy and transmission electron microscopy (TEM). At 35% titanium, the titanium atom is also in the framework showing the pattern of hexagonal mesostructure, as shown by DRUV, XRD and TEM results. The surface area is extraordinarily high, up to more than 2300 m2 g−1, and the pore volume is as high as 1.3 cm3 g−1 for a titanium loading range of 1–5%. Oxidative bromination reaction using Ti-MCM-41 as catalyst showed impressive results, with the 60 °C catalysts having higher activity. Copyright © 2005 John Wiley & Sons, Ltd.