A rapid and facile method was used to synthesize high quality titanium containing cubic MCM-48 mesoporous materials at room temperature. Four kinds of titanium containing MCM-48 mesoporous materials were prepared by addition of the titanium precursor at different stages during the formation of MCM-48 gel. The mesoporous structure and the light absorption characteristics of Ti-MCM-48 were studied by X-ray diffraction (XRD), diffuse reflectance spectra (DRS), and nitrogen isotherm studies. The photocatalytic activities of these heterogeneous Ti-MCM-48 catalysts were tested for photocatalytic hydrogen evolution from methanol water mixture under UV irradiation. High activity was achieved in the absence of platinum cocatalyst, which is usually indispensable to TiO(2) photocatalyst for hydrogen evolution. (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.