Abstract: Using cationic surfactant cetyltrimethylammonium bromide（CTAB）as the template，TiO2 and V/Ce/F-TiO2 mesoporous materials were synthesized by sol-gel method and characterized by X-ray powder diffractometry (XRD)，N2 absorptiometry，transmission electron microscope (TEM)，thermal analyses (TG-DTA) and UV-Vis DRS．By systematically studying the influence of the synthesis parameters such as gelling time，aging temperature and time，the optimal conditions for reproducible synthesis of mesoporous titania were established. Specific area up to 189 m2·g－1 was obtained with average pore size in the range of 3.1—5.1 nm. The mesoporous structure of pure TiO2 could be destroyed by removal of template at a calcination temperature of 450 ℃. However，the mesoporous structure of V/Ce/F-TiO2 which removed template by calcination was retaine，which suggests that the mesoporous structure can be stabilized by the doped ions. Shift of the adsorption edge to visible light was found for the doped mesoprous TiO2.