Ordered TiO 2 –SiO 2 mesoporous materials with BJH pore diameters in the range from 12 to 15nm were synthesized by a one-step hydrothermal synthesis method. In this route, tetraethoxysilane (TEOS) and titanium tetraisopropoxide (TTIP) in a low pH solution were used as SiO 2 and TiO 2 precursor, respectively with P123 as a template and hexane as a micelle expander in the presence of NH 4 F. In this work, we show the effect of different hydrothermal temperatures (70°C and 130°C) on pore structure and photocatalytic efficiency of the materials prepared. The synthesized materials were characterized by small-angle X-ray scattering (SAXS), N 2 adsorption–desorption experiments, X ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and field emission scanning electron microscopy (FESEM). The method could produce ordered mesoporous structure with uniform pore size of 12–15nm and high specific surface areas S BET up to 431m 2 /g. The photocatalytic activity of the samples was evaluated by degradation of MB under UV light irradiation and results showed these mesostructure materials have much higher photocatalytic efficiency in comparison with commercial P25 titania. The results also show that for materials synthesized using higher hydrothermal temperature (130°C) resulting in increased in photocatalytic activity due to higher formation of anatase phase and more open channels by comparison with lower hydrothermal treatment (70°C).