Photoactive TiO 2 was directly obtained by sol–gel method or from titanium dioxide/activated carbon composite (TiO 2/AC), then calcinated under air at 700 °C. The obtained materials were characterized by N 2 adsorption (77 K), X-ray diffraction (XRD), diffuse reflectance UV-vis spectroscopy (UV/DRS) and transmission electron microscopy (TEM). The solid prepared from (TiO 2/AC) composite was found to be mainly pure anatase phase with SiO 2 and Fe 2O 3 traces, whereas, pure TiO 2 was predominantly rutile. Adding activated carbon increases the surface area of photocatalyst, reduces the grain size of titania particles and causes a blue shift of the light absorption spectrum due to the quantization of band structure. Photocatalytic activity was tested and compared with that of TiO 2 Degussa P25 on the degradation of methylene blue (MB) in an aqueous solution under visible irradiation. TiO 2(AC-700) catalyst was found to be two times more active than TiO 2-P25.