Nanosized titanium dioxide photocatalysts with anatase structure or mixture of anatase and rutile phases have been synthesized. Homogeneous precipitation of aqueous solutions containing TiOSO4 and ammonia and following treatment with H2O2 was used to prepare porous yellowish (Ti-Per) gel. The gel was lyophilized for 48h and (Ti-Per)LYO-powder was obtained. Single phase anatase TiO2 samples were prepared by heating of the (Ti-Per)LYO powder. The lamella-like particle morphology of TiO2 samples determined by SEM were stable in air up to 950°C.The structure evolution during heating of the starting (Ti-Per)LYO powder was studied by DTA and XRD analyses in overall temperature range of phase transformation. The morphology and microstucture characteristics were also obtained by HRTEM and BET methods. The photocatalytic activity of the sample titania TI-LYO/950 heated to 950ºC in air contained 78.4% anatase and 21.6% rutile was higher than standard Degussa P25. Titania sample TI-LYO/950 reveals the highest catalytic activity during the photocatalyzed degradation course of 4-chlorophenol in aqueous suspension under UV-irradiation.