Abstract: Nano-TiO₂ photocatalysis material was prepared by sol-gel method using butyl titanate as precursor and polyethylene glycol as template agent. The samples of nano-TiO₂ were characterized by XRD,SEM and UV-Vis. The catalytic activities of the TiO₂ samples prepared at different calcination temperatures were tested under ultraviolet irradiation with methyl orange as simulative pollutant.The results show that the samples prepared at 500 and 600℃ are composed of single anatase phase and a mixed phase of anatase and rutile is obtained with calcination at 700℃ for the nano-TiO₂. The crystal size of the nanoTiO₂ increases with increase in the calcination temperature,leading to decrease in the degradation rate of methyl orange.The maximum adsorption peak of the nano-TiO₂ appears at the wavelength of 432 nm with a favorable adsorption effect and a quick adsorption speed,which can reach the adsorption equilibrium in about 30 min.