Two kinds of Fe3+/TiO2 catalysts are prepared by Sol-gel method and hydrolysis method. XRD, UV-Vis, BET, curves of N 2 adsorption-desorption and 3D fluorescence are used to analyze the structures and properties of the catalysts, and their photocatalytic activities are investigated through degradation of DBP. The results show that two kinds of catalysts are anatase TiO 2. The band gap of the Fe3+/TiO 2 catalysts prepared by Sol-gel and hydrolysis method are 2.6 eV and 3.2 eV respectively, and the former with an absorption edge at 477 nm, while the latter with no redshift. The curves of N 2 adsorption-desorption of the Fe3+/TiO 2 catalysts prepared by Sol-gel and hydrolysis method are type Ⅳ and Ⅴ, their BET specific surface areas are 57.03 m2/g and 10.94 m2/g, and the hysteresis loop of the latter shifts to the high relative pressure region with a smaller pore volume and a bigger average pore diameter. Two kinds of catalysts can reduce photoluminescence properties of TiO 2 at various degrees, and the catalyst prepared by Sol-gel method shows a weaker photoluminescence property. The results of degradation experiment show the degradation rate of DBP by catalyst prepared by Sol-gel method and hydrolysis method are 60.53% and 31.83% respectively after 2 h.