TiO2, 1%La/TiO2, 1%Ce/TiO2 and a series of Laand Ce co-doped TiO2 photocatalysts were prepared by sol-gel method. Using sol-gel method combine with hydrothermal method prepared rare earth La, Ce and nitrogen co-doped TiO2 photocatalysts. The microstructure, spectroscopy performance and ion doped form of prepared samples were characterized by X-ray powder diffraction (XRD), UV-Vis diffuse reflectance spectroscopy techniques and X-ray photoelectron spectroscopy (XPS). The photocatalytic activity of doped TiO2 were examined by measuring the photodegradation of methyl orange. The results showed that the products were all anatase TiO2 nano powder, doping Laor Cehinder the growth of TiO2 particle, further more, doping Laand Cetogether hinder the growth of TiO2 particle more effective, doping N broaden the light response range of TiO2 photocatalyst. At the same time, the photocatalytic activity results indicated that the prepared samples showed superior UV light photocatalytic activity, the sample 1% (La:Ce,9:1)-N/TiO2 showed the highest UV-vis photocatalytic activity.