Nanocrystalline La3+-doped TiO2 of 20-30 nm in size was prepared by a sol-gel technique. The photocatalytic activities of the samples were evaluated by the degradation of harmful acid orange 7(AO7) azo-dye in aqueous solution. The effects of La3+ ion implantation on the photocatalytic activity of TiO2 were also discussed. The results show that the La3+content plays an essential role in affecting the photocatalytic activity of the La3+-doped TiO2 and the optimum content of La3+-doped is 1.0 wt.%. The photocatalytic activity of the samples with La3+-doped TiO2 is higher than that of pure TiO2 in the treatment of AO7 wastewater. The photodegradation effect of AO7 effluent is the best by means of La3+-doped TiO2 with 1.0% La3+.