Abstract: Limonite/TiO₂ composite photocatalysis agent was prepared by sol-gel method in this paper.The XRD、SEM measurement and characterization and the degradation treatment experiments showed that, it had been loaded with a homogeneous TiO₂ film on its surface, and it had a firm nuclear/membrane structure, the removal rate of CODCr attained 70% after treatment and the residual CODCr was about 78.3 mg/L as compared with 251 mg/L under the condition of pH=4、catalyst dosage of 5 g/L and illumination time of 2 h, so it had better degradation effect, it also had superior recovery rate and better photocatalysis properties after recycle experiments.