Abstract: TiO2 loaded photocatalysts immobilized on fly ash micro-sphere were prepared by the sol-gel methods.The crystal phase and morphology of TiO2/ microsphere were investigated with XRD and SEM. The photocatalytic activities of TiO2/ microsphere with different preparation conditions and TiO2 amounts on micro-sphere were evaluated by degradation of phenol. The results showed the best conditions of preparation as follows：four times of catalyst loading，calcination at 550 ℃ centigrade for 2 hours. When phenol concentration was 102 mg/L，degeneration rate reached 60% after 120 minutes.