Abstract:Nano-silica microspheres prepared by conventional St?ber method were used as hard-template. The aluminum foil?assisted NaBH4 reducing black-mesoporous TiO2 prepared by aqueous sol-gel peptization process is co-doped with N and Zr, named Zr,N/mes.-TiO2—x. This research selects methylene blue as degradation object. The effects of pH value, temperature and photocatalyst dosage on degradation rate of methylene blue were studied by characterization methods such as SEM, BET，PL and so on. The results show that Zr,N/mes.-TiO2—x has fantastic photocatalytic performance. In addition, its unique pore structure has the synergistic effect of adsorption-photocatalysis. At room temperature, the catalyst can achieve 99% degradation of 10 mg/L methylene blue within 50 min.