TiO2/Al-MCM-41 composites with various titania content were prepared by loading titania into the mesopores of Al-MCM-41 mesoporous molecular sieve from coal-measure kaolin as silicon and aluminum source via general sol-gel method and incipient wetness impregnation method. TiO2/Al-MCM-41 composites were characterized by XRD, FT-IR and SEM, and the photocatalytic degradation of methyl orange solution under visible light irradiation. The results showed that the titania crystalline phase was anatase, and the particles size of TiO<sub>2</sub> increase with TiO<sub>2</sub> content. The photocatalytic degradation rates of all samples prepared by sol-gel method and incipient wetness impregnation have been become stable by visible light irradiation for 150 min, and the highest degradation rate was 83.7% and 76% respectively.
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