MIL-53 (Al) was synthesized by solvothermal method, and TiO2/MIL-53 (Al) photocatalyst was prepared by using TiO2 as the carrier for the catalytic degradation of methine blue in sewage. The photocatalytic performance of the TiO2/MIL-53(Al) and the TiO2/Al2O3 was compared. The catalysts were characterized by thermogravimetric-differential scanning calorimeter (TG-DSC), Fourier transform infrared(FTIR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and N2 adsorption-desorption. The photodegradation efficiency of submethyl blue was analyzed by photometric absorption method. The results showed that the degradation rate of methylene was more than 98.6% on TiO2/MIL-53(Al) photocatalyst, but that of methylene was only 70.3% on TiO2/Al2O3 photocatalyst. Therefore, the photocatalytic activity of TiO2/MIL-53(Al) photocatalyst exhibited much higher than that of the TiO2/Al2O3 photocatalyst in degradating methyl blue.