A intercalated TiO2photocatalyst loaded bentonite was prepared by sol-gel method. The effect of reaction time, reaction temperature,the amount of butyl titanate and other process parameters on prepared material of degradation of methyl orange,as well as the relationship between the concentration of methyl orange on degradation process and illumination time were discussed by single factor method.The results showed : the first absorbance of the intercalated TiO2photocatalyst loaded bentonite material was 0.342 and the average absorbance was respectively 0.7402 through 5 washing after the intercalated TiO2photocatalyst loaded bentonite irradiated at UV-irradiation 1.5h to 20mg/L methyl orange.