TiO2-coated palygorskite powder was prepared by different hydrolysable methods. Photocatalytic activity of TiO2-coated palygorskite powder was studied through photo-degrading the golden yellow BES dyestuff solution under a 300 W high-pressure mercury lamp. The amount of catalyst, the calcined temperature of catalyst and times of the repeated experiments on photo-degradation were studied.The experimental results show that 300℃ seems to be the most proper calcined temperature for the catalyst. This kind of catalyst prepared by hydrolysable method watered directly contains anatase TiO2. Nevertheless, it can only obtain amorphous TiO2 after the synthesis of catalyst hydrolyzed with steam. The experimental results show that, when the dosage is 1 g/L, hydrolysable method watered directly has more efficient catalytic activity compared with hydrolyzing with steamthrough contrast experiments of adsorption, photo-catalysis and repeated experiments. When the TiO2-coated palygorskite powder prepared by the hydrolysable method is watered directly, the decoloring rate can reach 93% after 2 h of reaction.