TiO2 and CuZSM-5 were mixed together as photocatalyst in dealing with photocatalytic degradation of methyl orange. Adsorption and photocatalytic degradation properties of the CuZSM-5 zeolite and mixture of TiO2 and CuZSM-5 were investigated. The CuZSM-5 zeolite has no photocatalytic activity under the experimental conditions. Methyl orange decoloration rate was 65.4%, which was 9.60% higher than that without using CuZSM-5, when TiO2 and CuZSM-5 were at the optimum ratio of 3.13:1. An optimum TiO2 concentration of 250 mg/l occurred when using pure TiO2. However, when using TiO2-CuZSM-5 mixture, the decoloration rate continuously increased with increasing photocatalyst concentration. After 70 min of irradiation, 98.4% of the initial methyl orange decoloration was found using TiO2-CuZSM-5 mixture at TiO2 concentration of 250 mg/l.