Abstract: The use of materials such as grapheme and metal organic framworks to enhance the electronic transmission capacity of semiconductor photocatalytic materials has become increasingly popular. In the experiment, ZnO/C was obtained from the metal organic framework MOF-5, which was used as precursor, by high-temperature treatment under nitrogen atmosphere. Then the nanocomposite photocatalyst ZnO/C/TiO2 composite was prepared by hydrothermal method using TiO2 as the basic particles. The crystal structure, morphology and composition properties of the samples were characterized by the approaches such as XRD, SEM, energy spectrum, surface area analyzer and porosity analyzer. By using orthogonal experiment method, the effects of MOF-5 treatment temperature was evaluated, and the influence of doping amount of ZnO/C and adding amount of butyl titanate on the photocatalytic properties of photocatalyst to methyl orange degradation were investigated by the orthogonal test as well. The results showed that the particle size of ZnO/C/TiO2 composite was 11.89 nm, the size of the sample was evenly distributed, and the particle size was nano-level, no agglomeration, the specific surface areas of TiO2 and ZnO/C/TiO2 were 87.5 and 109.0 m2/g, the average pore radius of them were 2.72 and 2.61 nm. The best conditions for the preparation of ZnO/C/TiO2 were as follows: MOF-5 was treated under 600℃, ZnO/C doping amount of 0.07 g, and addtion 1.5 mL of butyl titanate. After 90 min irradiation under UV light, the degradation rate of methyl orange was 62.1% with TiO2 as photocatalyst, the degradation rate was improved greatly to 99.5% with ZnO/C/TiO2 as photocatalyst. The catalytic activity increased substantially.