Abstract: Metal-organic framework material, Cu-MOF was synthesized by solvent-thermal method from terephthalic acid and copper nitrate hydrate, and then roasted at different temperaturein nitrogen to obtain copper-carbon composites, Cu-MOF-T (T=700 ℃, 800 ℃, 900 ℃, 1000 ℃). The materials were characterized by XPS, SEM and BET. The catalytic degradation performances of methyl orange (MO) simulated wastewater by Cu-MOF-T samples as Fenton like heterogeneous catalysts were investigated. The effects of initial pH, initial mass concentration of MO, and the stability of catalyst were optimized to explore the application of Cu-MOF-800. The results showed that Cu-MOF-T samples exhibited a porous lamellar structure with Cu, C, and O as the main components. The size (10～1μm) of Cu-MOF-T decreased with the increase of roasting temperature. Among these samples, Cu-MOF-800 had the maximum specific surface area, pore volumes and Cu+/Cu2+. Under the conditions of molar concentration of H2O2 10 mmol/L, mass concentration of catalyst 1 g/L, reaction temperature 50℃, pH value of solution 3, and mass concentration of MO 200 mg/, Cu-MOF-800 showed the best performance for the degradation of MO solution, and after 60 min of reaction, the degradation rate of MO could reach up to 99%. The degradation rate of Cu-MOF-800 for MO was still over 96% even after being for 5 cycles.