Cu3(PO4)2, Cu2P2O7, Cu5(P3O10) were synthesized by precipitation method. The oxidation of cyclohexane hydrogen peroxide was used as a probe reaction to investigate the influence of catalyst, the sorts and amounts of solvent, catalyst dosage, oxidant dosage, the reaction temperature and time and propose the oxidation mechanism. The results showed that Cu2P2O7 was exhibited the highest catalytic activity, using 10 mL of acetonitrile, 8 mmol of cyclohexane, 0.0300 g of Cu2P2O7 catalyst, 3.00 mL of w (H2O2)=30% hydrogen peroxide at temperature of 65 ℃ for 10 h, the cyclohexane conversion was 54. 1%, the cyclohexanol and cyclohexanone yield were 21.3% and 32.8%, respectively.