The spent silicon contact mass is the mixture of unreacted silicon powder and spent catalyst, as the activity of contact is reduced when the reaction proceeds. Since the reaction of Rochow that synthesize the organic silicon monomer, so the silicone industry can be rapidly developed, at the same time, large amounts of spent silicon contact mass was produced. For the effective recycling of resources and prevention of environmental pollution, we use the method of acid leaching to handle the spent silicon contact mass. Firstly, 10g spent silicon contact mass was oxidized by 27ω% H2O2 and acid leached by 1mol/L HCl to the obtain CuCl2 from the Cu catalyst. The optimum reaction situations (H2O2 : 2mL, HCl : 11mL, reaction time : 3h, total volume of the solution : 30mL) were determined by the orthogonal experimental method .The best order of each factor for the experimental impact are as follows: Volume of H2O2, Total volume of the solution, Volume of HCl, Reaction time. 98% of the copper were recycled to prepare the related catalyst. Finally the carbon was removed by sodium tungstate solution (density 1.30g/mL) to get high-purity silicon (99%) according to the different density of different substance. And then, we prepared nano-CuO and nano-Cu2O by the recovered copper chloride, and characterized the structure and morphology of copper oxide nanoparticles and cuprous oxide nanoparticles by XRD, SEM, BET, TGA，IR. The catalytic effect of CuO was measured by Hydrogen peroxide decomposition rate and the catalytic effect of Cu2O measured by Photocatalytic decomposition of methyl orange, the catalytic effect compared with commercial CuO and CuO prepared by commercial CuCl2, as the same of Cu2O. The results show that the catalytic effect of CuO prepared by recycled CuCl2 and CuO prepared by commercial CuCl2 is the same, and their catalytic effect were far superior to the CuO. The catalytic effect of Cu2O is all so like that.