The 0.4mol•L-1CuSO4 liquor and 5mol•L-1NaOH liquor were prepared by CuSO4•5H2O and NaOH as raw materials. The Cu2O powders were prepared by dextrose reducer and PVP dispersant. The DTA-TG-DTG curves obtaining is by SDT 2960 Simultaneous DSC-TGA analysis apparatus. The mensuration condition that rise temperature velocity was 15°C•min-1 and reduction reaction gas was N2 and H2 admixture gas. The kinetics was analysed by DTA-TG-DTG curves. The result indicate that form of CuO was sphericity，the CuO granularity was about 100、200、1000nm. The apparent activation energy leave each other 165.24、247.65、327.01 KJ•mol-1, increase with granularity Cu2O. The frequency gene leave each other 1.22×1016、2.84×1022、1.41×1030, increase with granularity Cu2O. The reaction progression leave each other 1.20、1.12、1.05, decrease with granularity Cu2O.