The thermal decomposition processes in solid state CoC2O4·2H2O have been studied in air using TG/DTA, DSC and XRD techniques. TG/DTA, DSC curves showed that the decomposition proceeded through two well-defined steps in air. Mass loss of the thermal decomposition of CoC2O4·2H2O was in good agreement with the theoretica1 one. XRD showed that the final product of the thermal decomposition was Co3O4. The activation energies were calculated through the ASTM E698 and Flynn-Wall-Ozawa (FWO) methods, and the possible conversion functions had been estimated through the multiple-linear regression method. The activation energies for the two steps decomposition of CoC2O4·2H2O were 140.18 kJ·mol-1 and 134.61 kJ·mol-1, respective1y.