The polyoxometalate (CPFX-HCl)3H3PW12O40·8H2O was prepared and characterized by elemental analysis, IR spectra and TG-DTA-DTG. The thermal decomposition mechanism and non-isothermal kinetic parameters of the polyoxometalate were obtained from the analysis of TG-DTG data using the Achar equation, Coats-Redfern equation (CR), Madhusudanan-Krishnan-Ninan equation (MKN) and Horowitz-Metzger equation (HM). And their mathematical expressions of the kinetic compensation effect were also calculated.