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The polyoxometalate complex (CPFX·HCl)4H5BW12O40·12H2O was prepared in aqueous solution for the first time, and characterized by elemental analysis, IR spectrum, and TG-DTG. The TG-DTG curves showed that its thermal decomposition was a our-step process consisting of the simultaneous collapse of Keggin anion. The intermediate and residue of the decomposition were identified by mean of TG-DTG, IR, and XRD technique. The non-isothermal kinetic data were analyzed by the Achar method and Coats-Redf method. The apparent activation energy (E) and the pre-exponential factor (ln A) of each decomposition were obtained. The most probable thermal decomposition reaction mechanisms were proposed by comparison of the kinetic parameters. The kinetic equation for both the second stage and the third stage can be expressed as dα/dt = Ae-EIRT·(1 - α)2, and the fourth stage dα/dt = Ae-EIRT·( 1 - α). And their athematic expressions of the kinetic compensation effects of thermal decomposition reaction were also determined.