A new polyoxometalate (CPFXβ’HCl) 3 H 4 SiW 12 O 40 β’10H 2 O was prepared from ciprofloxacin hydrochloride and H 4 SiW 12 O 40 β’nH 2 O in aqueous solution, and characterized by elemental analysis, IR spectra and DTA-TG-DTG techniques. The IR spectrum confirmed the presence of Keggin structure and the characteristic functional group for ciprofloxacin in the compound. The TG-DTA-DTG curves showed that its thermal decomposition was a four-step process consisting of simultaneous collapse of Keggin type structure. The residue of decomposition was the mixture of WO 3 and SiO 2 , confirmed by X-ray diffraction and IR spectroscopy. The decomposition mechanism and nonisothermal kinetic parameters of the polyoxometalate were obtained from an analysis to the TG-DTG curves by the single scanning methods (the Achar method and Coats-Redfern method) and the multiple scanning methods (the Kissinger method, Flynn-Wall-Ozawa method and Starink method). The results indicate that the kinetic equations with parameters describing the thermal decomposition reaction are 10495.5 6 2 3 d 6.65 10 [3(1 ) ]e d T t Ξ± Ξ± Γ -οΌ with EοΌ87.26 kJ/mol and AοΌ6.65Γ10 6 s -1 for the second step, 18770.7 9 οΌ with EοΌ739.78 kJ/mol and AοΌ9.77Γ10 43 s -1 for the fourth step.