Abstract: Polyoxometalate of ciprofloxacin with 12-phosphomolybdic acid was reported and characterized with elemental analysis, IR spectrum, and TG-DTA.The IR spectrum confirmed the presence of Keggin-type anion and the characteristic functional group of ciprofloxacin.The TG-DTG curves showed that its thermal decomposition was a three-step process.The intermediates and residue of the thermal decomposition were identified by means of TG-DTG, IR, and XRD technique.The non-isothermal kinetic data were analyzed with the Achar equation, Coats-Redfern equation, Kissinger equation, Flynn-Wall-Ozawa equation and Starink equation.The mechanism function and kinetic parameters of the thermal decomposition in the third step were obtained.The chemical reaction mechanism (F3) controlled the third thermal decomposition process.The apparent activation energy and the pre-exponential factor were 351 kJ·mol-1 and 2.57×10 30s-1 respectively.