Charge-Transfer Complex α-TBA5 [ SiW11 O39 Al-(H2O) ]·xH2O were synthesized by solid phase reaction in room temprature and was characterized by elementary analysis IR,TG-DTA,X-ray diffraction. The results indicate that heteropoly anion still remains Keggin structure in supennolecular compounds. The non-isothermal kinetic were investigated with the Used Coats-Redfern integral method,and Achar-Brindley-Sharp-Wendworth differential method. The mechanism function, kinetic parameters,apparent activation energy E and preexponential factor InA of the thermal decomposition were obtained.