Mg-Fe and Mg-Al Hydrotalcite were prepared by the conprecipitation method. A new technique of temperature programmed calcination (TPC) is designed to investigate the thermal decomposition of the hydrotalcites. The kinetic equation of thermal decomposition ln(h/S)=lnA-Ea/RT is derived from TPC graph, and then the thermal decomposition kinetics parameters of Mg-Fe and Mg-Al hydrotalcite can be obtained. Experimental results show that this method is more definite, convenient and sensitive for characterizing the thermal decomposition process of Mg-Fe and Mg-Al Hydrotalcite. The active energy Ea of decomposition of Mg-Fe and Mg-Al hydrotalcite is about 83～48 kJ·mol-1.
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