Abstract: After treating by reductant and inorganic acid, the clays were coagulated with natural latex to prepare natural rubber-clay composites. The composites were studied in different decomposition temperatures by using in-situ FTIR. In lower decomposition temperature, the decomposing gaseous products of the composites mainly were ethylene, lower molecular weight olefin and carbonyl compounds. With the increase of degradation temperature, the contents of lower molecular weight olefin reduce and more higher molecular weight olefin and alkyl compounds form. Furthermore, with the increase of the contents of the metal component in the clay, such as Co, Mn, Cu and Fe, the decomposing gaseous products contain more olefin and carbonyl compounds as well as CO₂. The metal components in the clay accelerate the oxidative degradation of natural rubber/clay composites.