The thermal behavior and decomposition of kaolinite–potassium acetate intercalation complex was investigated through a combination of thermogravimetric analysis and infrared emission spectroscopy. Three main changes were observed at 48, 280, 323, and 460 °C which were attributed to (a) the loss of adsorbed water, (b) loss of the water coordinated to acetate ion in the layer of kaolinite, (c) loss of potassium acetate in the complex, and (d) water through dehydroxylation. It is proposed that the potassium acetate intercalation complex is stability except heating at above 300 °C. The infrared emission spectra clearly show the decomposition and dehydroxylation of the kaolinite intercalation complex when the temperature is raised. The dehydration of the intercalation complex is followed by the loss of intensity of the stretching vibration bands at region 3600–3200 cm−1. Dehydroxylation is followed by the decrease in intensity in the bands between 3695 and 3620 cm−1. Dehydration is completed by 400 °C and partial dehydroxylation by 650 °C. The inner hydroxyl group remained until around 700 °C.
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