Thermal activation of clayzic catalyst has been thoroughly investigated by calcining anhydrous ZnCl2 impregnated on Mont-K10 with different ZnCl2 loadings (0.5-2.0 mmol g(-)1) under static or flowing air at 270 degreesC and also under N-2 flow at different temperatures (150-400 degreesC). Depending upon the ZnCl2 loading and calcination temperatures, an appreciable amount of HCl is evolved in the thermal activation, indicating an occurrence of reaction between the ZnCl2 and the surface hydroxyl groups of the clay (- OH + ZnCl2--> - O - Zn - Cl + HCl), leading to formation of new Lewis acid sites (- O - Zn -Cl). The Cl/Zn ratio, surface area and catalytic activity (in the benzene benzylation by benzyl chloride at 80 degreesC) of the clayzic formed in the thermal activation are influenced markedly by the ZnCl2 loading and calcination conditions (temperature and gas atmosphere). The maximum catalytic activity for the clayzic is observed at the optimum ZnCl2 loading (about 1.0 mmol g(-1)) and calcination temperature (about 270 degreesC). The thermal activation at 270 degreesC under flowing N-2 led to a most active clayzic catalyst for the benzene benzylation. A temperature-programmed evolution of HCl in the calcination of ZnCl2/Mont-K10 with different ZnCl2 loadings from 25 to 400 degreesC at a linear heating rate of 2 degreesC min(-1) has also been investigated.