Abstract: The deactivation and regeneration of HZSM-5 catalysts in hydration process of cyclohexene to prepare cyclohexanol were investigated, combining with characterization of various catalyst samples by FT-IR, XRD, ICP-AES and N2 adsorption-desorption techniques. Results indicated that the framework structure of deactivated HZSM-5 catalyst was basically unchanged, and a little dealumination of the catalyst could not cause the serious deactivation of catalyst, thus the deposition of coke species on catalyst surface and pore channel blockage should be the main causes of catalyst deactivation. The coke species was analyzed by FT-IR, TG-DTG and GC-MS. It was shown that the coke species was mainly consisted of dicyclohexyl ether and alkene oligomers. However, the deactivated HZSM-5 catalyst could be regenerated and reactivation by suitable methods to recover its catalytic activity for reuse.