Abstract: The effect of HF treatment on etherification activities of ZSM-5 zeolite was investigated. Appearance, crystal structure, pore structure, acid quality of treated zeolite was charactered. It was found that catalyst treated by HF remained typical MFI structure, but grain broken; pore volume and average pore diameter of treated zeolite increased obviously; Bronsted acid quantity decreased; etherification activities of fluorinate treatment of ZSM-5 zeolite increased obviously.