A novel methylacryloyloxyl-ethyl perfluorooctanoate(MAEF) monomer was prepared via a two-step reaction with perfluorooctanoic acid as a starting material. The main influencing factors in each reaction were stuided with an orthogonal design of experiment,and the optimal reaction conditions of acylchloridization were n(PFOA)∶n(SOCl_(2)) being 1∶2,the dosage of catalyst 3.2%(relative to mass percent of PFOA),reaction(temperature) 70~75 ℃,reaction time 2 h.The average yield was 97.1%.For the esterification,the optimal reaction conditions were that n(HEMA)∶n(PFOC) was 1∶1,PFOC addition time 2 h,reaction temperature 60~(62 ℃),(reaction) time 11 h,and the average yield was 75.2%.The products were characterized by(elemental) analysis and FTIR.