N-[3-perfluorohexylsuflonamido)propyl] -N,N,N-trimethyl ammoniuim iodide [I] was prepared by amidation from perfluorohexylsulphonyl fluoride [II] and N,N-dimethyl-1,3-propane diamine [III], then quaternization with methyl iodide [IV], and was characterized by IR, 1H NMR, and MS. The surface tension (γ) and critical micelle concentration (CMC) of aqueous solutions of I were investigated. The optimal process conditions of amidation: n(II)：n[III]＝1:1.2, the reactants agitated at room temperature for 3h in EtOAc and in the presence of N(Et)3. the reaction temperature to give C6F13SO2NHC3H6N(CH3)2 [V] in the yield of 90.9%. The optimal process conditions of quaternization: n[V] : n(IV)＝1:1.7, V and IV reacted at room temperature for 2h in CCl4 to give I in the yield of 97.6 %. The CMC of aqueous solution of I is 3.50 mmol/L and its γCMC is 17.8 mN/m which show excellent performance of surface activity of I.