A series of PF2DI surfactants were synthesized by the hydrosilylation with poly (methylhydro- siloxane) (PMHS),N-methyl-N-allyl-2-perfluoro-2ʹ-methyl-3ʹ-oxocaproamide (NF2) and N,N-dimethallylamine (DAEMA) and CH3I in the presence of the Karstedt catalyst and then by quaterisation with CH3I. The structures of the products were characterized by IR and 19FNMR. The effects of temperature, the catalyst dosage and the molar ratio of the reagents on the hydrosilylation were studied. The relative molecular mass, cationic-active matter content, solubility, surface tension and wettability were measured. The optimal process conditions of hydrosilylation were n (Si—H):n (NF2):n (DAEMA) =10:1:9, 2.5 g PMHS, 120 μL Karstedt catalyst (16.123 g Pt/L), 80℃ reacted for 6 h to give PF2DI in the yield of 58%. When n (Si—H):n (NF2):n (DAEMA) changed from 10:0.5:9.5 to 10:2:8, weight-average molar mass MW and number-average molar mass Mn , the content of cationic-active matter, the solubility in water and ethanol and the critical micelle concentration(CMC) decreased gradually; surface tension (γCMC) and the contact angle on the PMMA and paraffin surfaces first decreased and then increased. When n (Si—H):n (NF2):n (DAEMA) was 10:1:9, γCMC and the contact angles reached the minimum value and the wettabilities were the best.