氟硅阳离子表面活性剂的制备及性能

Synthesis and Properties of Fluoro-silicone Surfactant

摘要:

以含氢硅油（PMHS）、N-甲基-N-烯丙基-2-全氟-2ʹ-甲基-3ʹ-氧代己酰胺(NF2) (NF2)、N,N-二甲基烯丙胺（DAEMA）为原料，在 Karstedt催化剂作用下，经硅氢化反应后，再与CH3I进行季铵化反应，制备了氟硅阳离子表面活性剂PF2DI；研究了温度、催化剂、反应物比例对硅氢化反应的影响，采用IR和19FNMR对产物结构进行了表征，并测定了产物分子量、阳离子活性物含量、溶解度、表面张力和润湿性能。得到较优硅氢化反应条件：n（Si—H）: n（NF2）: n（DAEMA）=10:1:9，2.5g 含氢硅油，120μL Karstedt催化剂（16.123 g Pt/L），80℃反应6 h，转化率为58%。当n（Si—H）: n（NF2）: n（DAEMA）从10:0.5:9.5到10:2:8变化时，PF2DI的重均分子量MW和数均分子量Mn、阳离子活性物含量、在水和乙醇中溶解度、临界胶束浓度CMC逐渐减小；PF2DI水溶液的γCMC和在有机玻璃板和石蜡表面的接触角都先减小再增大；当n（Si—H）: n（NF2）: n（DAEMA）=10:1:9时，三者均达到最小值，此时润湿性能最佳。

Abstract:

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.