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以含氢硅油(PMHS)、N-甲基-N-烯丙基-2-全氟-2-甲基-3-氧代己酰胺(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);考察了温度、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∶9,2.5 g含氢硅油,120μL Karstedt催化剂(16.123 g Pt/L),80℃反应6 h,在该条件下转化率为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)均逐渐减小;PF2DI水溶液的γCMC和在有机玻璃板及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PF2DI水溶液润湿性能最佳。
Hydrogen silicone oil (PMHS), N-methyl-N-allyl-2-perfluoro-2-methyl-3-oxohexanamide (NF2), N, N-dimethylallylamine (DAEMA ) Was used as raw material to prepare fluorosilicone cationic surfactant (PF2DI) by hydrosilylation reaction and then quaternization reaction with CH3I under the action of Karstedt catalyst. The influences of temperature, catalyst and reactant ratio on the hydrosilylation reaction The structure of the product was characterized by IR and 19F NMR. The product molecular weight, cation active content, solubility, surface tension and wettability were determined. The optimum hydrosilylation conditions were as follows: n (Si-H): n (NF2): n (DAEMA) = 10:1:9,2.5 g hydrosilicone oil, 120μL Karstedt catalyst (16.123 g Pt / L) The reaction for 6 h, under the conditions of conversion was 58%. The weight average molecular weight Mw and number average molecular weight Mn, cationic active content of PF2DI, when n (Si-H): n (NF2): n (DAEMA) varied from 10: 0.5: 9.5 to 10: The solubility and critical micelle concentration (CMC) in water and ethanol decreased gradually. The contact angle of γCMC in PF2DI aqueous solution and the surface of plexiglass plate and paraffin decreased first and then increased. When n (Si-H): n (NF2): n (DAEMA) = 10: 1: 9, the three reached the minimum, at this time PF2DI aqueous solution best wettability.