一种含全氟壬烯基硅表面活性剂的制备

Preparation and Surface Activity of a Silicon Surfactant Containing Perfluorononenyl

研究了2-甲基-2-全氟壬烯氧基乙氧基羰基乙基甲基二聚乙氧基硅烷(Ⅴ)的制备方法和表面活性。以甲基丙烯酸-2-全氟壬烯氧基乙基酯(Ⅰ)和甲基二氯硅烷(Ⅱ)为原料,在氯铂酸催化下经过硅氢化反应得到2-甲基-2-全氟壬烯氧基乙氧基羰基乙基甲基二氯硅烷(Ⅲ),Ⅲ与聚乙二醇(Ⅳ)缩合反应得到非离子表面活性剂Ⅴ。用FTIR和MS对其结构进行了表征,优化了硅氢化反应工艺条件,测试了Ⅴ水溶液的表面张力和临界胶束浓度(CMC)。中间体Ⅲ的较优合成条件为:以四氢呋喃为溶剂,n(Ⅰ)∶n(Ⅱ)=1∶1.2,50℃下反应24 h,收率68.0%。表面活性剂Ⅴ水溶液的临界胶束质量浓度为0.22 g/L,此时的表面张力为19.5 mN/m,表明Ⅴ是高活性氟硅表面活性剂。

The preparation of 2-methyl-2-perfluorononenyloxyethoxycarbonyl ethyl-methyldipolyethoxyMlicane （V） and its surface activity were investigated. 2-Methyl-2-perfluorononenyloxyethoxycarbonyl ethyl methyldichlorosilicane （ III ） was synthesized from 2-perfluorononenyloxyethyl methacrylate （ I ） and methyldichlorosilicane（II） by hydrosilication in the presence of H2PtC16. 111 reacted with polyglycol （ IV ） to give non-ionic surfactant V, which was characterized by means of FTIR and MS. Its surface activities were investigated. The critical micelle concentration（CMC） of the aqueous solution of V was 0.22 g/L, the surface tension at CMC （3/CMC） was 19.5 mN/m. The reaction conditions of hydrosilication were optimized. When n（ I ）：n（ II ） = 1：1.2, I and II reacted in THF at 50 ℃ in the presence of 0.002% H2PtC16 for 24 h to give HI with a yield of 68.0%. V is a fluorosilicone surfaetant with high activity.