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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 and surface activity of 2-methyl-2-perfluoro-nonenoxyethoxycarbonylethylmethyldimethoxysilane (V) were studied. Using 2-perfluoro nonyloxyethyl methacrylate (I) and methyldichlorosilane (II) as starting materials, the reaction of 2-methyl-2- Fluorononyloxyethoxycarbonylethylmethyldichlorosilane (Ⅲ), Ⅲ and polyethylene glycol (Ⅳ) condensation reaction to obtain a nonionic surfactant Ⅴ. Its structure was characterized by FTIR and MS, the conditions of hydrosilylation reaction were optimized, and the surface tension and critical micelle concentration (CMC) of Ⅴ aqueous solution were tested. The optimum conditions for the synthesis of intermediate Ⅲ were as follows: tetrahydrofuran (n = 1): n (Ⅱ) = 1: 1.2 at 50 ℃ for 24 h, yield 68.0%. The critical micelle mass concentration of the aqueous solution of surfactant V was 0.22 g / L, and the surface tension at this time was 19.5 mN / m, indicating that V was a highly activated fluorosilicone surfactant.