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研究了2-甲基-2-全氟-2’-甲基-3’-氧代己酰氧基乙氧基羰基乙基甲基二聚氧乙烯基硅烷(Ⅴ)的制备方法和表面活性。以甲基丙烯酸-2-全氟-2’-甲基-3’-氧代己酰氧基乙基酯(Ⅰ)和甲基二氯硅烷(Ⅱ)为原料,0.5%Karsted催化剂存在下(以Ⅰ的质量计),发生硅氢化反应,得到2-甲基-2-全氟-2’-甲基-3’-氧代己酰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溶液的表面张力、临界胶束浓度(CMC)和处理玻璃后的疏水性能。以四氢呋喃为溶剂,中间体Ⅲ的较优合成条件为:n(Ⅰ)∶n(Ⅱ)=1.2∶1,50℃下反应28 h,化合物Ⅱ的转化率可达到68.2%。表面活性剂Ⅴ水溶液的CMC为0.52 g/L,临界表面张力γ_(CMC)为22.8 m N/m,用V的THF溶液处理玻璃后,玻璃表面具有很好的疏水性和较好的疏油性。
The preparation and surface activity of 2-methyl-2-perfluoro-2’-methyl-3’-oxohexanoyloxyethoxycarbonylethylmethyldipolyoxyvinylsilane (V) . Using 2-perfluoro-2’-methyl-3’-oxohexanoyloxyethyl methacrylate (I) and methyldichlorosilane (II) as raw materials, 0.5% Karsted catalyst Based on the mass of I), a hydrosilation reaction takes place to give 2-methyl-2-perfluoro-2’-methyl-3’-oxohexanoyloxyethoxycarbonylethylmethyldichlorosilane 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. The surface tension of V solution, the CMC concentration and the hydrophobic property of glass after treatment were tested. With tetrahydrofuran as solvent, the optimum conditions for the synthesis of intermediate Ⅲ are as follows: n (Ⅰ): n (Ⅱ) = 1.2:1, the conversion of compound Ⅱ can reach 68.2% at 50 ℃ for 28 h. The CMC of surfactant Ⅴ aqueous solution was 0.52 g / L and the critical surface tension γ CMC was 22.8 m N / m. The surface of glass was well hydrophobic and better oleophobic .