一种氟硅表面活性剂的合成及其表面活性  

Preparation and Surface Activity of Fluorosilicon Surfactant

作　　者：史鸿鑫[1] 莫春欢 钟佳琪[2] 沈海民[1] 武宏科[1] 

机构地区：[1]浙江工业大学化工学院,浙江杭州310032 [2]上海化工研究院,上海200062

出　　处：《精细化工》2015年第12期1364-1368,共5页Fine Chemicals

基　　金：浙江省科技厅资助项目(2011R09002-10)~~

摘　　要：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。Preparation and surface activity of 2-methyl-2-perfluoro-2＇-methyl-3＇-oxocaproyloxyl ethoxycarbonyl ethylmethyldipolyethoxylsilicane （V） were investigated. 2-Methyl-2-perfluoro-2＇- methyl-3＇-oxoeaproyloxyl ethoxycarbonyl ethylmethyldichlorosilieane （Ⅲ） was synthesized from 2- perfluoro-2＇-methyl-3＇-oxocaproyloxylethyl methacrylate （ Ⅰ ） and methyldichlorosilicane （ Ⅱ ） by hydrosilication in the presence of 0.5% Karstedt catalyst （ calculated by quality of Ⅰ ）. m reacted with polyglycol （IV） to give non-surfactant V which was characterized by FTIR and MS and its surface activities were investigated. The reaction conditions of hydrosilication in THF were optimized, n （ Ⅰ ） ： n（Ⅱ） = 1.2：1, Ⅰ and Ⅱ reacted at 50 ℃ for 28 h to give m at conversatin 68. 2% of Ⅱ.The critical micelle concentration （CMC） of aqueous solution of V was 0.52 g/L, surface tension of which at CMC （9＇cMc） was 22. 8 mN/m. Glass surface treated by V solution in THF shows excellent hydrophobic and good oilphobic performances.

关 键 词：氟硅表面活性剂 硅氢化反应 表面张力 临界胶束浓度 疏水性 表面活性剂 

分 类 号：O633.4[理学—高分子化学]