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作 者:史鸿鑫[1] 钟佳琪[1] 沈海民[1] 武宏科[1] 项菊萍[1]
机构地区:[1]浙江工业大学绿色化学合成技术国家重点实验室培育基地,浙江杭州310032
出 处:《精细化工》2014年第3期317-320,共4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.
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