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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

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【作者】 史鸿鑫钟佳琪沈海民武宏科项菊萍

【Author】 SHI Hong-xin;ZHONG Jia-qi;SHEN Hai-min;WU Hong-ke;XIANG Ju-ping;State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology,Zhejiang University of Technology;

【机构】 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

【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。

【Abstract】 The preparation of 2-methyl-2-perfluorononenyloxyethoxycarbonyl ethyl-methyldipolyethoxylsilicane(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 H2PtCl6.Ⅲ 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(γCMC) 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% H2PtCl6for 24 h to give Ⅲ with a yield of 68.0%.Ⅴ is a fluorosilicone surfactant with high activity.

【基金】 浙江省科技厅资助项目(2011R09002-10)~~
  • 【分类号】TQ423.2
  • 【被引频次】4
  • 【下载频次】190
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