一种氟硅表面活性剂的合成及其表面活性
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浙江省科技厅资助项目(2011R09002-10)


Preparation and Surface Activity of Fluorosilicon Surfactant
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    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,在Karstedt 催化剂存在下发生硅氢化反应,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溶液的表面张力和临界胶束浓度(CMC)和处理玻璃后的疏水性能。中间体III的较优合成条件为: 以四氢呋喃为溶剂,n (I ): n (II) = 1.2∶1,50 篊下反应28 h,转化率68.2%。表面活性剂V水溶液的CMC为0.52 g/L,此时的表面张力为22.8 mN/m,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。

    Abstract:

    Abstract: 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-oxocaproyloxyl] ethoxycarbonyl ethylmethyldichlorosilicane (III) was synthesized from 2-[perfluoro-2-methyl-3-oxocaproyloxyl] ethyl methacrylate (I)and methyldichlorosilicane (II) by hydrosilication in the presence of Karstedt catalyst. III 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 were optimized. n (I ): n (II) = 1.2∶1, I and II reacted in THF at 50℃ in the presence of 0.5% Karstedt catalyst( calculated by quality of I ) for 28h to give III at conversatin 68.2 %. The critical micelle concentration (CMC) of aqueous solution of V was 0.52 g/L, surface tension of which at CMC (γcmc) was 22.8 mN/m. Glass surface treated by THF solution of V shows excellent hydrophobic and good oilphobic performances.

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史鸿鑫,莫春欢,钟佳琪,沈海民,武宏科.一种氟硅表面活性剂的合成及其表面活性[J].精细化工,2015,32(12):

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  • 收稿日期:2015-09-01
  • 最后修改日期:2015-10-19
  • 录用日期:2015-10-23
  • 在线发布日期: 2015-12-10
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