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含全氟壬烯基丙烯酸酯单体合成及乳液聚合
Synthesis and Polymerization of Acrylate Containing Perfluorononenyl
【摘要】 研究了含全氟壬烯基丙烯酸酯的合成及其聚合反应。以全氟壬烯氧基苯磺酰氯为原料,经酰胺化、酯化得到N-甲基-N-p-全氟壬烯氧基苯磺酰胺基乙基丙烯酸酯(Ⅲ);确定了Ⅲ的较优合成工艺条件为:n(Ⅱ)∶n(丙烯酰氯)=1∶3,室温反应6 h,含氟单体Ⅲ的收率为75.0%;并将Ⅲ与甲基丙烯酸甲酯(MMA)、丙烯酸丁酯(BA)在K2S2O8(KPS)存在下,通过半连续乳液聚合法,制备了含氟丙烯酸酯乳液。用傅里叶变换红外光谱(FTIR)、核磁共振波谱(1HNMR)、质谱(ESI-MS)等对含氟丙烯酸酯单体(Ⅲ)和聚合物乳胶膜的结构进行了表征;考察了乳液的稳定性、Ⅲ的含量对聚合物膜上水接触角的影响。当含氟丙烯酸酯占单体总质量的20%时,水接触角为88.2°。
【Abstract】 The synthesis and polymerization of acrylate containing perfluoronineyl were investigated.N-Methyl-N-p-perfluorononenoxybenzenesulfamidethyl acrylate(Ⅲ) was synthesized from p-perfluorononenyloxybenzenesulfonyl chloride by amidation and esterification.The optimum conditions of esterification were n(Ⅱ):n(acryloyl chloride)=1:3,and the reaction being carried out at room temperature for 6 h.The yield of Ⅲ was 75.0%.The fluorinated copolymer emulsion with blue-fluorescence was synthesized by semicontinuous emulsion polymerization of Ⅲ initiated by K2S2O8 with butyl acrylate(BA),methyl methacrylate(MMA).Acrylate(Ⅲ) and copolymer film were characterized by means of FTIR,1HNMR and ESI-MS respectively.The copolymer′s emulsion stability and the effect of content of Ⅲ in copolymer on the water contact angle on the copolymer film were studied.When the film contains 20% Ⅲ in weight,the water contact angle on the film is 88.2°.
【Key words】 fluorinated acrylate; amidation; emulsion polymerization; contact angle;
- 【文献出处】 精细化工 ,Fine Chemicals , 编辑部邮箱 ,2013年07期
- 【分类号】TQ316.334
- 【被引频次】2
- 【下载频次】222