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

作　　者：史鸿鑫[1] 王正轩[1] 武宏科[1] 项菊萍[1] 陈立军[1] 沈海民[1] 

机构地区：[1]浙江工业大学化学工程与材料科学学院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》2013年第7期789-792,824,共5页Fine Chemicals

基　　金：浙江省科技厅资助项目(2011R09002-10)~~

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°。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°.

关 键 词：含氟丙烯酸酯 酰胺化 乳液聚合 接触角 

分 类 号：TQ316.334[化学工程—高聚物工业] TQ323.7