一种螺环原碳酸酯类膨胀单体的合成与表征.pdfVIP

B020 一种螺环原碳酸酯类膨胀单体的合成与表征 1 ＊ 陈小庆 ，黄培 ，时钧 (南京工业大学化学化工学院，南京，210009) 摘 要 本文经两步法合成了一种螺环原碳酸酯类膨胀单体：3,9-二羟甲基-3′,9′-二乙基-1,5,7,11- 四氧杂螺环[5.5]十一烷．该单体在固化剂三氟化硼单乙胺催化作用下，能进行阳离子双开环聚合 反应，红外光谱（FTIR ）证实了该单体及其均聚物结构．用示差扫描量热(DSC)跟踪环氧树脂及 其与膨胀单体混合后的固化反应过程，纯环氧树脂存在两个固化反应放热峰，结果表明，膨胀单 体的加入能提高环氧基团的转化率． 关键词 合成 螺环原碳酸酯 膨胀单体 开环聚合反应 环氧树脂 SYNTHESIS AND CHARACTERIZATION OF A SPIRO ORTHOCARBONATE EXPANDING MONOMER CHEN Xiaoqing, HUANG Pei and SHI Jun (College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009, Jiangsu, China) ABSTRACT A spiro orthocarbonate expanding monomer 3 ,9–diethyl-3,9-dihydroxymethyl-1,5,7,11-tetraoxa- spiro[5.5] undecane was synthesized by two steps in this paper. Its cationic double ring-opening polymerization was carried out with BF .C H NH as catalyst. The structures of the monomer and its homopolymer were 3 2 5 2 confirmed by IR. The curing processes of epoxy resin with or without expanding monomer were traced by differential scanning calometer (DSC). It was found that DSC curves showed two peaks in the case of pure epoxy resin, but only one peak for the epoxy resin with expanding monomer. The above observed phenomena indicated that the addition of the expanding monomer into the epoxy resin enhanced the conversion of epoxy group.. Key words synthesis, spiro orthocarbonate, expanding monomer, ring-opening polymerization, epoxy resin 大多数聚合过程中会或多或少地产生体积收缩，例如广泛应用的环氧树脂，固化时体积 [1] ．由于在固化过程中，热固性树脂在凝胶化后密度的变化引起树脂体积 收缩率在 5% 以上 收缩，进而在树脂内部产生收缩应力[2] ，此应力是一种潜在的破坏因素，它很容易使材料内 部应力集中，从而导致使材料的强度降低，甚至会造成材料的开裂、尺寸不稳定等[2].为了克 联系人：黄培，phuang@njut.edu.cn. 第一作者：陈小庆，男，27 岁，硕士研究生。 [3-5] 服树脂固