由苧烯合成脂环族双环氧化合物及固化物热性能

Synthesis of a bifunctional cycloaliphatic epoxy compound from natural limonene and thermal properties of the cured products

摘要:

以天然产物(R)-(+)-苧烯为原料，通过烯烃加氢烷基化、酯化和有机过氧化物环氧化反应合成得到含有苧烯结构单元的新型双官能团脂环族环氧化合物。利用核磁共振谱（1H NMR和13C NMR）、质谱和红外光谱（FTIR）来表征反应中间体和脂环族环氧化合物结构。以2-乙基-4-甲基咪唑为促进剂、酸酐为固化剂，采用示差扫描量热（DSC）和热重分析（TGA）方法研究该脂环族环氧固化物的热性能。环氧化合物与甲基六氢邻苯二甲酸酐、4-环己烯-1,2-二甲酸酐和内亚甲基邻苯二甲酸酐固化产物的Tg分别为158℃、137℃、150℃。结果表明，脂环族环氧化合物与酸酐固化剂热固化后得到的交联聚合物具有良好的热性能。

Abstract:

A bifunctional cycloaliphatic limonene based epoxy compound was prepared from natural D-limonene via hydroalkylation, esterification and epoxidation reaction. The structures of the intermediates and epoxy compound were characterized by 1H and 13C nuclear magnetic resonance (NMR)，MS and Fourier transform infrared (FTIR). The thermal properties of the epoxy compound cured with anhydride agents were investigated using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The glass transition temperature (Tg) of the epoxy compound cured with methylhexahydrophthalic anhydride，tetrahydrophthalic anhydride and nadic anhydride was 158 oC, 137 oC and 150 oC, respectively. The results indicated that the cured epoxy exhibited good thermal properties.