螺环原碳酸酯的预聚物与环氧树脂的共聚研究

SYNTHESIS OF PREPOLYMER CONTAINING SPIRO ORTHOCARBONATE AND ITS COPOLYMERIZATION WITH EPOXY RESIN

利用苯乙醛与甲醛之间的坎尼扎罗反应 ,合成新的三元醇 :2 苯基 2 羟甲基丙二醇 ,进而合成新的螺环化合物 :3 ,9 二羟甲基 3′,9′ 二苯基 1,5 ,7,11 四氧杂螺环 [5 ,5 ]十一烷。通过红外光谱、核磁共振氢谱和元素分析证实了它的结构。在三氟化硼单乙胺络合物的催化作用下 ,该化合物能够进行阳离子双开环聚合反应。用膨胀计法跟踪测试了在聚合反应过程中它的体积膨胀率约为 3 .8%。合成了它与 MDI反应生成的预聚物 ,研究了该预聚物与环氧树脂共聚固化反应 ,对共聚过程中的反应历程作了初步探讨。

The synthesis of a new spiro orthocarbonate 3,9 dihydroxymethyl 3′,9′ diphenyl 1,5,7,11 tetraoxaspiro[5,5] undecane was reviewed. Its prepolymer with 4,4′ diphenyl methane isocyanate(MDI) was prepared. Their structures were confirmed by proton NMR and IR data. And its expansion rate was determined by dilatometer. The curing reactions of epoxy resin with or without the prepolymer were followed by differential scanning calometer and IR spectroscopy. It was found that DSC curves is shifted to a higher position when the prepolymer is added. It is also indicated that conversion of epoxy group increases as the content of spiro orthocarbonate in epoxy resin system increases by IR spectroscopy. The mechanism of curing reaction was discussed.