降冰片烯酰亚胺型双苯并嗪的合成及性能

Preparation and properties of norbornene-imide-functionalized bis-benzoxazine

首先用降冰片烯二酸酐、对氨基苯酚为原料合成降冰片烯酰亚胺(NI),然后用合成的NI、4,4-二氨基二苯醚(ODA)和多聚甲醛为原料进行Mannich反应合成出降冰片烯酰亚胺型双苯并嗪(NI-BOZ),经高温固化后形成热固性树脂。用FTIR、1H NMR、13C NMR分析了NI和NI-BOZ的化学结构,证实了所得的目标产物;用DSC对NI-BOZ的固化动力学进行研究;用DMA和TGA分析了NI-BOZ的固化物的热性能。结果表明:NI-BOZ的固化反应活化能为86.27 k J·mol-1,反应级数为0.91;poly(NI-BOZ)树脂空气条件下的玻璃化转变温度为215℃,氮气条件下失重5%的温度为445℃,失重10%的温度为467℃,在800℃的残碳率为63%。

Norbornene imide（NI）, which was prepared from carbic anhydride and p-aminophenol, together with 4,4-2 amino diphenyl ether（ODA） and paraformaldehyde, was used to synthesize norbornene-imidefunctionalized benzoxazine（NI-BOZ） via Mannich reaction. A novel thermosetting resin was obtained from high temperature curing of NI-BOZ. Structure of NI and NI-BOZ were characterized by FTIR, 1H NMR and 13 C NMR. Curing kinetics of NI-BOZ was monitored by DSC and thermal properties of poly（NI-BOZ） were evaluated by DMA and TGA. The results showed that the activation energy of NI-BOZ thermal curing was 86.27 k J·mol-1 and the reaction order was 0.91. Poly（NI-BOZ） had glass transition temperature（Tg） of 215℃ in air environment. The polymer had 5% mass loss at 445℃, 10% mass loss at 467℃ and 63% char yield at 800℃ under nitrogen.