采用来源于可再生资源的愈创木酚、癸二胺和多聚甲醛等为原料合成了愈创木酚-癸二胺型苯并噁嗪单体(G-d),通过红外光谱、凝胶渗透色谱、核磁共振氢谱证明了其分子结构。差热扫描分析和热重分析测试结果表明,其树脂的起始固化温度为225℃,峰值固化温度为246℃。通过热固化工艺得到自固化产物PG-d,并研究其热固化行为、动态力学性能和热分解行为,PG-d的玻璃化转变温度为98.9℃,800℃残碳率为22%。此外,通过基于愈创木酚的苯并噁嗪G-d与传统双酚A-苯胺型苯并噁嗪(B-a)按照不同的比例共混形成二元共混体系。当G-d含量为10%时,G-d/B-a体系固化物的冲击强度是B-a均聚体系固化物的3倍以上,表明G-d中的柔性长链结构可有效改善共聚体系固化物的韧性。
The benzoxazine(G-d) was synthesised by using guaiacol (renewable phenolic compound),1,10-diaminodecane and p-formaldehyde,and confirmed the structure and purity of the monomer by fourier transform infrared spectroscopy(FT-IR),gel permeation chromatography(GPC) and nuclear magnetic resonance spectroscopy(NMR).Data obtained from differential thermal scanning(DSC),thermal gravimetric analysis(TGA) shown that the curing initiation temperature of G-d was 225℃ and the peak maximum at 246℃.The G-d polybenzoxazine was prepared by conventional thermal curing process,and its curing behaviour,dynamic mechanical properties and thermal decomposition behavior were studied,which indicated that the glass transition temperature of G-d was 98.9℃ and the char yield of 22% at 800℃.Moreover,this guaiacol based benzoxazine was blended in varying proportions with conventional bisphenol A based benzoxazine (B-a) as G-d/B-a binary system.The impact strength of G-d/B-a after curing attained three times as B-a polybenzoxazine when the content of G-d was 10%,which indicated that the flexible long-chain in G-d improved toughness in co-curing resins.
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基金资助
国家自然科学基金资助项目(51573009);广东省光信息材料与技术重点实验室(2017B030301007)