间氨基苯乙炔/苯酚型苯并恶嗪的合成研究  

Study on the synthesis of 3-phenylacetylene-3,4-dihydro-2H-1,3-benzoxazine

作　　者：李建川[1] 冉起超[1] 朱蓉琪[1] 顾宜[1] 

机构地区：[1]四川大学高分子科学与工程学院高分子材料工程国家重点实验室,四川成都610065

出　　处：《热固性树脂》2017年第3期1-5,18,共6页Thermosetting Resin

基　　金：国家自然科学基金资助项目(21174093)资助

摘　　要：以苯酚、多聚甲醛、间氨基苯乙炔为起始原料,通过三嗪路线、伯胺路线合成了3-苯乙炔-3,4-2H-1,3苯并恶嗪(PH-apa)。通过示差扫描量热分析、热失重分析、元素分析、高效液相色谱、傅里叶红外光谱和核磁共振氢谱研究了伯胺路线中溶剂以及温度对反应的影响。结果表明:间氨基苯乙炔型三嗪不与苯酚及甲醛进一步反应。采用伯胺路线时无溶剂工艺反应剧烈,所得产物组成复杂,而溶液工艺中溶剂的极性越低,反应温度越高,越有利于PH-apa的生成。The 3 -phenylacetylene -3,4 -dihydro -2H - 1,3 -benzoxazine （PH -apa） monomer was synthesized using the phenol, paraformaldehyde and 3-aminophenylacetylene as raw materials by triazine route and primary amine route. The effects of solvent and temperature on the reaction by primary amine route were investigated using DSC,TGA, EA,HPLC,FTIR and 1H-NMR. The results showed that the 3-aminophenylacetylene-based triazine could not continue to react with phenol and paraformaldehyde. The solventless reaction process of primary amine route was intense and the product composition was complicated. The lower polarity of the solvent and higher reaction temperature were more favorable to the formation of PH-apa under the solvent reaction process.

关 键 词：含炔基苯并恶嗪 三嗪 合成 伯胺路线 高效液相色谱 

分 类 号：TQ323.1[化学工程—合成树脂塑料工业]