由六氯环三磷腈(HCCP)与5,6二甲基苯并咪唑(DBM)反应合成了具有星型结构的咪唑衍生物DBCP.采用傅里叶变换红外光谱(FT-IR)、核磁共振氢谱(1H-NMR)和磷谱(31P-NMR)及飞行时间质谱(TOF-MS)对DBCP的化学结构进行了表征.以DBCP为促进剂加入到甲基六氢邻苯二甲酸酐(MeHHPA)固化的双酚A型环氧树脂(DGEBA)体系中,用示差扫描量热法(DSC)和旋转流变仪分别研究DBCP促进体系的固化行为与室温储存稳定性.结果显示,DBCP促进体系的表观活化能较低(68.82 kJ/mol),200℃下具有明显的固化放热峰,160℃下2 min 36s能够快速完成固化,且具有大于30 d的室温储存稳定性,表明DBCP具有加快固化反应速率,降低固化温度的效果,是一种能够长期潜伏,快速固化的环氧热潜伏性固化促进剂.动态热机械分析(DMA)、热重分析(TG)和冲击试验结果表明,DBCP促进体系具有良好的热性能和力学性能.
Synthesis and performance study of a novel imidazole thermal latent curing accelerator
The imidazole derivative(DBCP)with a star structure was synthesized by the reaction of hexachlorocyclotriphosphazene(HCCP)with 5,6 dimethylbenzimidazole(DBM).The chemical structure of DBCP was characterized by FT-IR,1H NMR,31P NMR,and TOF-MS.Adding DBCP as a promoter to the bisphenol A epoxy resin(DGEBA)system cured by MeHHPA,the curing behavior and room temperature storage stability of the promoted system by DBCP were studied by DSC and rotational rheometer,respectively.The re-sults showed that the activation energy of the promoted system by DBCP was low(68.82 kJ/mol)and the obvious curing exothermic peak appeared below 200 ℃.The promoted system could be cured in 2 min 36 s at 160 ℃,and had room temperature storage stability greater than 30 d.The results above indicated that the DBCP could accelerate the curing reaction rate and reduce the curing temperature and was an epoxy thermal latent curing accelerator that could be latent for a long time and cured quickly.The results of DMA,TG and impact test showed that the promoted system by DBCP had a good thermal and mechanical performance.
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