新型咪唑类热潜伏型固化促进剂的合成及性能研究  

Synthesis and performance study of a novel imidazole thermal latent curing accelerator

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作  者:刘华 潘大伟 刘坐镇 LIU Hua;PAN Da-wei;LIU Zuo-zhen(Sino Polymer Co.,Ltd.,of ECUST Shanghai Engineering Research Center of New Anticorrosion Material,Shanghai 200237,China.;College of Materials Science and Engineering,East China University of Science and Technology,Shanghai 200237,China.)

机构地区:[1]华东理工大学华昌聚合物有限公司,上海防腐蚀新材料工程技术研究中心,上海200237 [2]华东理工大学材料科学与工程学院,上海200237

出  处:《热固性树脂》2024年第2期7-14,共8页Thermosetting Resin

基  金:国家重点研发计划项目(2022YFB3709201);上海市科技计划项目(20511107302)。

摘  要: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 min36 s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。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,~(31)P 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 results 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.

关 键 词:环氧树脂 固化促进剂 热潜伏 咪唑 合成 

分 类 号:TQ323.5[化学工程—合成树脂塑料工业]

 

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