摘要
以二乙醇胺(DEA)、丙烯酸甲酯(MA)为原料,通过Michael加成反应合成AB2单体,再以三-(2-羟乙基)异氰脲酸酯(THEIC)为核,AB2单体为支化单元,通过酯交换反应合成端羟基超支化聚异氰脲酸酯-酯(HPICE).通过单因素和正交试验优化出合成HPICE的最佳条件:即反应时间为4.5h,反应温度为115℃,n(AB2)∶n(THEIC)为3.25∶1,催化剂用量为1.5%,采用红外光谱(FI-IR)、核磁氢谱(1 H-NMR)对产物结构进行了表征,并通过热分析法对产物的热稳定性进行了表征.结果表明:反应按预期设计路线进行,且产物具有良好的热稳定性.
AB2monomer was synthesized by Michael addition of diethanolamine(DEA)and methyl acrylate(MA).And then the hydroxyl-terminated hyperbranched poly isocyanurateester(HPICE)was prepared via transesterification of three-(2-hydroxyethyl)isocyanurate(THEIC)and AB2 monomer in which THEIC was used as the core and AB2 monomer as the branching unit.The synthesis conditions were optimized by single-factor and orthogonal experiments.The optimum conditions were that the reaction time was 4.5h,the reaction temperature was 115 ℃,n(AB2)∶n(THEIC)was 3.25∶1and the dosage of catalyst was1.5%.The structure of HPICE were characterized by Fourier transform infrared spectra(FT-IR)and nuclear magnetic resonance spectra(^1 H-NMR),as well as the thermal stability analysis of the product was also characterized.The results prove that the reaction is carried out as the expected route,and the product exhibits good thermal stability.
出处
《陕西科技大学学报(自然科学版)》
2016年第5期28-33,43,共7页
Journal of Shaanxi University of Science & Technology
基金
陕西省科技厅科研创新团队计划项目(2013KCT-08)
陕西省教育厅专项科研计划项目(14JK1090)
陕西科技大学科研创新团队计划项目(TD12-04)
关键词
异氰脲酸酯
端羟基超支化聚合物
合成
表征
isocyanurate
hydroxyl-terminated hyperbranched polymers
synthesis
characterization