酯交换-熔融缩聚法合成PEF工艺及性能研究  

Study on process and properties of poly(ethylene 2,5-furandicarboxylate)synthesized by transesterification melt polycondensation method

作　　者：王树霞 戴钧明 黄洛玮 王玉合 司虎 Wang Shuxia;Dai Junming;Huang Luowei;Wang Yuhe;Si Hu(Research Institute of Sinopec Yizheng Chemical Fibre Co.,Ltd.,Yizheng Jiangsu 211900,China;Jiangsu Key Laboratory of High Performance Fiber,Yizheng Jiangsu 211900,China)

机构地区：[1]中国石化仪征化纤有限责任公司研究院,江苏仪征211900 [2]江苏省高性能纤维重点实验室,江苏仪征211900

出　　处：《合成技术及应用》2021年第1期1-5,共5页Synthetic Technology & Application

摘　　要：以2,5-呋喃二甲酸二甲酯(DMFD)和乙二醇为原料,通过酯交换-熔融缩聚法合成了聚呋喃二甲酸乙二醇酯(PEF),研究了催化剂用量、酯交换温度及缩聚温度对反应速率的影响,利用红外(FTIR)和核磁(NMR)对合成的PEF结构进行了表征,并对合成的PEF进行了差示扫描量热(DSC)和热失重(TGA)测试。研究结果表明,酯交换催化剂添加量为300~500μg/g时,酯交换反应速度随催化剂添加量增加而呈线性增长,当添加量超过500μg/g时,反应速度不再增加;酯交换反应温度为160~210℃时,酯交换反应速率随升温速率增加而加快;缩聚温度为245~255℃时,分子量随缩聚温度升高呈快速增长趋势。缩聚产物的红外和核磁表征结果显示,得到了预期的目标产物。合成的PEF玻璃化转变温度为88.97℃,起始热分解温度为396.52℃。Poly(ethylene 2,5-furandicarboxylate)(PEF)was synthesized with dimethyl furan dicarboxylate and ethylene glycol(EG)through transesterification-polycondensation routine.The effects of the amount of catalyst,transesterification temperature and polycondensation temperature on the reaction rate were studied.The structure and properties of PEF were characterized by infrared spectrum(FTIR),nuclear magnetic resonance(NMR),differential scanning calorimeter(DSC)and themogravimetric analysis(TGA).The results showed that the transesterification reaction rate was raised linearly with the increase of transesterification catalyst when the amount of catalyst was 300~500μg/g,and the reaction rate stopped raising when catalyst was over 500μg/g.The transesterification reaction began from 160℃to 210℃,the reaction rate was raised with the increase of heating rate.The molecular weight increased rapidly with the polycondensation temperature under 245℃to 255℃.The determination results showed that the expected PEF was obtained,which glass transition temperature was 88.97℃and onset thermal decomposition temperature was 396.52℃.

关 键 词：聚呋喃二甲酸乙二醇酯 酯交换-熔融缩聚法 工艺 性能 

分 类 号：TQ322[化学工程—合成树脂塑料工业]