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直接酯化法合成聚2,5-呋喃二甲酸乙二酯

刘茜1,姜敏2,周光远2,张强2,叶冲1,熬玉辉1*   

  1. (1,长春工业大学化学与生命科学学院 长春 130022；
    2.中国科学院长春应用化学研究所,中国科学院生态环境高分子材料重点实验室 长春 130022)
  • 收稿日期:2011-08-08 修回日期:2011-09-29 出版日期:2012-07-10 发布日期:2012-07-10
  • 通讯作者: 敖玉辉，教授; Fax:0431-85956241; E-mail:aoyuhui@mail.ccut.edu.cn; 研究方向：聚合物材料改性

Synthesis of Poly(ethylene 2,5-furandicarboxylate) via Direct Esterification Method

LIU Qian1, JIANG Min2, ZHOU Guangyuan2, ZHANG Qiang2, YE Chong1, AO Yuhui1*   

  1. (1.College of Chemistry and Life Sciences,Changchun University of Technology,Changchun,130022,China；
    2.Key Laboratory of Polymer Ecomaterials,Changchun Institute of Applied Chemistry,Chinese Academy of Sciences,Changchun 130022,China)
  • Received:2011-08-08 Revised:2011-09-29 Published:2012-07-10 Online:2012-07-10
  • Contact: Yuhui ao

PDF

2309

被引次数

11

摘要： 以2,5-呋喃二甲酸(FDCA)和乙二醇(EG)为原料，草酸亚锡为催化剂，采用直接酯化法制备了聚2,5-呋喃二甲酸乙二酯(PEF)。 考察了酯化反应、酯化产物、缩聚反应及缩聚产物的影响因素，结果表明，草酸亚锡在该体系中既可催化酯化反应又可催化缩聚反应，当n(FDCA)∶n(EG)=1∶1.6、草酸亚锡摩尔分数为0.1%、酯化温度为210 ℃、缩聚温度为240 ℃、缩聚反应时间为480 min、磷酸三甲酯摩尔分数为0.03%时，酯化程度最高（酯化产物的酸值在94％以上），缩聚产物相对分子量最高（比浓粘度达到1.29 dL/g），端羧基含量最低（34.3 mol/t）；采用FTIR和1H NMR对目标产物的结构进行了表征。

关键词: 聚呋喃二甲酸乙二酯, 呋喃二甲酸, 直接酯化法, 基于可再生资源

Abstract: Poly(ethylene 2,5-furandicarboxylate)(PEF) was directly and successfully synthesized via the direct esterification method(PTA method) starting from 2,5-furandicarboxylic acid(FDCA) and ethylene glycol(EG), in which stannous oxalate was chosen as catalyst. Effect of the molar ratio of FDCA to EG(1∶12~1∶2.0), dosage of stannous octanoate(0.3×10-3~5×10-3 mol/mol FDCA), esterification temperature(180~220 ℃), polycondensation temperature(220~250 ℃) and dosage of trimethyl phosphate(1×10-4~3×10-3 mol/mol FDCA) on the esterification and polycondensation processes were studied in details. The optimized process conditions were found to be:n(FDCA)∶n(EG)=1∶1.6, stannous oxalate dosage is 1×10-3 mol/mol FDCA, polycondensation temperature is 240 ℃, polycondensation time is 480 min and trimethyl phosphate dosage is 3×10-4 mol/mol FDCA. The results of Fourier transform infrared spectroscopy(FTIR) and nuclear magnetic resonance spectroscopy(1H NMR) confirmed the expected PEF structure.

Key words: poly(ethylene furandicarboxylate), furandicarboxylic acid, direct esterification method, renewable resources

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