引用本文:
刘茜, 姜敏, 周光远, 张强, 叶冲, 敖玉辉. 直接酯化法合成聚2,5-呋喃二甲酸乙二酯[J]. 应用化学,
2012, 29(7): 751-756.
doi:
10.3724/SP.J.1095.2012.00348
Citation: LIU Qian, JIANG Min, ZHOU Guangyuan, ZHANG Qiang, YE Chong, AO Yuhui. Synthesis of Poly(ethylene 2, 5-furandicarboxylate) via Direct Esterification Method[J]. Chinese Journal of Applied Chemistry, 2012, 29(7): 751-756. doi: 10.3724/SP.J.1095.2012.00348
Citation: LIU Qian, JIANG Min, ZHOU Guangyuan, ZHANG Qiang, YE Chong, AO Yuhui. Synthesis of Poly(ethylene 2, 5-furandicarboxylate) via Direct Esterification Method[J]. Chinese Journal of Applied Chemistry, 2012, 29(7): 751-756. doi: 10.3724/SP.J.1095.2012.00348
直接酯化法合成聚2,5-呋喃二甲酸乙二酯
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。
English
Synthesis of Poly(ethylene 2, 5-furandicarboxylate) via Direct Esterification Method
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.
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