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
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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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