Abstract
The esterification step during poly(ethylene terephthalate) (PET) polymerization was studied using ethylene glycol (EG) and terephthalic acid (TPA), together with microwave radiation in a closed system. First, the effects of temperature and molar ratio EG/TPA on the number-average molecular weight (\( \bar{M}_{n} \)) were determined. The reaction products were then identified using Fourier transform infrared spectroscopy and proton nuclear magnetic resonance (1H NMR). The molecular weight was determined through gel permeation chromatography, and the thermal behavior was obtained with differential scanning calorimetry. The PET number-average molecular weight, \( \bar{M}_{n} \), ranged between 308 and 1504 g mol−1, which were close values regarding those produced after 240–300 min under conventional heating. The reaction products were obtained after 45 min of reaction without water or EG removal. It was also determined that temperature and the molar EG/TPA ratio were correlated with \( \bar{M}_{n} \), as an indication of the variation of the solubility of TPA in the reaction mixture.
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Acknowledgements
The authors thank Consejo Nacional de Ciencia y Tecnología (CONACYT from Mexico) for the funding through Grants CB-2014-01 241960 and CB-2009 132699. The authors are also grateful to Silvia Torres Rincón (from CIQA, México), Olga Dávalos Montoya (from Autonomous University of San Luis Potosí, México) and Judith Nazaret Cabello Romero (CIQA) for their technical support and Dr. Roberto Yañez Macías (CIQA, México) for his valuable support during manuscript preparation. The support of CONACYT through Grant 294030 (LANIAUTO) is greatly appreciated.
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Espinosa-López, A.C., Ávila-Orta, C.A., Medellín-Rodríguez, F.J. et al. Microwave-assisted esterification step of poly(ethylene terephthalate) (PET) synthesis through ethylene glycol and terephthalic acid. Polym. Bull. 76, 2931–2944 (2019). https://doi.org/10.1007/s00289-018-2521-9
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DOI: https://doi.org/10.1007/s00289-018-2521-9