Microwave-assisted esterification step of poly(ethylene terephthalate) (PET) synthesis through ethylene glycol and terephthalic acid

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 (...

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Bibliographic Details
Published in:Polymer bulletin (Berlin, Germany) Germany), 2019-06, Vol.76 (6), p.2931-2944
Main Authors: Espinosa-López, Ana Christy, Ávila-Orta, Carlos Alberto, Medellín-Rodríguez, Francisco Javier, González-Morones, Pablo, Gallardo-Vega, Carlos Alberto, De León-Martínez, Patricia Adriana, Navarro-Rosales, Maribel, Valdez-Garza, Janett Anaid
Format: Article
Language:English
Subjects:
Acids
Characterization and Evaluation of Materials
Chemistry
Chemistry and Materials Science
Complex Fluids and Microfluidics
Esterification
Ethylene glycol
Fourier transforms
Gel chromatography
Microwaves
Molecular weight
NMR
Nuclear magnetic resonance
Organic Chemistry
Original Paper
Physical Chemistry
Polyesters
Polyethylene terephthalate
Polymer Sciences
Polymerization
Positron emission
Radiation
Reaction products
Soft and Granular Matter
Spectrum analysis
Temperature
Temperature effects
Terephthalic acid
Thermodynamic properties
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Summary: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 ( M ¯ n ) were determined. The reaction products were then identified using Fourier transform infrared spectroscopy and proton nuclear magnetic resonance ( 1 H 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, 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 M ¯ n , as an indication of the variation of the solubility of TPA in the reaction mixture.
ISSN:0170-0839
1436-2449
DOI:10.1007/s00289-018-2521-9