STRUCTURAL ANALYSIS OF BIS-2-HYDROXYETHYLENE TEREPHTHALATE OBTAINED FROM DEPOLYMERIZATION OF POLYETHYLENE TEREPHTHALATE

Diana Masiulionytė1, Monika Čekavičiūtė1, Laura Pečiulytė1, Joana Bendoraitienė1

1 Department of Polymer Chemistry and Technology, Kaunas University of Technology, Lithuania

[email protected]

Polyethylene terephtalate (PET) is one of the most utilized plastics for food and beverages packaging. PET does not have side effects in nature. However, there is a huge problem of increasing amount of plastic wastes in the world. Chemical recycling is one of the options to reduce PET wastes.

PET glycolysis, chemical recycling method, is a transesterification reaction. There are four main techniques of glycolysis: (i) catalyzed glycolysis; (ii) solvent-assisted glycolysis; (iii) supercritical glycolysis; (iv) microwave-assisted glycolysis. PET flakes dissolve in ethylene glycol (EG) in the presence of catalyst and causes formation of bis-2-hydroxyethyl terephthalate (BHET) monomer (Scheme 1) [1].

In our research, mayenite (Ca12Al14O33) was used as a catalyst for glycolysis reaction. Synthesis and preparation of mayenite have influence for its catalytic activity. The highest surface area (m2/g) and reducibility (mmol H2/g) of mayenite particles, the more active catalysis [2].

BHET synthesis was carried out in three-neck round bottom flask. Mayenite, which calcination temperature was 900 °C, was added to EG solvent, heated until 196 °C, then PET flakes were added and mixture was heated for 2.5 hours. After 2.5 hours, the mixture was cooled in ice-bath; boiling water was poured and heated until 100 °C. Mixture was filtered still hot. The filtrate was reheated until its clear, cooled to 5 °C and left for 16 h. The obtained crystals were dried at 60 °C. The BHET structure was proved by NMR, FTIR, XRD, TA analysis and compared to reference BHET, which was received from Sigma-Aldrich and recrystallized (Fig. 1).

Figure Scheme 1
Fig. Scheme 1. Synthesis of BHET
Figure 1
Fig. 1. a – XRD spectra of BHET and reference; b and c – SEM images of BHET and reference crystals respectively, magnification 2500x

[1] A. Sheel, D. Pant, 4 - Chemical Depolymerization of PET Bottles via Glycolysis, Recycling of Polyethylene Terephthalate Bottles, ISBN 978-0-12-811361-5, India, 61-84 (2019).

[2] A. Intiso, F. Rossi, A. Proto, R. Cucciniello, The fascinating world of mayenite (Ca12Al14O33) and its derivatives, Rendiconti Lincei. Scienze Fisiche e Naturali 32, 699-708 (2021).