Synthesis, Characterization and Ring-opening Polymerization of Poly(trimethylene terephthalate) Cyclic Oligomers

Abstract

Abstract: Cyclic oligomers of poly(trimethylene terephthalate)(PTT) were prepared by reaction of 1,3-propanediol with terephthaloyl chloride(TPC) under diluted conditions and separated from the linear products by silica gel column. The structures of PTToligomeric cyclics were confirmed by means of ¹H NMR, mass spectrometry, and elementary analysis. Cyclic dimer, trimer, tetramer, pentamer and heptamer were further separated by gel permeation chromatography and high performance liquid chromatography. They were found to constitute most of the cyclics mixtures with a preponderance of the cyclic trimer. The cyclic oligomers melt at 92.3～222.6 ℃, providing liquids of low viscosity. Ring opening polymerization was carried out by heating the sample mixtures at 250 ℃ for 15 minutes in the presence of conventionally used catalysts, such as Sn(Oct) 2, 1-ethoxy-3-chlorotetrabutyldistannoxane, Ti(OBu)₄ and antimony oxide. The inherent viscosity of PTT prepared via ring opening polymerization was as high as 0.49 dL/g.

Key words: Poly(trimethylene terephthalate), Cyclic oligomers, Ring-opening polymerization, Matrix-assisted laser desorption/ionization-time of flight mass spectrometry

CLC Number:

O631

TrendMD:

WAN Xin-Hua, CAO Yu, ZHANG Fei, SUN Ling, ZHOU Qi-Feng . Synthesis, Characterization and Ring-opening Polymerization of Poly(trimethylene terephthalate) Cyclic Oligomers[J]. Chem. J. Chinese Universities, 2002, 23(1): 147.

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Synthesis, Characterization and Ring-opening Polymerization of Poly(trimethylene terephthalate) Cyclic Oligomers

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