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High-transparency and high-heat-resistance copolyester resin and preparation method thereof

A copolyester and high heat-resistant technology, which is applied in the field of high-transparency and high-heat-resistant copolyester resin and its preparation, can solve the problems of poor thermal stability, poor transparency, gas clogging, etc., and achieve good heat resistance and reduce Effects of consumption and recovery of load, and solution to clogging

Active Publication Date: 2021-08-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The present invention aims to solve the problems of poor thermal stability, easy sublimation to generate gas and block pipeline equipment, poor transparency, and easy discoloration of CBDO-based copolyesters in the prior art. Copolyester with CBDO monomer, the copolyester has excellent thermal stability and mechanical strength, and has high transparency and is not easy to change color

Method used

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  • High-transparency and high-heat-resistance copolyester resin and preparation method thereof
  • High-transparency and high-heat-resistance copolyester resin and preparation method thereof
  • High-transparency and high-heat-resistance copolyester resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0127] Example 1 Synthesis

[0128] (1) a solution of N 2 The reactor atmosphere was added dimethyl terephthalate, 67.96g (0.35mol), 2,2,4,4- tetramethyl-1,3-cyclobutanediol (cis content 62%) 30.28g ( 0.21mol), 3- methyl-1,5-pentanediol 37.22g (0.315mol) and dibutyltin oxide 0.2039g, and added primary stabilizer and auxiliary stabilizer 10100.068g 6260.034g, for 3h at 220 ℃, to give transesterification product; during the reaction, not observed in the solid line.

[0129] (2) a transesterification product of a polycondensation at 260 ℃, absolute pressure ≤200Pa conditions 2.7h, to give intrinsic viscosity of 0.75dL / g, φ cB Is 34.3mol%, φ cis,cB Copolyester was 63.8mol% - poly (2,2,4,4-tetramethyl-1,3-cyclobutanediol terephthalate - co-3-methyl-1,5-pentanediol ester), referred to as During the reaction, a viscous clear liquid was observed to be drawn out of the reactor, finally into a collection bottle, conduit unblocked. Melt level has remained stable during the reaction, a ...

Embodiment 2

[0130] Example 2 Synthesis

[0131] (1) a solution of N 2 The reactor atmosphere was added dimethyl terephthalate, 67.96g (0.35mol), 2,2,4,4- tetramethyl-1,3-cyclobutanediol (cis content 62%) 37.86g ( 0.2625mol), 2- methyl-1,3-propanediol 23.66g (0.2625mol) and dibutyltin oxide 0.2039g, and add the primary stabilizer and the auxiliary stabilizer 10100.068g 6260.034g, 2.5h the reaction at 220 ℃, to give the ester exchange product; during the reaction, not observed in the solid line.

[0132] (2) a transesterification product of a polycondensation at 260 ℃, absolute pressure conditions ≤200Pa 1.5h, to give intrinsic viscosity of 0.70dL / g, φ cB Is 46.5mol%, φ cis,cB Copolyester was 64.0mol% - poly (2,2,4,4-tetramethyl-1,3-cyclobutanediol terephthalate - co-2-methyl-1,3-propylene glycol) , denoted During the reaction, a viscous clear liquid was observed to be drawn out of the reactor, finally into a collection bottle, unblocked conduit (e.g. figure 2 Indicated). Melt level has rem...

Embodiment 3

[0133] Example 3 Synthesis

[0134] (1) a solution of N 2 Reactor atmosphere of terephthalic acid was added 58.15g (0.35mol), 2,2,4,4- tetramethyl-1,3-cyclobutanediol (cis content 60%) 45.43g (0.315mol) , 1,5-pentanediol 21.87g (0.21mol) of dibutyltin oxide and 0.1744g, reacted at 210 ℃ 1h, the reaction 220 ℃ 1h, 230 ℃ reaction 5h, to obtain an esterification product. During the reaction, not observed in the solid line.

[0135] (2) esterification products of the polycondensation at 260 ℃, absolute pressure conditions ≤200Pa 3h, to give intrinsic viscosity of 0.67dL / g, φ cB Is 54.6mol%, φ cis,cB Copolyester was 62.8mol% - poly (terephthalate 2,2,4,4-tetramethyl-1,3-cyclobutanediol - 1,5-pentanediol co-ester), referred to as During the reaction, a viscous clear liquid was observed with a small amount of white solid is extracted reactor, finally into a collection bottle, conduit unblocked. Melt level has remained stable during the reaction, a small amount of bubbles.

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Abstract

The invention relates to a polyester high polymer material, and discloses a high-transparency and high-heat-resistance copolyester resin and a preparation method thereof. The copolyester resin comprises the following components: (1) a binary acid component comprising: (a) 80-100 mol% of terephthalic acid residue, (b) 0-20 mol% of aromatic diacid residues; and (2) a dihydric alcohol component comprising: (a) 20-85 mol% of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol residues, (b) 15-80 mol% of a first diol residue, and (c) 0-30 mol% of a second diol residue. According to the copolyester resin disclosed by the invention, pentanediol residues or propylene glycol residues are introduced, so that blockage is avoided in the preparation process, the intrinsic viscosity is increased, the loss of CBDO monomers is inhibited, and the obtained copolyester has high glass transition temperature and excellent strength, toughness and thermal stability; and the foaming, foaming and expansion phenomena caused by thermal decomposition can be effectively inhibited in the melt processing process.

Description

Technical field [0001] The present invention relates to polyester polymeric materials, particularly relates to a resin and method for preparing highly transparent high heat copolyester. Background technique [0002] Polycarbonate-based (PC) of bisphenol A is the most common polymer material highly transparent high heat resistance. PC is excellent in transparency, heat resistance and toughness, light transmittance> 90%, the glass transition temperature of about 150 deg.] C, long-term use at 120 deg.] C, is an important engineering plastics, also commonly used in glass, bottle, housewares. Since the PC will be released at high temperatures bisphenol A (BPA), BPA and absorbed by the body can cause endocrine disorders, PC security concern, is prohibited for baby bottles and other food contact products. [0003] In 2007, Eastman developed high monomeric hindered diol 2,2,4,4-tetramethyl-1,3-cyclobutanediol (CBDO), and 1,4-cyclohexadiene by the CBDO dimethanol (of CHDM), dimethyl te...

Claims

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Application Information

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IPC IPC(8): C08G63/199C08G63/78
CPCC08G63/199C08G63/78
Inventor 吴林波陈妍如李伯耿
Owner ZHEJIANG UNIV
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