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Polymerizing production method for transparent amorphous copolyester

A production method and copolyester technology, which are applied in the field of polymerization production of transparent amorphous copolyester, can solve the problems of reducing catalytic activity and prolonging condensation reaction time, so as to reduce the content of terminal carboxyl groups, shorten the esterification time, and reduce side effects

Active Publication Date: 2013-11-27
JIANGSU JINGHONG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the publication numbers are CN1216051A, CN1951976A, CN1440993A, CN1121727A and CN1800236A Chinese patents and relevant polyester synthesis method open documents, heat stabilizers are usually added in the esterification stage or the initial stage of polycondensation, but the phosphorus-containing compound is easy to react with the metal of the condensation catalyst. Ion complexation reduces the catalytic activity and greatly prolongs the condensation reaction time. It is also necessary to develop new process conditions and parameters to suppress the promotion of metal ions on thermal decomposition.

Method used

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  • Polymerizing production method for transparent amorphous copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 70 parts of PTA, 40 parts of EG, 15 parts of CHDM, monobutyltin oxide / dibutyltin oxide / ethylenediaminetetraacetic acid are 0.01 part / 0.04 part / 0.05 part, 0.05 part of phosphite tris(2,4- Di-tert-butylphenyl) ester antioxidant and 0.1 part of 2,2 methylene-bis(4-methyl-6-tert-butylphenol) antioxidant, 0.01 part of cobalt acetate and 0.06 part of antimony acetate / B Diaminetetraacetic acid (mass ratio 1:1) complex was beaten into slurry A.

[0033] Put the slurry A into the esterification kettle, fill it with nitrogen to 0.2MPa, raise the temperature to 220°C, control the pressure release rate, and maintain it at 0.3-0.35MPa. At normal pressure, the esterification time is 2h.

[0034] Press the esterified product into the condensation kettle, gradually raise the temperature to 250°C, reduce the reaction pressure to 0.4-0.5MPa, polymerize for 1.5-2 hours, then gradually reduce the pressure to less than 200Pa, and gradually reduce the temperature of the polycondensation rea...

Embodiment 2

[0036] In Example 1, after adding 0.05 part of triphenyl phosphite, the condensation reaction was carried out for 30 minutes, and the material was discharged to obtain a copolyester with an intrinsic viscosity of 0.83 dL / g and a carboxyl content of 7.3 mol / t.

Embodiment 3

[0038] 70 parts of PTA, 40 parts of EG, 20 parts of CHDM, monobutyltin oxide / dibutyltin oxide / ethylenediaminetetraacetic acid are 0.03 parts / 0.06 parts / 0.09 parts, 0.05 parts of phosphite tris(2,4- Di-tert-butylphenyl) ester antioxidant and 0.1 part of 2,2 methylene-bis(4-methyl-6-tert-butylphenol) antioxidant, 0.01 part of cobalt acetate and 0.06 part of ethylene glycol antimony / ethylenediaminetetraacetic acid (mass ratio 1:1) complex was beaten into slurry A.

[0039] Put the slurry A into the esterification kettle, fill it with nitrogen to 0.2MPa, raise the temperature to 220°C, control the pressure release rate, and maintain it at 0.3-0.35MPa. At normal pressure, the esterification time is 1.5h.

[0040] Press the esterified product into the condensation kettle, gradually raise the temperature to 250°C, reduce the reaction pressure to 0.4-0.5MPa, polymerize for 1.5-2 hours, then gradually reduce the pressure to less than 200Pa, and gradually reduce the temperature of the...

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Abstract

The invention discloses a polymerizing production method for transparent amorphous copolyester. The method has the advantages of low esterification temperature, short esterification time and high esterification rate. The method comprises the following steps of: carrying out an esterification reaction and a condensation reaction on dihydric alcohol and dicarboxylic acid to obtain the transparent amorphous copolyester, wherein the esterification reaction comprises the following specific procedures of: breaking various materials into pulp by using a pulping machine and carrying out the esterification reaction on the pulp at the temperature of 220-240DEG C for 1.0-1.5 hours to obtain an esterified product; the condensation reaction comprises the following specific procedures of: polymerizing the esterified product obtained by the esterification reaction at the reaction pressure of 0.2-0.5MPa and the temperature of 250-260DEG C for 1.5-2 hours; then reducing the pressure to be less than 200MPa within 0.5 hour; raising the condensation reaction temperature to be 275DEG C from 260DEG C; adding a thermal stabilizer; and after the condensation reaction, obtaining a polyester copolymer with the inherent viscosity of greater than 0.75dL / g and the carboxyl content of less than 10mol / t.

Description

technical field [0001] The present invention relates to a method for producing a polymer, more particularly to a method for producing a transparent amorphous copolyester by polymerization. Background technique [0002] PETG is an amorphous copolyester prepared by using terephthalic acid, ethylene glycol, and 1,4-cyclohexanedimethanol as monomers. It has excellent impact resistance, high transparency, and chemical resistance. It has a wide range of thermoformability and is extremely easy to form, cold bending without stress cracking or whitening. The excellent processing performance of PETG can completely replace expensive polycarbonate (PC) and general polymethacrylates (PMMA), polyvinyl chloride (PVC), etc. At the same time, PETG will not release toxic gases when incinerated. It will not pollute groundwater sources after landfill treatment, so it has good application prospects in food packaging, daily necessities, photochemistry and medicine. [0003] PETG is generally pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/199C08G63/85
Inventor 江国栋陈双俊张军吴培龙符朝贵陆银秋
Owner JIANGSU JINGHONG NEW MATERIAL TECH
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