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A kind of synthetic method of biodegradable aliphatic-aromatic copolyester

A technology for degrading fats and aromatics, applied in the field of polyester, can solve the problems of poor hydrolysis resistance, lower thermal stability, and inability to add and mix chain extenders conveniently, so as to reduce side reactions and reduce product terminal carboxyl groups value, to solve the effect of increasing the b value of resin color

Active Publication Date: 2021-11-02
RACHEM CHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the high content of terminal carboxyl groups will easily lead to poor hydrolysis resistance of products and reduced thermal stability during plastic processing.
[0005] Another method to improve the molecular weight of the resin is to use chain extenders, such as using isocyanates, oxazolines and other class chain extenders (CN1071342C, US5889135). During continuous process production, chain extenders cannot be easily added to the reactor and Mix evenly with high-viscosity materials, as described in patent CN102844336B, add a chain extender to the kettle when the solution intrinsic viscosity of the polycondensate is not greater than 0.6dL / g, to ensure that the resin and the chain extender are mixed evenly
When the viscosity of the resin is high, it is necessary to add mixing equipment such as a screw extruder. In addition, it is difficult for the chain extender to react completely. The residue of isocyanate and small molecule epoxide makes the degradable resin unsuitable for food contact materials, which limits the application of the product. Chain extenders with good safety such as carbodiimide are relatively expensive

Method used

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  • A kind of synthetic method of biodegradable aliphatic-aromatic copolyester
  • A kind of synthetic method of biodegradable aliphatic-aromatic copolyester
  • A kind of synthetic method of biodegradable aliphatic-aromatic copolyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1) 23kg / h of terephthalic acid and 28kg / h of 1,4-butanediol are continuously added to the beating kettle and mixed, and the mixed slurry is continuously sent into the esterification reaction kettle, and In addition, 12kg / h of 1,4-butanediol and 0.015kg / h of tetrabutyl titanate (TBOT) were added, the pressure of the control reactor was -10KPa, the temperature was 220°C, and the residence time was 2 hours. The water generated by the reaction, Tetrahydrofuran and butanediol were distilled off, and the obtained esterified product A was continuously removed from the reactor. The carboxyl-terminal content of the esterified product A was 180 mol / t.

[0059] 2) 22kg / h of adipic acid and 25kg / h of 1,4-butanediol are continuously added to the beating tank and mixed, and the mixed slurry is continuously sent into the esterification reactor, and additionally Add 10kg / h of 1,4-butanediol and 0.001kg / h of tetrabutyl titanate (TBOT), the temperature is 200°C, the residence time is 2 h...

Embodiment 2

[0062] 25kg / h of terephthalic acid, 23kg / h of adipic acid and 36kg / h of 1,4-butanediol are continuously added to the beating kettle for mixing, and then the mixed slurry is continuously sent to the In the esterification reaction kettle. Another way continuously feeds 7kg / h of 1,4-butanediol and 0.02kg / h of tetrabutyl titanate (TBOT) into the esterification reactor, and esterifies at a temperature of 220°C and a pressure of -20KPa. Time 2h, water, tetrahydrofuran and butanediol were distilled off. The carboxyl-terminal content of the obtained esterified product was 120 mol / t.

[0063]Then continuously enter into two precondensation reactors connected in series, add tetrabutyl titanate 0.02kg / h simultaneously, add epoxy soybean oil (epoxy value 6.0%) 2.4kg / h simultaneously, material temperature is by 210 ℃, The pressure of the reactor was reduced from 20KPa to 200Pa, the residence time was 2h, the excess butanediol was distilled off, and the intrinsic viscosity of the obtained...

Embodiment 3

[0066] 25kg / h of terephthalic acid, 23kg / h of adipic acid and 36kg / h of 1,4-butanediol are continuously added to the beating kettle for mixing, and then the mixed slurry is continuously sent to the In the esterification reaction kettle. Another way continuously feeds 7kg / h of 1,4-butanediol and 0.02kg / h of tetrabutyl titanate (TBOT) into the esterification reactor, and esterifies at a temperature of 220°C and a pressure of -20KPa. Time 2h, water, tetrahydrofuran and butanediol were distilled off. The carboxyl-terminal content of the obtained esterified product was 120 mol / t.

[0067] Then continuously enter into two precondensation reactors connected in series, add tetrabutyl titanate 0.02kg / h simultaneously, add epoxy soybean oil (epoxy value 6.0%) 0.24kg / h simultaneously, material temperature is by 200 ℃, The pressure of the reactor was reduced from 20KPa to 200Pa, the residence time was 2.5h, the excess butanediol was evaporated, and the intrinsic viscosity of the obtaine...

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Abstract

The invention discloses a method for preparing a biodegradable aliphatic-aromatic copolyester. The steps include: adding epoxy soybean oil after continuous esterification of aromatic dicarboxylic acid and aliphatic dicarboxylic acid, and continuously Pre-condensation, in the pre-condensation process, the epoxy group is inserted into the polybutylene terephthalate-adipate-PBAT molecular chain through transesterification, and then the polycondensation is carried out continuously at a higher temperature, so that the molecular weight , The intrinsic viscosity reaches the target value. The preparation method of the biodegradable aliphatic-aromatic copolyester disclosed by the present invention can make it easier for the polyester to reach the target intrinsic viscosity and molecular weight, reduce the polycondensation time of high-temperature and high-viscosity materials, reduce side reactions, and reduce product ends. Carboxyl value, solve the problem of resin yellowing. The preparation method of the biodegradable aliphatic-aromatic copolyester disclosed by the invention does not use a small molecule chain extender to extend the chain, and solves the problem of the migration of the residual chain extender from plastic to food.

Description

technical field [0001] The invention belongs to the technical field of polyester, in particular to a preparation method of biodegradable aliphatic-aromatic copolyester. Background technique [0002] Aliphatic-aromatic copolyester resin, as a biodegradable polymer with good comprehensive performance, has been studied a lot, such as patent documents US6046248, WO2010130098, CN1071342C, WO1996025446, CN102007159B, etc. disclose aliphatic / aromatic copolymerization Melting point, intrinsic viscosity of ester resin, composition and composition range of aliphatic diacid / aromatic diacid capable of exhibiting biodegradability, and various methods for improving performance such as improving molecular weight and reducing carboxyl terminal content of resin have been proposed . [0003] The commercialized varieties of aliphatic-aromatic copolyesters mainly include polybutylene terephthalate-adipate PBAT, polybutylene terephthalate-succinate PBST, polyterephthalic acid Diformic acid-seb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/78C08G63/85
CPCC08G63/183C08G63/78C08G63/85
Inventor 侯远杨吴开建寇雪晨赵燕超董栋张宁
Owner RACHEM CHINA CO LTD
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