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Preparation method of butyleneadipate-terephthalate with low terminal carboxyl group content

A technology of butylene phthalate and terephthalic acid, which is applied in the field of preparation of poly(butylene adipate-terephthalate) with low carboxyl content, can solve the problem of affecting processing performance and later use performance, The problems of high production cost of degradable polyester and easy aging and degradation of synthetic resin can achieve the effect of less catalyst consumption, improved heat resistance and processing performance, and reduced production cost

Active Publication Date: 2013-11-27
甘肃莫高聚和环保新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are still a series of problems in the synthesis of polybutylene adipate-terephthalate, such as the high content of carboxyl groups, which makes the synthetic resin easy to age and degrade during storage, affecting its processing performance and later use performance
At the same time, due to the high production cost of this degradable polyester, its large-scale application in various fields such as industrial and agricultural production and daily life is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix 136g of butanediol, 80g of adipic acid and 75g of terephthalic acid in a reactor, add 0.612g of glycerin and 0.582g of aqueous titanium lactate complex, stir well, and under nitrogen protection, the temperature is 235°C The esterification reaction was carried out under the same conditions, and the reaction was carried out at a constant temperature for 2 hours. Then, the temperature was raised to 250° C., and the pressure was reduced to 50 Pa to carry out polycondensation reaction, and the reaction was carried out for 3 hours to obtain polybutylene adipate-terephthalate.

[0025] The carboxyl group content of poly(butylene adipate-terephthalate) is 26mol / t, and the molecular weight is 16.4×10 4 , the tensile strength is 18.3MPa, and the elongation at break is 641%.

Embodiment 2

[0027] Mix 180g of butanediol, 102g of adipic acid and 50g of terephthalic acid in a reactor, add 0.332g of pentaerythritol and 0.582g of aqueous titanium phosphorus complex, stir well, and under the protection of helium, the temperature is 215°C The esterification reaction was carried out at a constant temperature for 3 hours. Then, the temperature was raised to 230° C., and the pressure was reduced to 100 Pa to carry out polycondensation reaction for 4.5 hours to obtain polybutylene adipate-terephthalate ends.

[0028] The carboxyl content of poly(butylene adipate-terephthalate) is 15mol / t, and the molecular weight is 11.0×10 4 , the tensile strength is 15.6MPa, and the elongation at break is 749%.

Embodiment 3

[0030] Mix 92g of butanediol, 88g of adipic acid and 66g of terephthalic acid in the reactor, add 0.369g of xylitol, 0.738g of water-based triethanolamine zirconium salt, stir well, under the protection of neon gas, the temperature is 200°C Carry out esterification reaction under the condition of constant temperature reaction 3.5 hours. Then the temperature was raised to 240° C., the pressure was reduced to 30 Pa to carry out polycondensation reaction, and the reaction was carried out for 4 hours to obtain polybutylene adipate-terephthalate.

[0031] The carboxyl group content of polybutylene adipate-terephthalate is 21mol / t, and the molecular weight is 18.3×10 4 , the tensile strength is 19.8MPa, and the elongation at break is 585%.

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Abstract

The invention belongs to the technical field of fully-biodegradable fat-aromatic copolyester, in particular to a preparation method of butyleneadipate-terephthalate with low terminal carboxyl group content. The preparation method comprises the following steps: mixing butanediol, adipic acid and terephthalic acid; after polyhydric alcohols are added, adding a water-soluble catalyst; stirring uniformly; performing esterification reaction under the protection of gas with inactive chemical property; then performing condensation polymerization so as to obtain butyleneadipate-terephthalate. The preparation method provided by the invention has the advantages that the operation is simple, the terminal carboxyl group content of butyleneadipate-terephthalate is lowered, heat resistance and processability of butyleneadipate-terephthalate are improved on the premise that the biodegradability of a polymer is not changed, the stability during the process of storage is improved, a non-poisonous pollution-free fourth monomer is added, so that rate of polymerization is increased, the terminal carboxyl group content of products is lowered, characteristics of green and environmental protection of the products are not affected, the dosage of a catalyst is less, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of completely biodegradable aliphatic-aromatic copolyesters, and in particular relates to a preparation method of polybutylene adipate-terephthalate with low carboxyl content. technical background [0002] Since the birth of the first synthetic resin in the early 20th century and the realization of industrialized production, mankind has opened up a new era of mass production and the use of polymer materials. However, due to some excellent properties of plastic, it is not easy to rot after use, and it accumulates over time, seriously affecting the ecological environment of the earth. It is urgent to seek a new degradable material to alleviate the environmental pollution caused by traditional materials. In recent years, degradable polyester has become a research hotspot at home and abroad due to its degradation characteristics. [0003] Polybutylene adipate-terephthalate is one of the completely biodegradable polyester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/20C08G63/78
Inventor 杨苹苹杨军李宗华卢伟
Owner 甘肃莫高聚和环保新材料科技有限公司
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