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Biodegradable aromatic-aliphatic copolyester and preparation method thereof

An aliphatic copolyester and biodegradation technology, which is applied in the field of aromatic-aliphatic copolyester, can solve the problems of incomplete progress, consumption of polylactic acid, high temperature requirements for transesterification, etc., and achieve the effect of high molecular weight and excellent performance

Active Publication Date: 2010-06-02
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the transesterification catalyst stannous chloride and p-toluenesulfonic acid used in the system are easy to catalyze the lactic acid polymer to generate the by-product lactide at a higher temperature and consume a large amount of polylactic acid; The melting point of the alcohol ester polymer is relatively high (210-225°C), and the requirements for the transesterification temperature are high. Polylactic acid is prone to degradation at a high transesterification temperature, so that the polycondensation reaction of the system cannot be carried out completely, so the molecular weight of the obtained product is There are only a few thousand and cannot be used as a material

Method used

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  • Biodegradable aromatic-aliphatic copolyester and preparation method thereof
  • Biodegradable aromatic-aliphatic copolyester and preparation method thereof
  • Biodegradable aromatic-aliphatic copolyester and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Put 160g of dimethyl terephthalate, 200g of lactic acid and 0.36g of zinc acetate into a 1L stainless steel reactor, vacuumize and deoxidize, and fill nitrogen to an atmospheric pressure after the deoxidation is complete; After the fraction reaches 90% of the theoretical value, cool the reaction system, cool to 100°C, add 200g of lactic acid, and react under high vacuum at 160°C for 2 hours; add 46g of ethylene glycol, and react at 180°C for 0.6h; Raise it to 230°C, draw a low vacuum at the same time, start a high vacuum after 45 minutes, add 0.18g tetrabutyl titanate, and react for 2.6 hours under a vacuum degree of ≤70Pa to obtain a copolyester with an intrinsic viscosity of 0.71.

Embodiment 2

[0041]Put 160g of dimethyl terephthalate, 154g of glycolic acid and 0.31g of zinc acetate into a 1L stainless steel reactor, vacuumize and deoxidize, and fill nitrogen to an atmospheric pressure after the deoxidation is completed; under an atmospheric pressure, the system is reacted at 185°C for 4 hours, After the methanol fraction reaches 90% of the theoretical value, cool the reaction system, cool to 100°C, add 154g glycolic acid, and react under high vacuum at 160°C for 2 hours; add 46g ethylene glycol, and react at 180°C for 0.3h; The temperature was gradually raised to 230°C, while low vacuum was drawn, and high vacuum was started after 45 minutes, 0.15g of tetrabutyl titanate was added, and the reaction was carried out for 2.2 hours at a vacuum degree of ≤70Pa to obtain a copolyester with an intrinsic viscosity of 0.63.

Embodiment 3

[0043] Put 160g of dimethyl terephthalate, 200g of lactic acid and 0.36g of zinc acetate into a 1L stainless steel reactor, vacuumize and deoxidize, and fill nitrogen to an atmospheric pressure after the deoxidation is complete; After the fraction reaches 90% of the theoretical value, cool the reaction system, cool to 100°C, then add 200g of lactic acid, and react under high vacuum at 160°C for 2 hours; add 78g of butanediol, and react at 180°C for 0.6h; Raise it to 230°C, draw a low vacuum at the same time, start a high vacuum after 45 minutes, add 0.21g of tetrabutyl titanate, and react for 2.5 hours under a vacuum degree of ≤70Pa to obtain a copolyester with an intrinsic viscosity of 0.74.

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Abstract

The invention provides biodegradable aromatic-aliphatic copolyester and a preparation method thereof, which is characterized in that the copolyester is randomly formed by an A repeat unit, a B repeat unit and a C repeat unit, wherein the structures of A, B and C are general formulae as follows. The preparation method comprises the following steps: firstly, preparing a polyhydroxy acid blocked aromatic compound; secondly, blocking the aromatic compound by diol to improve the thermal stability of the hydroxyl acid polymer; thirdly, performing melt polycondensation at a higher reaction temperature; and finally, obtaining the aromatic-aliphatic copolyester with novel structure and high hydroxyl acid content. Compared with the prior art, the copolyester has the advantages of high molecular weight, has excellent mechanical performance, heat resistance, corrosion resistance, easy biodegradability, simple preparation process, and easy synthesis. The A is -COOR1-COOR3-CH2-O-R2-O-, B is -COR4-O-, and C is -COOR1-COOR5-O-, wherein R1 is any one of the following groups: -C6H6-, -C6H4-, -C10H6- and [-CH2-]m; and m and n are natural numbers; and R2, R3, R4 and R5 are [-CH2-]n, and n is between 2 and 6.

Description

technical field [0001] The invention relates to a biodegradable aromatic-aliphatic copolyester, and also relates to a preparation method of the copolyester. Background technique [0002] Aromatic polyesters, such as polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT), polybutylene terephthalate (PBT), due to their excellent mechanical properties, It is widely used due to its heat resistance and chemical corrosion resistance, and is currently mainly used in the fields of fiber, packaging and coatings. However, aromatic polyesters have a long degradation cycle, and their extensive use has caused great pollution to the environment, making them an uncompromising environmentally unfriendly material. [0003] In order to improve the degradability of aromatic polyesters, researchers at home and abroad have carried out a lot of work, mainly focusing on two aspects of blending and copolymerization modification. In terms of blending, PET is mainly blended with nat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/60C08G63/78
CPCC08G63/80C08G63/66C08G63/60
Inventor 黎俊顾群蒋志强刘吉周坚施文涛魏明峰王玉忠
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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