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Spiro ethylene glycol-based copolyester and preparation method and product thereof

A technology of spiroethylene glycol and copolyester, which is applied in the field of spiroethylene glycol-based copolyester and its preparation, which can solve the uncontrollable degradation process of degradable materials, the inability to meet the toughness at the same time, and the impact of degradation speed It can improve the glass transition temperature and temperature resistance, broaden the mechanism and scope, and achieve the effect of easy implementation

Active Publication Date: 2020-04-28
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, these degradable materials still have problems such as insufficient strength and toughness, insufficient melting point, and insufficient thermal stability.
In addition, these degradable materials often require composting conditions during the degradation process, and the degradation time is relatively long. Changes in the degradation environment have a great impact on the degradation rate, making the degradation process of these degradable materials uncontrollable

Method used

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  • Spiro ethylene glycol-based copolyester and preparation method and product thereof
  • Spiro ethylene glycol-based copolyester and preparation method and product thereof
  • Spiro ethylene glycol-based copolyester and preparation method and product thereof

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preparation example Construction

[0027] The invention provides a kind of preparation method based on spiroethylene glycol copolyester, comprising:

[0028] S1, mixing spiroethylene glycol with the first component, the second component, and an esterification catalyst, and performing an esterification reaction at a first temperature to obtain an esterified product, wherein the first component is a binary Acid and / or dibasic acid ester compound, the second component is aliphatic dihydric alcohol;

[0029] S2, the esterification product is subjected to polycondensation reaction at a second temperature to obtain a copolyester based on spiroethylene glycol, and the structural formula of the copolyester is shown in the following formula (1):

[0030]

[0031] Among them, R 1 is a structural unit corresponding to the first component a, R 2 As a structural unit corresponding to the second component c, x and y are both integers, and the ratio of x to y is 10:1˜1:10.

[0032] Spiroethylene glycol contains an aceta...

Embodiment 1

[0063] Add 43.8g (0.3mol) of 1,4-dimethyl succinate, 29.4g (0.326mol) of 1,4-butanediol, and 53.0g (0.174mol) of spiroethylene glycol into the reactor, and then 0.1% of the total mass of tetrabutyl titanate was added, and under the protection of high-purity nitrogen, it was reacted at 180-200° C. for 5 hours to obtain an esterification product.

[0064] Continue to add 0.2% antimony trioxide, 0.5% phosphoric acid and 0.5% antioxidant 1010 to the reactor, gradually reduce the vacuum to 1000Pa, and then reduce the pressure to less than 50Pa after 30 minutes, and react at 240°C After 6 hours, a white copolyester product was obtained.

[0065] Tests such as nuclear magnetic resonance, DSC, TGA, mechanical properties, molecular weight, intrinsic viscosity, and degradation performance were carried out on the copolyester respectively.

[0066] figure 1 , figure 2 Contains the NMR and DSC primary temperature rise diagrams of the copolyester. From figure 1 It can be seen that the...

Embodiment 2

[0074] Add 43.8g (0.3mol) of 1,4-dimethyl succinate, 34.8g (0.386mol) of 1,4-butanediol, and 34.7g (0.114mol) of spiroethylene glycol into the reactor, and then 0.2% of the total mass of anhydrous zinc acetate is added, and under the protection of high-purity nitrogen, the reaction is carried out at 170-190° C. for 4 hours to obtain an esterification product.

[0075] Continue to add 0.2% tetrabutyl titanate, 0.4% triphenyl phosphate and 0.6% antioxidant 1010 to the reactor, gradually reduce the vacuum to 500Pa, and reduce the pressure to less than 30Pa after 30 minutes , 220 ° C for 5 hours to obtain a white copolyester product.

[0076] Tests such as nuclear magnetic resonance, DSC, TGA, mechanical properties, molecular weight, intrinsic viscosity, and degradation performance were carried out on the copolyester respectively. It can be seen from the nuclear magnetic resonance test that the copolyester has a clear structure, and the ratio of the number of structural units of ...

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Abstract

The invention relates to spiro ethylene glycol-based copolyester as well as a preparation method and a product thereof. The structural formula of the spiro ethylene glycol-based copolyester is shown as the following formula (1): wherein R1 is a structural unit corresponding to a first component, R2 is a structural unit corresponding to a second component, x and y are integers, and the ratio of x to y is 10: 1-1: 10. The copolyester provided by the invention has excellent strength, modulus, toughness, heat resistance and other properties, wide degradation range and controllable speed, and is suitable for preparing packaging materials, medical materials, films, fibers, toys and other products.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to spiroethylene glycol-based copolyesters, preparation methods and products thereof. Background technique [0002] At present, artificially synthesized degradable materials mainly include polylactic acid, polyglycolic acid, polybutylene terephthalate adipate, polybutylene succinate, etc. However, these degradable materials still have problems such as insufficient strength and toughness, insufficient melting point, and insufficient thermal stability. In addition, these degradable materials often require composting conditions during the degradation process, and the degradation time is relatively long. Changes in the degradation environment have a great impact on the degradation rate, making the degradation process of these degradable materials uncontrollable. Contents of the invention [0003] Based on this, it is necessary to provide a spiroethylene glycol-based copolye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/83C08G63/85C08G63/86
CPCC08G63/672C08G63/83C08G63/85C08G63/866
Inventor 胡晗张若愚王静刚田莹朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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