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Method for synthesizing aromatic polyester without catalyst and product thereof

An aromatic polyester and catalyst technology, applied in the field of polymer material synthesis, can solve the problems of large amount of organic catalysts, low catalytic efficiency, low molecular weight of polyester, etc., and achieve the effect of avoiding biological toxicity and high product purity

Active Publication Date: 2020-11-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic efficiency of this type of organic catalyst is low, and the molecular weight of the synthesized polyester is low, and there is no commercial example yet.
Moreover, in order to make up for the lower catalytic efficiency, the amount of organic catalyst used is relatively large, which will also lead to a certain degree of biological toxicity (Nachtergael, Amandine, et al.Biomacromolecules 16.2(2015):507-514.)

Method used

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  • Method for synthesizing aromatic polyester without catalyst and product thereof
  • Method for synthesizing aromatic polyester without catalyst and product thereof
  • Method for synthesizing aromatic polyester without catalyst and product thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Prepolymerization stage: Add 52.46g of terephthalic acid (PTA) and 20.00g of ethylene glycol into a 250mL three-necked flask, and heat to 200°C under 0.3MPa pressure to carry out esterification reaction. The reaction time was 2 hours, and a hydroxyl-terminated prepolymer was obtained. through 1 H NMR test shows that in the hydroxyl-terminated prepolymer, the molar ratio of terephthalic acid and ethylene glycol units is 1:1.3.

[0029] Then 2.66g of succinic acid (SA) was added, and the molar ratio of terephthalic acid, succinic acid and ethylene glycol was 0.98:0.07:1. The reaction was continued at 200° C. for 2 hours, during which the water generated by the reaction was removed by using a condensation reflux device. After the reaction is completed, the carboxyl-terminated prepolymer is obtained. through 1 H NMR test shows that in the carboxyl-terminated prepolymer, the molar ratio of terephthalic acid, succinic acid and ethylene glycol units is 0.94:0.08:1.

[003...

Embodiment 2～4

[0035] The synthesis process is the same as in Example 1, except that the molar ratios of terephthalic acid, succinic acid and ethylene glycol are replaced by 0.3:0.8:1, 0.6:0.5:1 and 0.95:0.15:1 in sequence.

[0036] After testing, the intrinsic viscosity of the polyester product obtained in Example 2 is 0.78dL / g, and the viscosity average molecular weight is 35500Da.

Embodiment 3

[0037] The intrinsic viscosity of the polyester product obtained in Example 3 is 0.71dL / g, and the viscosity average molecular weight is 31200Da.

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Abstract

The invention discloses a method for synthesizing aromatic polyester without a catalyst. The method comprises the following steps: a pre-polymerization stage: under the condition of no additional catalyst, carrying out esterification reaction on aromatic dicarboxylic acid and excessive molar ratio of dihydric alcohol to obtain a hydroxyl-terminated prepolymer; then adding cyclized dicarboxylic acid or corresponding anhydride with the molar weight greater than that of the hydroxyl-terminated prepolymer, and continuously carrying out esterification reaction to obtain a carboxyl-terminated prepolymer; and a polymerization stage: under the condition of reduced pressure, controlling the reaction temperature to be not lower than the boiling point of anhydride corresponding to the cyclized dicarboxylic acid, and removing anhydride corresponding to the cyclized dicarboxylic acid from the carboxyl-terminated prepolymer to obtain the aromatic polyester. The synthesis method provided by the invention can be used for preparing aromatic polyester without catalyst residues, so that the problems of biotoxicity, accelerated aging and the like caused by use of the catalyst are avoided, and the method can be safely applied to the fields of food contact materials, medical materials and the like.

Description

technical field [0001] The invention relates to the technical field of polymer material synthesis, in particular to a catalyst-free method for synthesizing aromatic polyester and its products. Background technique [0002] Polyester is a polymer whose main chain repeating units are connected by ester bonds. Because of its excellent mechanical and thermal properties, it is widely used in the fields of clothing fibers, sheets, films, and bottle plastics. Industrially, polyester is usually synthesized by melt polycondensation of dibasic carboxylic acid and dibasic alcohol, followed by two stages of esterification reaction and transesterification reaction. Among them, the esterification reaction is a prepolymerization stage, and a hydroxyl-terminated prepolymer is formed after esterification of a dicarboxylic acid and a diol with an excess molar ratio of 0.05 to 0.2; the polymerization stage is to remove the excess diol through transesterification. , so as to obtain polyester p...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G63/183C08G63/672C08G63/685
CPCC08G63/183C08G63/672C08G63/6856C08G63/78
Inventor 朱蔚璞蔡秋泉
Owner ZHEJIANG UNIV
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