Preparation method of glycolide

A glycolide and ethanol technology, applied in the field of materials, can solve the problems of increasing the difficulty of product purification, increasing the cost of separation and purification, and increasing the cost of production, so as to reduce production costs, solve product pollution, and improve production efficiency.

Active Publication Date: 2022-05-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the reaction speed and yield of this method are improved to a certain extent, the introduction of a large number of polyether segments increases the cost of production, and the by-product polyether segments will be collected together with glycolide, which improves the efficiency of subsequent separation and purification. Cost, increasing the difficulty of product purification

Method used

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  • Preparation method of glycolide
  • Preparation method of glycolide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]1.1 Add 1520g of 100% glycolic acid, 2000g of hydroxyl-terminated polybutadiene (HTPB2500, Zibo Qilong Chemical), 10g of succinic acid and 2g of catalyst stannous octoate into a 5L round-bottomed flask in sequence, and heat up to 130 degrees for stirring , react at normal pressure for 3 hours, then raise the temperature to 160 degrees, vacuumize the polycondensation reaction, P=3000Pa, after 5 hours, increase the vacuum degree to P=600Pa, continue the polycondensation reaction for 10 hours, and obtain hyperbranched polybutadiene-oligomeric Glycolic acid copolymer 3100g.

[0032] The hyperbranched polybutadiene-oligoglycolic acid copolymer obtained in the present invention is analyzed by gel permeation chromatography, and the number average molecular weight of the polymer is measured to be 5100 g / mol.

[0033] 1.2 The hyperbranched polybutadiene-oligoglycolic acid copolymer among the embodiment 1.1 and 5g cracking catalyst antimony trioxide are warmed up to 220 degree, af...

Embodiment 2

[0039] 2.1 Add 1520g of 100% glycolic acid, 3000g of hydroxyl-terminated polybutadiene (HTPB2500, Zibo Qilong Chemical), 20g of succinic acid and 3g of catalyst stannous chloride into a 5L round-bottomed flask in turn, and heat up to 140 degrees to carry out Stir, react at normal pressure for 3 hours, then heat up to 170 degrees, vacuumize for polycondensation reaction, P=3000Pa, after 4 hours, increase the vacuum degree to P=700Pa, continue polycondensation reaction for 10 hours, and obtain hyperbranched polybutadiene-low Polyglycolic acid copolymer 4095g.

[0040] The hyperbranched polybutadiene-oligoglycolic acid copolymer obtained in the present invention is analyzed by gel permeation chromatography, and the number average molecular weight of the polymer is measured to be 5500 g / mol.

[0041] 2.2 The hyperbranched polybutadiene-oligoglycolic acid copolymer in embodiment 2.1 and 7g cracking catalyst zinc oxide are warmed up to 230 degrees, after the copolymer melts complete...

Embodiment 3

[0045] 3.1 Add 1520g of 100% glycolic acid, 2000g of hydroxyl-terminated polybutadiene (HTPB4500, Zibo Qilong Chemical), 20g of adipic acid and 4g of catalyst stannous benzoate into a 5L round-bottomed flask in turn, and heat up to 150 degrees for Stir, react at normal pressure for 3 hours, then heat up to 170 degrees, vacuumize for polycondensation reaction, P=3000Pa, after 2 hours, increase the vacuum degree to P=700Pa, continue polycondensation reaction for 10 hours, and obtain hyperbranched polybutadiene-low Polyglycolic acid copolymer 3098g.

[0046] The hyperbranched polybutadiene-oligoglycolic acid copolymer obtained in the present invention is analyzed by gel permeation chromatography, and the number average molecular weight of the polymer is 7500 g / mol.

[0047] 3.2 The hyperbranched polybutadiene-oligoglycolic acid copolymer in embodiment 3.1 and 5g cracking catalyst antimony acetate are warmed up to 240 degrees, after the copolymer melts completely, depolymerize by ...

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Abstract

The invention provides a glycolide preparation method, which comprises: carrying out a condensation polymerization reaction on a glycolic acid monomer, a polyolefin polyol and a binary acid monomer under the action of a catalyst to obtain a branched polyolefin-glycolic acid copolymer, or carrying out condensation polymerization on the glycollic acid monomer, the polyolefin polybasic acid and the dihydric alcohol monomer under the action of the catalyst to obtain the branched polyolefin-glycollic acid copolymer, the branched polyolefin-glycollic acid copolymer is subjected to a cracking reaction, and glycolide is obtained. According to the method provided by the invention, the problems of low glycolic acid cracking speed and product pollution caused by introduction of a high-boiling-point solvent in the cracking process are well solved, the product purity is relatively high, the separation process of glycolide and the solvent in the product is avoided, the production efficiency is improved, the production cost is reduced, and the method can be used for industrial production of glycolide.

Description

technical field [0001] The invention relates to the technical field of materials, in particular to a preparation method of glycolide. Background technique [0002] Polyglycolic acid is a green polymer material with good biodegradability and biocompatibility. It also has high mechanical strength and excellent gas barrier properties. It can be applied in the field of packaging materials and medical polymer materials. At present, the synthesis methods of polyglycolic acid mainly include direct polycondensation method and glycolide ring-opening polymerization method. Using glycolic acid for direct dehydration and oligomerization, the molecular weight of the product is low, and it is difficult to meet the performance of the material. In order to obtain polyglycolic acid with high molecular weight and high performance, it is necessary to use the ring-opening polymerization method of glycolide, in which the preparation of glycolide is the key At present, researchers have done a lo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/12B01J23/14B01J23/18B01J27/135B01J31/04C08G63/60
CPCC07D319/12B01J23/14B01J23/18B01J27/135B01J31/04C08G63/60
Inventor 张宝边新超陈学思李杲
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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