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A kind of technical method of synthesizing glycolide

A process method and technology of glycolide, which is applied in the field of synthesis of biodegradable materials polyglycolide and its copolymer polymerization monomers, can solve the problems of easy pollution of high boiling point polar solvents, toxic metal catalysts, etc., and achieve easy The effect of industrial implementation, high purity and simplified process flow

Active Publication Date: 2019-01-29
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of toxic metal catalysts and high boiling point polar solvents that easily contaminate products in the existing glycolide synthesis process, and to provide an all-green process for synthesizing glycolide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] After adding 50kg of the raw material 70% glycolic acid aqueous solution into the reaction kettle, firstly, the temperature of the reactant was raised from room temperature to 100°C at a rate of 1.0°C / min, and the dehydration reaction was carried out at normal pressure for 1.0h, starting from 100°C at a rate of 1.0°C / min The rate of min is increased to 140°C, and the dehydration reaction at normal pressure is 1.0h. From 140°C, the rate is increased to 155°C at a rate of 1.0°C / min. The rate of dehydration at normal pressure is 1.0h. to 200°C, and at the same time, the absolute pressure is reduced from normal pressure to 90.0 torr at a rate of 1.0 torr / min, and the reaction is continued for 1.0 h under this condition, while maintaining this temperature, the absolute pressure of the reaction system is reduced from 90.0 torr to a rate of 1.0 torr / min To 10.0torr, continue the reaction under this condition for 1.0h, after the dehydration oligomerization stage reaction control...

Embodiment 2

[0040] After adding 50kg of the raw material 70% glycolic acid aqueous solution into the reaction kettle, firstly, the temperature of the reactant was raised from room temperature to 100°C at a rate of 1.0°C / min, and the dehydration reaction was carried out at normal pressure for 1.0h, starting from 100°C at a rate of 1.0°C / min The rate of min is increased to 140°C, and the dehydration reaction at normal pressure is 1.0h. From 140°C, the rate is increased to 155°C at a rate of 1.0°C / min. The rate of dehydration at normal pressure is 1.0h. to 200°C, and at the same time, the absolute pressure is reduced from normal pressure to 90.0 torr at a rate of 1.0 torr / min, and the reaction is continued for 1.0 h under this condition, while maintaining this temperature, the absolute pressure of the reaction system is reduced from 90.0 torr to a rate of 1.0 torr / min To 10.0torr, continue the reaction under this condition for 1.0h, after the dehydration oligomerization stage reaction control...

Embodiment 3

[0044] After adding 50kg of the raw material 70% glycolic acid aqueous solution into the reaction kettle, firstly, the temperature of the reactant was raised from room temperature to 100°C at a rate of 1.0°C / min, and the dehydration reaction was carried out at normal pressure for 1.0h, starting from 100°C at a rate of 1.0°C / min The rate of min is increased to 140°C, and the dehydration reaction at normal pressure is 1.0h. From 140°C, the rate is increased to 155°C at a rate of 1.0°C / min. The rate of dehydration at normal pressure is 1.0h. to 200°C, and at the same time, the absolute pressure is reduced from normal pressure to 90.0 torr at a rate of 1.0 torr / min, and the reaction is continued for 1.0 h under this condition, while maintaining this temperature, the absolute pressure of the reaction system is reduced from 90.0 torr to a rate of 1.0 torr / min To 10.0torr, continue the reaction under this condition for 1.0h, after the dehydration oligomerization stage reaction control...

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Abstract

An all-green process for synthesizing glycolide. The process method provided by the invention is to use a non-toxic cyclic organic guanidine compound and a non-toxic linear organic guanidine compound to form a binary composite catalytic system, use a glycolic acid aqueous solution with a mass content of 70% as a raw material, and use a reactive vacuum distillation method A high-yield (≥98.0%) synthesis of high-purity (≥99.9%) glycolide is achieved. The advantages of the present invention are: the binary composite catalytic system adopted is a non-toxic, metal-free and non-cytotoxic organic guanidine compound, with high catalytic efficiency and low consumption; the synthesized glycolide has high yield and high purity; Solvent-free, closed-cycle process is adopted, no three wastes are discharged, the process flow is simplified, and it is easy to implement industrially.

Description

technical field [0001] The invention belongs to the field of synthesis of biodegradable material polyglycolide (i.e. "polyglycolic acid") and its copolymer polymerization monomers, specifically a kind of binary organic guanidine compound as a composite catalyst, all-green synthetic glycolide process method. Background technique [0002] Polyglycolide (PGA) is a biodegradable aliphatic synthetic polyester with excellent biodegradability and compatibility. PGA has achieved many important applications in the fields of biomedicine and tissue engineering, such as: absorbable surgical sutures, implantable hard tissue repair materials and devices, controlled release / targeted drug carriers, etc. At the same time, as an environmentally friendly material, PGA can also be used to make films, injection molding products, etc. Glycolide is a monomer for synthesizing PGA and its copolymers by ring-opening polymerization, and high-purity glycolide (purity ≥ 99.9%) is the key to preparing ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/12B01J31/04
CPCB01J31/04C07D319/12B01J2231/763B01J31/0244B01J31/0251C08G63/08C08G63/82
Inventor 李弘张全兴盛家业黄伟江伟李爱民潘丙才
Owner NANJING UNIV
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