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Preparation method of polyglycolic acid

A technology of polyglycolic acid and glycolic acid, which is applied in the field of preparation of polyglycolic acid, can solve the problems of long reaction time, complicated process, and increased energy consumption of the preparation process, and achieve the effects of shortened reaction time, increased molecular weight, and reduced energy consumption

Pending Publication Date: 2020-05-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of polyglycolic acid by the two-step method is much more complicated than the one-step method, and a large amount of high-boiling solvents are used in the polymerization process, which increases the energy consumption of the preparation process, and at the same time puts forward higher requirements for the recycling of solvents.
[0005] Patent CN102295765B reported using biomass creatinine as a catalyst to obtain a copolymer with a molecular weight between 18,000 and 177,000 through solid-phase copolymerization of glycolic acid and lactic acid, but the reaction time of the solid-state polymerization was more than 96 hours, and the reaction time long
In addition, there is no report that this method is used to prepare polyglycolic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 1200g of glycolic acid crystals and 2.0g of stannous octoate into a 5L reactor, heat to 90°C under normal pressure to completely melt the reactants, then raise the temperature of the system from 90°C to 200°C within 2 hours, and at this temperature Reacted for 2h, during which the water generated in the reaction was distilled off. Then evacuate to a system pressure of 5000 Pa, and continue the reaction for 2 hours to obtain polyglycolic acid. Utilize GPC to measure its weight-average molecular weight M w It is 14000, the molecular weight distribution coefficient PDI is 2.06, and its intrinsic viscosity is 0.33dl / g.

[0027] Add 20g of N,N'-dicyclohexylcarbodiimide to the reaction kettle, raise the temperature to 210°C, evacuate to a system pressure of 1000pa, and continue the reaction for 10h to obtain 907g of polyglycolic acid solid. Utilize GPC to measure its weight-average molecular weight M w It is 79300, the molecular weight distribution coefficient PDI is 1...

Embodiment 2

[0029] Add 2000 g of 60% glycolic acid aqueous solution and 2.0 g of stannous octoate into a 5 L reactor, heat to 140° C. under normal pressure and react at this temperature for 1 h, and distill off water. Afterwards, the system was heated from 140°C to 200°C within 2 hours, and reacted at this temperature for 1 hour, during which time the water generated in the reaction was distilled off. Then evacuate to a system pressure of 5000 Pa, and continue the reaction for 2 hours to obtain polyglycolic acid. Utilize GPC to measure its weight-average molecular weight M w It is 13200, the molecular weight distribution coefficient PDI is 1.99, and its intrinsic viscosity is 0.31dl / g.

[0030] Add 20g of N,N'-dicyclohexylcarbodiimide to the reaction kettle, raise the temperature to 210°C, evacuate to a system pressure of 1000pa, and continue the reaction for 10h to obtain 900g of solid polyglycolic acid. Utilize GPC to measure its weight-average molecular weight M w It is 78500, the m...

Embodiment 3

[0032] Add 1200g of glycolic acid crystals and 2.0g of stannous octoate into a 5L reactor, heat to 90°C under normal pressure to completely melt the reactants, then raise the temperature of the system from 90°C to 200°C within 2 hours, and at this temperature Reacted for 2h, during which the water generated in the reaction was distilled off. Then evacuate to a system pressure of 5000 Pa, and continue the reaction for 2 hours to obtain polyglycolic acid. Utilize GPC to measure its weight-average molecular weight M w It is 14000, the molecular weight distribution coefficient PDI is 2.06, and its intrinsic viscosity is 0.33dl / g.

[0033] Add 20g of N,N'-diisopropylcarbodiimide to the reaction kettle, raise the temperature to 210°C, evacuate to a system pressure of 1000pa, and continue the reaction for 10h to obtain 899g of polyglycolic acid solid. Utilize GPC to measure its weight-average molecular weight M w It is 77600, the molecular weight distribution coefficient PDI is 1....

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Abstract

The invention relates to a preparation method of polyglycolic acid, and mainly solves the problem that a polymer with a weight-average molecular weight Mw of more than 20,000 cannot be obtained by a poly-condensation reaction of polyglycolic acid. The technical scheme is as follows: the preparation method of polyglycolic acid is adopted; the preparation method comprises the following steps: step 1, reacting glycolic acid or glycolate to obtain polyglycolic acid with a weight-average molecular weight Mw lower than 20000, and step 2, adding a dehydrating agent into the obtained polyglycolic acidto carry out further polymerization; the problems are well solved, polyglycolic acid with higher weight-average molecular weight can be obtained, and the preparation method can be used for industrialproduction of polyglycolic acid with a high weight-average molecular weight.

Description

technical field [0001] The invention relates to a preparation method of polyglycolic acid. Background technique [0002] Polyglycolic acid, also known as polyglycolic acid (PGA), is a biodegradable aliphatic polymer, which is hydrolyzed under the catalysis of enzymes or acids and bases in microorganisms or organisms, and finally forms carbon dioxide and water. Due to its excellent biocompatibility, it has been widely used in the medical field. Polyglycolic acid can be used to prepare absorbable surgical sutures, protective sleeves after cutting emphysema, tissue engineering materials, ligatures in liver resection, isolation mesh to prevent intestinal adhesion after surgery, and materials to promote cell attachment , orthopedic materials, etc. In addition, polyglycolic acid resins are also used for well treatment fluids in oil extraction because of their small environmental load. Films made of polyglycolic acid are also excellent in gas barrier properties, so polyglycolic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/06C08G63/85
CPCC08G63/06C08G63/85
Inventor 朱煜王睿周芬
Owner CHINA PETROLEUM & CHEM CORP
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