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Purification method of glycolide

A technology of glycolide and refining methods, applied in the direction of organic chemistry, etc., to achieve good technical effects

Active Publication Date: 2021-02-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

DuPont also reported the use of polyglycolic acid and polyether in patent US4835293 to reduce the proportion of oligomer impurities after obtaining block copolymers, but whether these methods can be applied to industrial scale production has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 400g of glycolic acid to the three-necked flask, heat to 90°C under normal pressure to completely melt the reactant, then raise the temperature of the system from 90°C to 200°C within 2h, and react at this temperature for 2h, during which time the reactant is distilled off. water produced in. Then the system pressure was reduced to 5kPa by vacuuming, and the reaction was continued for 2h until the reactant solidified into milky white to obtain a glycolic acid oligomer. Add 2.0g of stannous octoate to the oligomer, raise the temperature to 260°C, and increase the vacuum to 100pa. As the reaction proceeded, a light yellow liquid was continuously evaporated, and a yellow solid was obtained after cooling, which was the product crude glycolide. After 3 h, the reaction was stopped, and the crude product was collected, and the calculated yield was 92%. Utilize acid-base titration to measure the terminal carboxyl group content in crude glycolide to be 7.90×10 -4 mol.g -...

Embodiment 2

[0032] The preparation of thick glycolide is with embodiment 1.

[0033] The product crude glycolide (277g) was dissolved in 600g of acetone, stirred at room temperature until a uniform transparent solution was formed, and the powdery insolubles were removed by filtration through a quartz sand funnel. After collecting the filtrate, use a rotary evaporator to remove most of the solvent, add the solid after removing the solvent to a round bottom flask and add 250g of anhydrous methanol, stir it mechanically for 1h, and then use a quartz sand funnel to carry out suction filtration until half After drying, the filter cake was transferred to the flask again and 250 g of anhydrous methanol was added to stir for 1 h. After repeating the steps of washing-filtering three times, the collected solid was vacuum-dried at 60° C. for 5 h to obtain 221 g of white crystals, with a total yield of 72.3%. Utilize acid-base titration to measure the carboxyl-terminal content in the refined glycoli...

Embodiment 3

[0035] The preparation of thick glycolide is with embodiment 1.

[0036]The product crude glycolide (278g) was dissolved in a mixed solvent of 400g acetone and 400g ethyl acetate, stirred at room temperature until forming a uniform transparent solution, and filtered with a quartz sand funnel to remove powdery insolubles. After collecting the filtrate, use a rotary evaporator to remove most of the solvent, add the solid after removing the solvent into a round bottom flask and add 250g of absolute ethanol, stir it mechanically for 1h, and then use a quartz sand funnel to carry out suction filtration until half After drying, the filter cake was transferred to the flask again and 250 g of absolute ethanol was added to stir for 1 h. After repeating the steps of washing-filtering three times, the collected solid was vacuum-dried at 60° C. for 5 h to obtain 212 g of white crystals, with a total yield of 69.6%. Utilize acid-base titration to measure the carboxyl group content in the ...

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PUM

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Abstract

The invention relates to a method for purifying glycolide, which mainly solves the problem in the prior art that impurities with large molecular weights are difficult to remove in the recrystallization process. By adopting the refining method of glycolide, comprising the following steps: 1) dissolving the crude glycolide product obtained by the depolymerization reaction in solvent I, and filtering to remove insoluble matter; 2) heating and distilling the collected filtrate to remove solvent I, Obtain the crude glycolide of solid phase; 3) mix and stir the crude glycolide obtained in step 2) with solvent II, then filter the solid-liquid mixture to collect the filter cake, and repeat the operation at least 3 times to remove the filter cake Vacuum drying to obtain a refined glycolide product; wherein, the solvent I is at least one of methylene chloride, tetrahydrofuran, acetone, ethyl acetate, and 1,4-dioxane; the solvent II is alcohol The technical scheme of at least one of class, ethers, esters and ketones solves this problem well and can be used in the industrialized production of glycolide.

Description

technical field [0001] The invention relates to a method for purifying glycolide. Background technique [0002] Glycolide is a cyclic ester formed by the dehydration of two molecules of glycolic acid, and it is an important compound that can be used to prepare polyglycolic acid and its copolymers. Polyglycolic acid and its copolymers are biodegradable, can eventually degrade into carbon dioxide and water, and have excellent gas barrier properties and mechanical strength. They have been widely used in the field of biomedical materials such as surgical sutures, artificial tissues, and drug controlled release systems. application. Therefore, research on polyglycolic acid and glycolide has attracted extensive attention in recent years. [0003] In order to obtain high-molecular-weight polyglycolic acid, it is necessary to use glycolic acid as a raw material to obtain glycolide through a two-step reaction. Polyglycolic acid with a molecular weight of tens of thousands to hundr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/12
CPCC07D319/12
Inventor 朱煜王睿周文乐熊金根周芬
Owner CHINA PETROLEUM & CHEM CORP
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