Synthetic method of polylactic acid-polyethylene glycol

A polyethylene glycol and synthesis method technology, applied in the field of material chemistry, can solve the problems of application limitation, high cost, low molecular weight of polylactic acid-polyethylene glycol, etc., and achieve complete degradation cycle, short degradation cycle and fast reaction rate Effect

Inactive Publication Date: 2012-08-08
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the high cost of lactide makes the manufacturing cost of polylactic acid-polyethylene glycol very high, and the application is limited
The second is to use lactic acid and polyethylene glycol to directly polymerize and synthesize under the joint action of stannous octoate and p-toluenesulfonic acid. Although this method reduces the reaction steps, due to the low catalytic efficiency of the catalyst, the prepared polylactic acid-polymer The molecular weight of ethylene glycol is low, and the application of copolymers in the medical field is greatly limited due to the residue of traditional catalysts

Method used

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  • Synthetic method of polylactic acid-polyethylene glycol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Firstly, the L-lactic acid to be reacted was dried with 5A molecular sieve for 2-3 hours, and then placed for use. In a 250 ml reaction flask, add 200 grams of preliminarily dried L-lactic acid, 22 grams of PLEG with a molecular weight of 400, and 0.1 grams of 1,3-dimethylimidazole p-toluenesulfonate, then heat to reflux and control with a vacuum pump The pressure in the reaction bottle is 800Pa, 170°C, stir and react for 6 hours, then slowly cool down to room temperature to obtain a brownish-yellow solid, add 50 ml of chloroform solvent, stir and dissolve the reactant, and then add it dropwise while stirring with methanol until it becomes cloudy , and a precipitate slowly precipitated out, and stood still for 1 hour. After the precipitation was completed, the crude product was obtained by vacuum filtration. Then recrystallize with chloroform-acetone complex solvent to obtain refined polylactic acid-polyethylene glycol product. The molecular weight of the copolymer was...

Embodiment 2

[0028]Firstly, the L-lactic acid to be reacted was dried with 5A molecular sieve for 2-3 hours, and then placed for use. In a 250 ml reaction flask, add 200 grams of preliminarily dried L-lactic acid, 25 grams of PLEG with a molecular weight of 600, 0.1 gram of 1-ethyl-3-methylimidazole p-toluenesulfonate, and then heat to reflux, And use a vacuum pump to control the pressure in the reaction bottle to be 800 Pa, 170 ° C, stir and react for 6 hours, then slowly cool down to room temperature, add 50 ml of chloroform solvent, stir and dissolve the reactant, then add dropwise while stirring with methanol until turbidity occurs, And a precipitate slowly precipitated out, and stood still for 1 hour. After the precipitation was completed, the crude product was obtained by vacuum filtration. Then recrystallize with chloroform-acetone complex solvent to obtain refined polylactic acid-polyethylene glycol product. The molecular weight of the copolymer was measured by GPC, the thermal an...

Embodiment 3

[0030] Firstly, the L-lactic acid to be reacted was dried with 5A molecular sieve for 2-3 hours, and then placed for use. In a 500 ml reaction bottle, add 300 grams of preliminarily dried L-lactic acid, 35 grams of PLEG with a molecular weight of 1000, 0.1 gram of 1-ethyl-2,3-dimethylimidazole methanesulfonate, and then heat to Reflux, and use a vacuum pump to control the pressure in the reaction bottle to 600 Pa, 175 ° C, stir for 6 hours, then slowly cool down to room temperature, add 80 ml of chloroform solvent, stir and dissolve the reactant, and then add it dropwise while stirring with methanol until it appears It was turbid, and a precipitate slowly precipitated out. After standing still for 1 hour, the precipitation was completed, and the crude product was obtained by vacuum filtration. Then recrystallize with chloroform-acetone complex solvent to obtain refined polylactic acid-polyethylene glycol product. The molecular weight of the copolymer was measured by GPC, the ...

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Abstract

The invention discloses a synthetic method of polylactic acid-polyethylene glycol, which utilizes L-lactic acid and polyethylene glycol as raw materials to synthesize the polylactic acid-polyethylene glycol in a polymerization mode, and utilizes ionic liquid as a catalytic agent. Due to the fact that the ionic liquid has good dissolving characteristics to product polymerization, the polymerization reaction is performed under conditions of the homogeneous reaction, good catalysis is obtained, the reaction rate is fast, and a product with high molecular weight can be obtained within 6-10 hours. Matter in the ionic liquid is dissoluble and can be dissolved in the solvent in the final settlement of the product, so that the product is free of residues, and residual poisons do not need to be considered in the prepared product. The preparation of the ionic liquid can perform screening according to reaction products of the polymerization, good crystal products can be obtained, degradation of the product can be facilitated, the degradation period is short, and the degradation is complete.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, and in particular relates to a synthesis method of polylactic acid-polyethylene glycol. Background technique [0002] As an excellent biodegradable polymer material, polylactic acid has been widely used in the field of clinical medicine. But with the development of medicine, polylactic acid alone can no longer meet the requirements. For example, the degradation rate of polylactic acid is very fast, the degradation cycle is difficult to control, and the strength of the body decreases rapidly after erosion. In addition, polylactic acid is brittle, has poor impact resistance, is hard and tough, lacks flexibility and elasticity, and is extremely easy to bend. Deformation etc. However, the degradation performance, crystallinity, hydrophilicity and mechanical properties of polylactic acid can be improved by plasticizing, copolymerizing, blending, molecular modification, compounding and oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/664C08G63/87
Inventor 任会学应汉杰
Owner NANJING UNIV OF TECH
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