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A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer

A technology of glycolic acid and maleic anhydride, which is applied in the field of synthesis of maleic anhydride-modified lactic acid-glycolic acid copolymer, can solve the problems of high cost, complicated process, high operating cost, etc., and achieve the effect of reducing losses

Inactive Publication Date: 2016-04-13
NANTONG TEXTILE VOCATIONAL TECH COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But in the synthetic technology of above-mentioned maleic anhydride-lactic acid copolymer, there is following defect: 1, maleic anhydride is only aimed at the modification of polylactic acid
2. The method of ring-opening polymerization is adopted, the process is complicated, the yield is low, and the cost is high
[0006] But this method has the following two unfavorable factors: 1. In the synthesis of high molecular weight polylactic acid-glycolic acid, when the molecular weight of the copolymer reaches 50,000, the unreacted groups in the system should be controlled within 3 / 1000, so the reversible Lower moisture requirement in equilibrium copolymerization
2. The vacuum degree of the reaction system is generally within 130Pa, and the operating cost is high, which is not conducive to the realization of industrial production

Method used

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  • A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer
  • A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer
  • A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer

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specific Embodiment 1

[0025] A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer, comprises the steps:

[0026] 1), the preparation of maleic anhydride-polylactic acid-glycolic acid copolymer crude product:

[0027] Add a certain mole fraction (50% lactic acid content) of lactic acid and glycolic acid into a four-necked flask with a temperature and stirring device, start the water circulation vacuum pump and stirring device, decompress to 4000Pa and vacuumize for 20 minutes, turn on the electric heating mantle to heat, But when the temperature rises to 63°C, boiling occurs in the flask, adjust the heating rate to keep boiling and dehydration for 2 hours, to obtain cyclization products such as glycolide, lactide and glycolide, stop heating, and cool down to 80°C , open the nitrogen valve to feed nitrogen for 10 minutes, turn off the vacuum pump, add (m 复合催化剂 / m （乳酸+羟基乙酸） =0.2%) composite catalyst and (m 复合催化剂 / m （乳酸+羟基乙酸） =2%) maleic anhydride, start th...

specific Embodiment 2

[0030] A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer, comprises the steps:

[0031] 1), the preparation of maleic anhydride-polylactic acid-glycolic acid copolymer crude product:

[0032] Add a certain mole fraction (99% lactic acid content) of lactic acid and glycolic acid into a four-necked flask with temperature and stirring device, start the water circulation vacuum pump and stirring device, decompress to 6000Pa and vacuumize for 40 minutes, turn on the electric heating mantle to heat, But when the temperature rises to 68°C, boiling occurs in the flask, adjust the heating rate to keep boiling and dehydration for 3 hours to obtain cyclization products such as glycolide, lactide and glycolide, stop heating, and cool down to 90°C , open the nitrogen valve to feed nitrogen for 20min, turn off the vacuum pump, add (m 复合催化剂 / m （乳酸+羟基乙酸） =0.5%) composite catalyst and (m 复合催化剂 / m （乳酸+羟基乙酸） =10%) maleic anhydride, start the stirr...

specific Embodiment 3

[0035] A kind of synthetic technique of maleic anhydride modified lactic acid-glycolic acid copolymer, comprises the steps:

[0036] 1), the preparation of maleic anhydride-polylactic acid-glycolic acid copolymer crude product:

[0037]Add a certain mole fraction (90% lactic acid content) of lactic acid and glycolic acid into a four-necked flask with temperature and stirring device, start the water circulation vacuum pump and stirring device, decompress to 5000Pa and vacuumize for 30 minutes, turn on the electric heating mantle to heat, However, when the temperature rises to 65°C, boiling occurs in the flask. Adjust the heating rate to maintain boiling and dehydration for 2.5 hours to obtain cyclization products such as glycolide, lactide, and glycolide. Stop heating and cool down to 85°C. ℃, open the nitrogen valve and let in nitrogen for 15 minutes, then turn off the vacuum pump and add (m 复合催化剂 / m （乳酸+羟基乙酸） =0.3%) composite catalyst and (m 复合催化剂 / m （乳酸+羟基乙酸） =8%) maleic...

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Abstract

The invention discloses a synthetic process for maleic anhydride-modified poly(lactic-co-glycolic acid). The synthetic process comprises the following steps: preparing crude product maleic anhydride-poly(lactic-co-glycolic acid); purifying the crude product maleic anhydride-poly(lactic-co-glycolic acid). According to the synthetic process, the preparation and purification of lactide, glycolide or lactic-co-glycolic acid in ring-opening polymerization reaction can be omitted, the loss of intermediates can be reduced, and the utilization rate of main ingredients of lactic acid, glycolic acid and the like can achieve 80-90%. By utilizing maleic anhydride as a modifier, on one hand, a series of oligomer can be formed by utilizing a cyclic anhydride structure contained in the molecules in a manner of ring-opening polymerization together with lactide, glycolide or lactic-co-glycolic acid, on the other hand, maleic anhydride molecules contain unsaturated double bonds which can generate additional polymerization reaction under high-temperature condition in the presence of a catalyst, to form a chain type high-molecular polymer with a plurality of poly(lactic-co-glycolic acid) side chains.

Description

technical field [0001] The invention specifically relates to a synthesis process of a maleic anhydride-modified lactic acid-glycolic acid copolymer. Background technique [0002] The copolymerization of lactic acid and glycolic acid is a condensation polymerization reaction, and its synthesis routes mainly include ring-opening polymerization and direct polycondensation. The ring-opening polymerization method is the most traditional synthesis method of PLGA. According to its synthetic polymer, it can be divided into two types: random copolymer (Ran-PLGA) and alternating copolymer (Alt-PLGA). Random PLGA copolymers use lactide and glycolide as comonomers, and undergo ring-opening polymerization according to different feed ratios to form PLGA polymers with different compositions. However, due to the different competitive Polymerization rate, it is difficult to strictly control the degree of randomness and composition reproducibility of Ran-PLGA, especially when the feed ratio ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/78
Inventor 郭立强艾亚菲
Owner NANTONG TEXTILE VOCATIONAL TECH COLLEGE