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A kind of preparation method of maleic anhydride modified lactic acid-glycolic acid copolymer

A technology of maleic anhydride and glycolic acid, which is applied in the field of preparation of maleic anhydride-modified lactic acid-glycolic acid copolymers, can solve the problems of high cost, unfavorable industrial production, and low water requirement for reversible equilibrium copolymerization reaction , to achieve the effect of reducing the loss

Active Publication Date: 2017-01-18
黑龙江臻旸生物科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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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 the maximum, the unreacted groups in the system should be controlled within 3 / 1000, so the reversible equilibrium copolymerization Lower moisture requirements in the reaction
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 preparation method of maleic anhydride modified lactic acid-glycolic acid copolymer
  • A kind of preparation method of maleic anhydride modified lactic acid-glycolic acid copolymer
  • A kind of preparation method of maleic anhydride modified lactic acid-glycolic acid copolymer

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specific Embodiment 1

[0028] A kind of preparation method of maleic anhydride modified lactic acid-glycolic acid copolymer, comprises the steps:

[0029] 1. Preparation of crude polylactic acid-glycolic acid copolymer:

[0030] 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 to keep boiling and dehydration for 2 hours, and obtain cyclization products such as glycolide, lactide and glycolide, stop heating, and cool down to 20°C. After opening the nitrogen valve and feeding nitrogen for 10 minutes, turn off the vacuum pump and add (m 复合催化剂 / m （乳酸+羟基乙酸） =0.2%), start the stirring device to mix evenly, close the nitrogen valve, start the vacuum pump to evacu...

specific Embodiment 2

[0036] A kind of preparation method of maleic anhydride modified lactic acid-glycolic acid copolymer, comprises the steps:

[0037] 1. Preparation of crude polylactic acid-glycolic acid copolymer:

[0038] 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 to keep boiling and dehydration for 3 hours, and obtain cyclization products such as glycolide, lactide and glycolide, stop heating, and cool down to 30°C. After opening the nitrogen valve and feeding nitrogen for 20 minutes, turn off the vacuum pump and add (m 复合催化剂 / m （乳酸+羟基乙酸） =0.5%), start the stirring device to make it evenly mixed, close the nitrogen valve, start the vacuum pump ...

specific Embodiment 3

[0044] 一种顺丁烯二酸酐改性乳酸-羟基乙酸共聚物的制备方法,包括如下步骤:

[0045] 1、聚乳酸-羟基乙酸共聚物粗品的制备:

[0046] 将一定摩尔分数(乳酸含量79%)的乳酸、羟基乙酸加入到带有温度和搅拌装置的四口烧瓶中,启动水循环真空泵和搅拌装置,减压至4860Pa抽真空29min后,打开电热套加热,但温度升至66℃时,烧瓶内出现沸腾,调节加热,使其维持沸腾脱水2.3h,得到乙交酯、丙交酯和乙丙交酯等的环化产物,停止加热,降温至23℃,打开氮气阀通入氮气14min后,关闭真空泵,加入(m 复合催化剂 / m （乳酸+羟基乙酸） =0.4%),启动搅拌装置使其混合均匀,关闭氮气阀、启动真空泵抽真空至476Pa,然后打开加热套加热至100℃左右,调节加热功率,使反应体系以1.6℃ / min的速率缓慢升温,当温度升至177℃时,保温反应至13h得到顺丁烯二酸酐-聚乳酸-羟基乙酸共聚物粗品。

[0047] 2、粗品的纯化:

[0048] 将上述所得的聚合物粗品溶于四氢呋喃和N,N-二甲基甲酰胺(四氢呋喃:N,N-二甲基甲酰胺的体积比为1:1)的混合溶液中配制成10~15%的溶液,经过滤后,再用相同体积的甲醇沉淀并过滤,将沉淀物置于真空烘箱中50~60℃下干燥10~12h,得到纯净干燥的聚乳酸-羟基乙酸共聚物的纯净物。

[0049] 3、顺丁烯二酸酐-聚乳酸-羟基乙酸共聚物的制备:

[0050] 将100g上述纯净物,0.7g过氧化二异丙苯催化剂和0.4g复合催化剂,溶于19ml丙酮的0.7g顺丁烯二酸酐加入反应器中,混合均匀,抽真空脱出丙酮,控制系统真空在400Pa,并在169℃下反应至7h停止,经过以上纯化,得到纯净的聚合物。

[0051] 根据实验,对实施的效果说明如下:

[0052] (1)顺丁烯二酸酐用量对特性粘度作用

[0053] Such as figure 1 顺丁烯二酸酐用量对特性粘度的影响曲线图所示,随着扩链剂用量的增加,共聚物特性粘度呈现先增加后下降的趋势,当扩链剂用量为4g时达到最大值。随着扩链剂用量的增加使得它与共聚物大分子碰撞的机会增加,导致顺丁烯二酸酐接枝几率变大,因此特性粘度逐渐增加。当扩链剂与大分子反应达到平衡时,继续增加扩链剂,体系中的活性基团并没有增加,变化...

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Abstract

The invention discloses a preparation method for maleic anhydride-modified poly(lactic-co-glycolic acid) copolymer. The preparation method comprises the following steps: preparing crude poly(lactic-co-glycolic acid); purifying the crude poly(lactic-co-glycolic acid); preparing maleic anhydride-modified poly(lactic-co-glycolic acid). According to the preparation method, a biodegradable material suitable for different medical situations can be prepared by changing the usage amount of maleic anhydride and regulating the molecular weight and molecular chain structure of the copolymer through adopting maleic anhydride as a modifier. In the preparation method, a medical high-molecule material with adjustable hydrophilicity and degradation rate can be synthesized by regulating the raw material ratio of lactic acid and glycolic acid.

Description

technical field [0001] The invention specifically relates to a preparation method 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): C08F283/02C08G63/08C08G63/90
Inventor 郭立强尹桂波
Owner 黑龙江臻旸生物科技有限公司