Preparation method of polyethylene-b-polylactic acid amphiphilic diblock copolymer

A technology of diblock copolymer and polyethylene glycol is applied in the field of preparation of polyethylene glycol-b-polylactic acid amphiphilic diblock copolymer, and can solve the problems of high production cost, high price, complicated process, etc. question

Inactive Publication Date: 2003-04-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of anionic ring-opening polymerization process is complicated, and it is difficult to realize industrial production
[0009] The preparation methods of the above two kinds of PEG-b-PLA all use polyethylene glycol monomethyl ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 17g of 88% L-lactic acid solution and 15g of polyethylene glycol monomethyl ether with a molecular weight of 2000 into a round bottom flask, seal it, and remove water under reduced pressure at 140°C for 2 hours under the protection of nitrogen. Then 0.06 g of stannous octoate catalyst was added under normal pressure, and the melt polycondensation reaction was carried out for 8 hours at 200° C., under the pressure of 20 mmHg, and nitrogen flow. After the reaction, dissolve the product in chloroform, then add 4 to 10 parts of acetone / ether mixed solution with a volume ratio of 1:4 below 10°C for precipitation, centrifuge, and vacuum dry at 30°C to 50°C to obtain the product.

Embodiment 2

[0021] The device and operation are the same as in Example 1. Add 27g of 88% L-lactic acid solution and 6g of polyethylene glycol monomethyl ether with a molecular weight of 2000 into the flask. After sealing, remove water under reduced pressure at 140°C for 2 hours under the protection of nitrogen. . Then add 0.06 g of catalyst stannous octoate under normal pressure, and carry out melt polycondensation reaction for 8 hours at 200 DEG C, under a pressure lower than 20 mmHg, under the condition of blowing nitrogen. After the reaction, dissolve the product in chloroform, then add 4 to 10 parts of acetone / ether mixed solution with a volume ratio of 1:4 below 10°C for precipitation, centrifuge, and vacuum dry at 30°C to 50°C to obtain the product.

Embodiment 3

[0023] The device and operation are the same as in Example 1. Add 17 g of 88% L-lactic acid solution and 15 g of polyethylene glycol monomethyl ether with a molecular weight of 2000 into the flask. After sealing, remove water under reduced pressure at 140°C for 2 hours under the protection of nitrogen. . Then add catalyzer stannous octoate 0.06g under normal pressure, equimolar p-toluenesulfonic acid 0.028g, at 200 ℃, under the pressure of 20mmHg, under the condition of blowing nitrogen, carry out melt polycondensation reaction for 8 hours. After the reaction, dissolve the product in chloroform, then add 4 to 10 parts of acetone / ether mixed solution with a volume ratio of 1:4 below 10°C for precipitation, centrifuge, and vacuum dry at 30°C to 50°C to obtain the product.

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PUM

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Abstract

The preparation method of polyethylene glycol-b-polylactic acid amphiphilic diblock copolymer (PEG-b-PLA) includes the following steps: adding lactic acid liquor and monocapoped polyethylene glycol or monocapped epoxyethane and epoxypropane copolymer in polymerization still according to a certain proportion, under the protection of nitrogen gas, reducing pressure and dewatering at 120-160 deg.C, adding a proper quantity of catalyst, under the condition of 160-200 deg.C and below 20 mmHg continuously reacting to obtain crude product, using chloroform to dissolve said crude product at room temp., adding acetone/ethyl ether mixer solution at below 10 deg.C to make precipitation and separation, centrifugal separating or reduced pressure suction filtering so as to obtain the invented product which can be self-assembled into nano ball as nano carrier for control-releasing medicine.

Description

technical field [0001] The invention relates to a preparation method of polyethylene glycol-b-polylactic acid amphiphilic diblock copolymer (PEG-b-PLA). It belongs to the preparation technology of amphiphilic diblock copolymer. Background technique [0002] The structural formula of polyethylene glycol-b-polylactic acid diblock copolymer (PEG-b-PLA) is: [0003] HO[COCH(CH 3 )O] m [CH 2 CH 2 O] n R' (1) R'=CH in the formula 3 , CH 2 CH 3 and other groups. [0004] This amphiphilic diblock copolymer is biodegradable and can self-assemble into stable nanoparticles in water, which is a very potential nano drug carrier. [0005] There are mainly two kinds of preparation methods of PEG-b-PLA diblock copolymers reported in literature and patents. The first method is to use tin salt compounds as catalysts and prepare through ring-opening polymerization of polyethylene glycol monomethyl ether (mPEG) and lactide. The general reaction mechanism...

Claims

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Application Information

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IPC IPC(8): C08G65/48
Inventor 董岸杰邓联东
Owner TIANJIN UNIV
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