Method for preparing biomedical polyether/polyester block copolymer

A polyester block and biomedical technology is applied in the preparation of polyether and polyester block copolymers, and the preparation of biomedical polyether/polyester block copolymers. The problems of low yield of copolymer and long reaction time can achieve the effect of easy control of reaction conditions, good molecular weight uniformity and shortened reaction time.

Active Publication Date: 2011-09-14
上海谊众药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: in the process of adding lactone and catalyst, the reaction system is inevitably in contact with the outside world, and it is very easy to bring in moisture in the air, and the lactone is very easy to hydrolyze in the molten state
However, this method has the following obvious disadvantages: firstly, the polymerization activity of lactic acid is low, and a large amount of lactic acid remains in the final product, and it is necessary to remove the remaining lactic acid monomer through repeated dissolution-precipitation. Low, and the stability between batches of products is poor, and the harmful heavy metal catalysts cannot be effectively removed in the repeated precipitation process
In addition, due to the high temperature of polycondensation and the long reaction time, the product is easy to oxidize and turn yellow.
Therefore, the above method is generally not suitable for the preparation of biomedical copolymer materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 26.5g polyethylene glycol monomethyl ether (molecular weight 2000), 25.8g D,L-lactide were added to a fully dried polymerization bottle, and 1mL of 0.1g / mL stannous octoate / dichloromethane solution was added. Heat the polymerization flask to 80° C. with an oil bath to dissolve the polyethylene glycol monomethyl ether, turn on the stirring and evacuated to remove the residual water and dichloromethane in the system. After 6 hours, the polymerization bottle was melt-sealed under vacuum, and the polymerization bottle was placed in an oil bath at 180° C. for polymerization for 1 hour. After breaking the polymerization bottle, the product was dissolved in deionized water. After stirring at room temperature for 24 hours, the temperature was raised to 70 °C, and the polymer was precipitated. The precipitate was vacuum-dried, dissolved in dichloromethane, and centrifuged at 10,000 rpm for 10 minutes. The liquid was precipitated with a large amount of anhydrous ether and dried i...

Embodiment 2

[0036] 20 g of polyethylene glycol (molecular weight 2000) and 14.4 g of L-lactide were added to a fully dried polymerization bottle, and 0.7 mL of a diethylzinc / toluene solution with a concentration of 0.1 g / mL was added. The polymerization flask was heated to 80° C. with an oil bath to dissolve the polyethylene glycol, and the stirring was turned on and vacuum was applied to remove the residual moisture and toluene in the system. After 6 hours, the polymerization bottle was melt-sealed under vacuum, and then the polymerization bottle was placed in an oil bath at 150° C. for polymerization for 2.5 hours. After breaking the polymerization bottle, the product was dissolved in dichloromethane, deionized water was added and stirred at room temperature for 24 hours. The organic layer was dried with anhydrous magnesium sulfate and then centrifuged at 10,000 rpm for 10 minutes. The supernatant was precipitated with a large amount of methanol and then vacuum-dried. get the final prod...

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PUM

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Abstract

The invention belongs to the technical field of biological materials and particularly relates to a method for preparing a biomedical polyether/polyester block copolymer. In the method, the polyether/polyester block copolymer is prepared by triggering lactone to perform ring-opening polymerization under the vacuum condition by using fully dried polyether. The method comprises the following steps of: adding polyether, the lactone and a catalyst into a polymerization bottle; and heating and vacuumizing the polymerization bottle to remove moisture and solvent remained in a polymerization system to prepare the polyether/polyester block copolymer. The method is simple and practicable, the reaction conditions are easy to control, and a series of copolymers with different molecular weights can be obtained only by controlling the feed ratio of the polyether to the lactone; the reaction time can be shortened by a polymerization process so as to avoid side reaction, and the obtained copolymer has a stable structure, and high uniformity of molecular weight; and the content of the unreacted monomer and a heavy metal catalyst is extremely low, and the requirements of biomedical materials can be met.

Description

technical field [0001] The invention belongs to the technical field of biological materials, and relates to a preparation method of a polyether and polyester block copolymer, in particular to a preparation method of a biomedical polyether / polyester block copolymer. Background technique [0002] In recent years, nanotechnology-based drug delivery methods have attracted great attention from researchers. Among them, the nanomicellar carrier system formed by self-assembly of amphiphilic block copolymers in aqueous solution has become a new type of drug carrier with great application prospects. At present, there is a lot of evidence that polymer nanomicelles have unique advantages compared with other drug carriers: resistance to dilution, stable structure in blood; long circulation characteristics; small particle size of micelles Leaky vascular areas (such as tumor sites) have stronger penetration capacity and have more opportunities to accumulate at the target site; the targeti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/664C08G63/78
Inventor 龚飞荣孙菁李端周劲松沈亚领
Owner 上海谊众药业股份有限公司
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