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Hybrid polymerization amphiphilic block copolymer, synthesis method and application thereof

A technology of amphiphilic block and synthesis method, which is applied in the field of synthesis of hybrid polymerization block copolymers, can solve the problems of less research, less free radical hybrid polymerization, unclear reaction conditions, etc., and achieve simple separation and purification, Excellent controllability of the polymerization reaction

Active Publication Date: 2020-06-09
FUDAN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] At present, the methods of anionic and cationic hybrid polymerization are widely used, but there are few types of monomers suitable for free radical hybrid polymerization.
In addition, there are few studies on this type of polymerization reaction, and the reaction conditions are still unclear, so it still needs to be explored

Method used

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  • Hybrid polymerization amphiphilic block copolymer, synthesis method and application thereof
  • Hybrid polymerization amphiphilic block copolymer, synthesis method and application thereof
  • Hybrid polymerization amphiphilic block copolymer, synthesis method and application thereof

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preparation example Construction

[0053] In addition, the embodiment of the present invention discloses a method for synthesizing an amphiphilic block copolymer with controllable molecular weight and molecular weight distribution and applying anionic hybrid polymerization. The synthesis method specifically includes the following steps:

[0054] (1) Macromolecular polyethylene glycol is dissolved in toluene, and anhydrous PEG toluene solution is obtained by azeotropic water removal;

[0055] (2) cooling the toluene solution to room temperature, adding anhydrous methyl methacrylate and lactone or lactide monomers under an inert gas atmosphere, and then adding a phosphazene base catalyst to obtain a mixed reaction solution;

[0056] (3) seal the mixed reaction solution in an oil bath at a predetermined temperature for a predetermined time, and terminate the polymerization with a mixed solution of hydrochloric acid and methanol (the volume ratio of hydrochloric acid and methanol is 1:20) to obtain a product solutio...

Embodiment 1

[0066] Weigh 0.5 mmol of polyethylene glycol (molecular weight: 1000, 0.500 g) into a reaction flask, add 20 mL of toluene, and carry out azeotropic water removal under the protection of argon. When about 5 mL of toluene remains in the reaction bottle, stop heating. The toluene solution was cooled to room temperature, the argon was replaced three times, and 2 mmol (0.2 g) of anhydrous methyl methacrylate and 8 mmol (0.912 g) of anhydrous ε-hexane were added to the system with a syringe under the protection of argon. Lactone monomer, finally add 0.1mL of t-BuP via syringe 4 Catalyst n-hexane solution to obtain a mixed solution. The mixed solution was locked in an oil bath at 25° C. for 12 hours, and the polymerization was terminated with a mixed solution of hydrochloric acid and methanol (the volume ratio of hydrochloric acid and methanol was 1:20) to obtain a product solution. The product solution was added dropwise into glacial ether for sedimentation treatment, the superna...

Embodiment 2

[0069]Weigh 0.5 mmol of polyethylene glycol monomethyl ether (molecular weight: 550, 0.275 g) into a reaction flask, add 20 mL of toluene, and perform azeotropic water removal under the protection of argon. When about 5 mL of toluene remains in the reaction bottle, stop heating. The toluene solution was cooled to room temperature, the argon was replaced three times, and 2 mmol (0.2 g) of anhydrous methyl methacrylate and 16 mmol (1.824 g) of anhydrous ε-hexane were added to the system with a syringe under the protection of argon. Lactone monomer, finally add 0.1mL of t-BuP via syringe 4 Catalyst n-hexane solution to obtain a mixed solution. The mixed solution was locked in an oil bath at 25° C. for 12 hours, and the polymerization was terminated with a mixed solution of hydrochloric acid and methanol (the volume ratio of hydrochloric acid and methanol was 1:20) to obtain a product solution. The product solution was added dropwise into glacial ether for sedimentation treatmen...

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Abstract

The invention belongs to the field of biomedical polymer materials, discloses a hybrid polymerization amphiphilic block copolymer, a synthesis method and application thereof, and particularly relatesto a method for obtaining an amphiphilic block copolymer through macromolecular polyethylene glycol initiation and hybrid polymerization of methyl methacrylate, lactone and lactide monomers. Accordingto the invention, the hybrid polymerization amphiphilic block copolymer disclosed by the invention has controllable molecular weight and molecular weight distribution and a special molecular structure, wherein side chain functional groups such as ester groups and the like can be introduced into the polyester chain segment of the block copolymer; in the presence of a catalyst phosphazene base (t-BuP4), macromolecular alcohols such as polyethylene glycol, polyethylene glycol monomethyl ether and other macromolecules are used as initiators, and methyl methacrylate, caprolactone and other lactones and lactide monomers are subjected to one-step hybrid copolymerization to obtain the polymer; and the hybrid polymerization amphiphilic block copolymer can form micelles in an aqueous solution, canbe used as a novel polyester biomedical material, and is potentially applied to drug loading and delivery.

Description

technical field [0001] The invention relates to a synthesis method of a hybrid polymerized block copolymer, in particular to a hybrid polymerized amphiphilic block copolymer and its synthesis method and application, especially a kind of macromolecule polyethylene glycol initiated, A method for obtaining an amphiphilic block copolymer through hybrid polymerization of methyl methacrylate and lactone or lactide monomers. Background technique [0002] Biomedical polymer materials have many advantages such as good biocompatibility and easy-to-adjust degradability, and are an important content of biomedical material research. They have broad application prospects in drug delivery systems, tissue engineering and other fields. Among them, amphiphilic block copolymers are one of the most widely used biomedical polymer materials. However, most of them are polyester materials with a relatively simple structure, which is not enough to load various drugs with different structures and fu...

Claims

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Application Information

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IPC IPC(8): C08G63/664C08G63/78C08F293/00C08F220/14A61K47/34
CPCC08G63/664C08G63/78C08F293/005C08F220/14A61K47/34
Inventor 俞麟吴凯婷丁建东
Owner FUDAN UNIV
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