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One-step synthetic method of degradable branched polyester

A synthesis method and one-step technology, which are applied in the field of one-step synthesis of degradable branched polyesters, can solve problems such as inability to realize industrialization, cumbersome preparation process, and limited methods, and achieve wide application range, simple polymerization process, and branched polyester. controllable effect

Active Publication Date: 2013-12-04
安徽壹敏新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are limited methods for synthesizing degradable branched polyesters, and the preparation process is cumbersome. It is necessary to prepare self-initiating monomers or branched monomers in advance, which cannot be industrialized.

Method used

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  • One-step synthetic method of degradable branched polyester
  • One-step synthetic method of degradable branched polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 1.1g (10mmol) of caprolactone and 24.2μL (0.2mmol) of hydroxyethyl methacrylate, put them in a 25mL sealed tube with a rotor, then add 0.4g of toluene as a solvent, freeze in liquid nitrogen, and replace argon three times. Immediately inject 20 μL (0.02 mmol) of t-BuP under argon atmosphere 4 of n-hexane solution, sealed the tube, placed in an oil bath at 60 °C, and reacted for 2 h. After the reaction, dissolve the reaction product with tetrahydrofuran and add 5 mL of 10 wt% hydrochloric acid solution and 10 mL of ethanol to terminate the reaction and wash the branched polycaprolactone, and then use 100 mL of n-hexane to fully wash the polymer under rapid stirring to remove unreacted. Monomer, (protonated) t-BuP 4 and toluene, filtered, vacuum dried at 50 °C for 12 h, molecular weight was 1.23′10 5 g / mol.

Embodiment 2

[0028] Take 6.6g of caprolactone (60mmol) and 24.2μL (0.2mmol) of hydroxyethyl methacrylate, put them in a 25mL sealed tube with a rotor, then add 3.3g of toluene as a solvent, freeze in liquid nitrogen, and replace argon three times. Immediately inject 1 mL (1 mol) of t-BuP under argon atmosphere 4 of n-hexane solution, sealed the tube, placed in an oil bath at 60 °C, and reacted for 2 h. After the reaction, dissolve the reaction product with tetrahydrofuran and add 5 mL of 10 wt% hydrochloric acid solution and 20 mL of ethanol to terminate the reaction and wash the branched polycaprolactone, and then use 200 mL of n-hexane to fully wash the polymer under rapid stirring to remove unreacted. Monomer, (protonated) t-BuP 4 and toluene, filtered, vacuum dried at 50 °C for 0.5 h, molecular weight was 2.41′10 5 g / mol.

Embodiment 3

[0030] Take 1.1 g (10 mmol) of caprolactone and 24.2 μL (0.2 mmol) of hydroxyethyl methacrylate, put them in a 25 mL sealed tube with a rotor, then add 0.6 g of toluene as a solvent, freeze with liquid nitrogen, and replace argon three times. Immediately inject 60 μL of t-BuP under argon atmosphere 4 The n-hexane solution was sealed, and the tube was placed in an acetone / liquid nitrogen system at -100 °C to react for 2 h. After the reaction, dissolve the reaction product with tetrahydrofuran and add 5 mL of 10 wt% hydrochloric acid solution and 10 mL of ethanol to terminate the reaction and wash the branched polycaprolactone, and then use 100 mL of n-hexane to fully wash the polymer under rapid stirring to remove unreacted. Monomer, (protonated) t-BuP 4 and toluene, filtered, vacuum dried at 50 °C for 48 h, molecular weight was 1.51′10 5 g / mol.

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Abstract

The invention discloses a one-step synthetic method of degradable branched polyester, and belongs to the technical field of polymer synthesis. According to the method, a reactive monomer comprises internal ester, anhydride, cyclic carbonate and the like; a self-initiated monomer comprises acrylic acid hydroxy ester and a methacrylic acid hydroxy ester compound, and a catalyst is a phosphine nitrile alkali compound structurally containing a double bond in which P is equal to N. The one-step synthetic method has the advantages that all raw materials for the polymerization reaction are commercialized and the conditions of the polymerization reaction are mild, is suitable for industrialized production, has an excellent application prospect, and is mainly used for the technical field of the polymer synthesis.

Description

technical field [0001] The invention relates to a one-step synthesis method of degradable branched polyester, belonging to the technical field of polymer synthesis. [0002] Background technique [0003] Aliphatic polyesters are a class of degradable, environmentally friendly, and biocompatible polymers, which have broad application prospects in medicine, agriculture, and coatings. However, since most aliphatic polyesters are partially crystalline polymers, their degradation rate is slow, which limits their applications. [0004] Hyperbranched polymers are a class of highly branched macromolecules with three-dimensional structures, which have potential applications in coatings, drug carriers, and processing aids. The introduction of branched structures in polyesters can effectively control the crystallization behavior of polymers and reduce the crystallinity of polyesters. At present, there are limited methods for synthesizing degradable branched polyesters, and the prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/08C08G63/87C08G64/30
Inventor 杨宏军钱小磊张广照蒋必彪黄文艳
Owner 安徽壹敏新材料有限公司
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