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A method for preparing polymer network using rare earth catalyzed click chemistry system

A technology of click chemistry and rare earth catalysis, which is applied in the field of polymer network preparation using rare earth catalyzed click chemistry system, can solve the problems of limiting the potential application of polymer gel materials, and achieve the effect of simple method and mild reaction conditions

Inactive Publication Date: 2017-02-22
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymer gel materials prepared by the traditional click method cannot meet the requirements of these special functions, which limits the potential application of polymer gel materials in functional materials of life, environment and medical science

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] a) Synthesis of terminal alkynyl compounds: Accurately weigh 5g of polyethylene glycol (Mn=2000) and 0.432g of sodium hydride, dissolve it in 50ml of anhydrous tetrahydrofuran solvent at room temperature, stir for 3 hours in a nitrogen atmosphere, and accurately weigh Propylene bromide (3ml) was dissolved in 20ml of anhydrous tetrahydrofuran. Under the condition of 0°C, the propyne bromide tetrahydrofuran solution was slowly added dropwise into the polyethylene glycol tetrahydrofuran solution using a liquid funnel under constant pressure. Slowly warm up to room temperature, and react for 24 hours under magnetic stirring. The obtained product was removed with neutral alumina and diatomaceous earth to remove unreacted sodium hydride and by-product salts, the obtained solution was rotary evaporated to remove tetrahydrofuran, and the remaining product was precipitated in ether to obtain 4.5 g of white powder.

[0030] b) Synthesis of polyterminal azido compounds: add 3.2g ...

Embodiment 2

[0037] The basic process is the same as in Example 1, the difference is that:

[0038] In step 1), the multi-terminal azido polyethylene glycol derivative (M n =10000) is 0.4g (0.04mmol), 0.16g (0.08mmol) terminal alkynyl polyethylene glycol derivative (M n =2000), 5uL 1mol / L rare earth metal inorganic compound neodymium chloride solution, 5uL 1mol / L free radical initiator azobisisoheptanonitrile tetrahydrofuran solution, solvent 1ml tetrahydrofuran dissolving, under the protection of nitrogen, the reaction temperature is 70 ℃, the reaction time is 1h to form a polymer gel network compound.

[0039] In step 2), the reacted polymer gel network is taken out, put into a methanol solution to remove unreacted reactants remaining in the polymer network, and a regular polymer network is obtained after drying.

[0040] The rest are completely consistent with Example 1.

Embodiment 3

[0042] The basic process is the same as in Example 1, the difference is that:

[0043] In step a), the synthesis of terminal alkynyl compounds: Accurately weigh 5 g of polyethylene glycol (Mn=1000) and 0.8 g of sodium hydride at room temperature and dissolve in 50 ml of anhydrous tetrahydrofuran solvent, and stir for 3 hours in a nitrogen atmosphere. Accurately weigh propargyl bromide (6ml) and dissolve in 20ml of anhydrous tetrahydrofuran. Under the condition of 0°C, the propyne bromide tetrahydrofuran solution was slowly added dropwise into the polyethylene glycol tetrahydrofuran solution using a liquid funnel under constant pressure. Slowly warm up to room temperature, and react for 24 hours under magnetic stirring. The obtained product was removed with neutral alumina and diatomaceous earth to remove unreacted sodium hydride and by-product salts, the obtained solution was rotary evaporated to remove tetrahydrofuran, and the remaining product was precipitated in ether to o...

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Abstract

The invention discloses a method for preparing a polymer network by utilizing a rare-earth catalytic click chemistry system. The method comprises the following steps: generating free radicals under initiation of a certain temperature by utilizing a free radical initiator, reducing high-valence rare earth metal ions into low-valence rare earth metal ions, and performing synchronous catalysis on an alkynyl compound and an azide to carry out a click reaction. According to the method disclosed by the invention, the controllability of the free radical initiation efficiency at the temperature is utilized, and an organic compound containing three or more than three multi-terminal azide groups and an organic compound containing at least two terminal alkynyl groups are used for synthesizing the polymer network with a regular structure according to the method. According to the method disclosed by the invention, the operation is simple, a ligand is not needed, the reaction materials are readily available, the reaction is rapid, and the reaction conditions are mild. Moreover, the polymer network prepared by the method disclosed by the invention has high biocompatibility, regular structure and high mechanical strength and the advantages of rare-earth metallic magnetism, fluorescence, conductivity, catalytic performance and the like.

Description

technical field [0001] The invention belongs to the field of polymer synthesis methods, and relates to a method for preparing a polymer network by using a rare earth catalyzed click chemistry system. Background technique [0002] Due to the special structure of rare earth elements (rare earth elements have an unfilled 4f electron layer structure, and thus produce a variety of electronic energy levels), they have many optical, electrical, and magnetic properties that other elements do not have. It can be prepared into many new materials that can be applied to high-tech, so it is known as the "treasure house" for building new materials in the information age. [0003] "Click chemistry" is an organic synthesis method with fast chemical reaction, high yield, few by-products, mild reaction conditions and high stereoselectivity. It was proposed by Sharpless, the winner of the Nobel Prize in Chemistry in 2001, and its core is a new chemical synthesis method based on the heteroatom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00
Inventor 付国东李扬姚芳
Owner SOUTHEAST UNIV
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