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Method of preparing polymer network by utilizing controllable click chemical reaction system

A click chemistry reaction and polymer technology, which is applied in the field of the controllable click chemistry reaction system for the preparation of polymer networks, can solve the problems of limiting the potential application of polymer gel materials, and can eliminate the formation of macroscopic defects and reduce the formation of microscopic defects. , the effect of increasing strength

Inactive Publication Date: 2014-04-02
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polymer gel materials prepared by traditional methods cannot meet the requirements of these special functions, which limits the potential application of polymer gel materials in bionic tissues and organs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] a) Synthesis of alkynyl compounds: Add pentaerythritol (2g), anhydrous N,N-dimethylformamide solvent (50ml), sodium hydroxide (12.5g) into a three-necked flask, and stir the mixture magnetically at 5°C After reacting for 30 minutes, propargyl bromide (20 g) was slowly added dropwise therein, and reacted at a temperature of 40° C. for 24 hours. Cool, add 100ml of water to the reaction product, extract the organic phase with diethyl ether, wash the organic phase with water and brine three times, then dry with anhydrous sodium sulfate, remove the diethyl ether, and use the developer ethyl acetate on the silica gel column as the residue: Alkane=1:4 separation and purification to obtain pentaerythyne.

[0028] b) Synthesis of azide compound: Polyethylene glycol 1000 (2g) was dissolved in 20ml of pyridine, methanesulfonyl chloride (2ml) was added dropwise thereto, reacted at room temperature for 12h, pyridine was removed, and dissolved in anhydrous sodium bicarbonate aqueous ...

Embodiment 2

[0034] The basic process is the same as in Example 1, the difference is that:

[0035]In step 1), the linear polyethylene glycol 1000 whose end group is azide is 0.13g (0.118mmol), 0.021g (0.073mmol) pentaerythyne, 6uL1mol / L transition metal compound copper nitrate solution, 6uL1mol / L free The tetrahydrofuran solution of the base initiator azobisisoheptanonitrile was dissolved in 1ml of tetrahydrofuran as the solvent, and 6uL of the tetrahydrofuran solution of 1mol / L ligand 2,2'-bipyridine was added, and replaced with nitrogen three times under refrigeration.

[0036] In step 2), the reaction temperature is 70° C., and the reaction time is 10 minutes to form a polymer gel network compound.

[0037] The rest are completely consistent with Example 1.

Embodiment 3

[0039] The basic process is the same as in Example 1, the difference is that:

[0040] In step b), synthesis of azide compounds: polyethylene glycol 2000 (4g) was dissolved in 20ml of pyridine, methanesulfonyl chloride (2ml) was added dropwise thereto, reacted at room temperature for 12h, pyridine was removed, and anhydrous bicarbonate was used to Neutralize the residue with sodium aqueous solution, extract 3 times with dichloromethane, spin dry the dichloromethane, precipitate the spin-dried residue with ether, obtain a solid and dry it, and dissolve the dried solid in N,N-dimethyl Add 0.8g of sodium azide to the mixed solvent of formamide and water, react at 60°C for 24h, extract with dichloromethane for 3 times, spin dry the dichloromethane, precipitate the spin-dried residue with ether, obtain a solid and dry it , that is, linear polyethylene glycol 2000 with an azide terminal group.

[0041] In step 1), the linear polyethylene glycol 2000 whose terminal group is azide is...

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Abstract

The invention discloses a method of preparing polymer network by utilizing a controllable click chemical reaction system. The method comprises the following steps: generating a free radial by utilizing a free radial initiator to initiate at a certain temperature; reducing high-valence-state metal ions into low-valence-state metal ions; and synchronously catalyzing an azide compound and an alkynyl compound to carry out click reaction. The method disclosed by the invention utilizes controllability of the free radial initiation efficiency under the temperature to synthesize the polymer network with a regular structure by the polyfunctional-group micromolecule or macromolecule azide compound and the alkynyl compound, so that generation macroscopic defects of the polymer network is avoided, formation of micro defects is reduced and regularity of the polymer network is improved, and therefore, strength of the polymer network is improved.

Description

technical field [0001] The invention belongs to the field of polymer synthesis methods, and relates to a method for preparing a polymer network with a controllable click chemical reaction system. Background technique [0002] Polymer gel network is a kind of polymer with three-dimensional network structure, and it is a special soft wet material that can swell in solvent but not dissolve. Polymer gel networks, especially hydrogels, are materials that have very similar structures and properties to human and animal biological tissues. In the gaps of the polymer network, some small molecular substances can move like in the biofilm to transmit information and substances. The polymer hydrogel with high strength, highly regular molecular structure and function has the function similar to biological membrane, so it has important applications in bionic organs with membrane function, such as artificial blood vessels, skin, eyes and artificial tissues and organs. prospect. Therefore...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00
Inventor 付国东李克文姚芳
Owner SOUTHEAST UNIV
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