Preparation method of network interpenetrating functional aquagel

A network interpenetrating, hydrogel technology, applied in the field of functional hydrogel preparation, can solve the problems of increasing phase transition temperature, reducing original polymer, reducing temperature sensitivity, etc. The effect of good capacitance and rapid response

Inactive Publication Date: 2010-07-28
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, copolymerization usually weakens or reduces some properties of the original polymer, such as preparing gel by copolymerizing N-isopropylacrylamide with monomers with hydrophilic or hydrop

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0036] Example One-terminal azido-based PEG preparation

[0037] Accurately weigh 10 g of polyethylene glycol (Mn=2000) and dissolve it in 50 ml of anhydrous pyridine. Ice bath, the temperature of the system was lowered to 0°C. Weigh 1.43g (12.5mmol) of methanesulfonyl chloride and dissolve it in 10ml of anhydrous dichloromethane.

[0038] The methanesulfonyl chloride dichloromethane solution was slowly added dropwise into the polyethylene glycol pyridine solution using a constant pressure dropping funnel at 0° C. (about 20 minutes). The reaction system was raised to room temperature, and reacted for 12 hours under magnetic stirring.

[0039] The excess solvent was distilled off and washed with saturated NaHCO 3 and dichloromethane for multiple extractions. The organic layer was dried over anhydrous magnesium sulfate. After fully drying and filtering, the clear liquid was placed in a pear-shaped flask, and the excess solvent was removed by rotary evaporation, and precipit...

example 2

[0042] Example two contains the preparation of polyethylene glycol esters of four terminal alkynyl groups

[0043] The preparation of the polyethylene glycol ester comprises the following steps:

[0044] 1. Synthesis of Diethyl Diacetylmalonate

[0045] 4.27ml of diethyl malonate, 25ml of ethanol, and 1.3g of solid sodium were placed in a 100ml round bottom flask. After the mixture was reacted for 5 minutes, 5.072ml of propyne bromide was added dropwise to the round bottom flask. After the reaction was refluxed for half an hour, the solvent was evaporated to dryness, the residue was dissolved in water and extracted three times with ether, the organic layers were combined, dried and evaporated to remove the ether to obtain a yellow oily liquid, the fractions were collected by distillation and placed in a refrigerator to obtain white crystals. Yield 80%.

[0046] 2. Synthesis of bis-alkynyl malonic acid

[0047] Add concentrated NaOH solution to the white crystals and react o...

example 3

[0052] The preparation of example tripentaerythroxypropargyl ether

[0053] Accurately weigh 2 g (0.014 mmol) of pentaerythritol and 12.5 g (0.22 mmol) of potassium hydroxide and dissolve in 25 ml of anhydrous DMF. In an ice bath, the system was kept at 5°C under magnetic stirring for 30 minutes. Under the condition of ice bath, propargyl bromide was slowly added dropwise using a constant pressure dropping funnel (dropping was completed in about 30 minutes). Then the reaction system was heated to 40°C overnight.

[0054] Stop stirring and cool to room temperature, add 100ml deionized water. Diethyl ether was extracted several times. The organic layer was washed several times with deionized water and saturated saline respectively. Dry over anhydrous magnesium sulfate overnight. After fully drying and filtering, the supernatant was placed in a pear-shaped bottle, and the excess solvent was evaporated by rotary evaporation. Separation and purification by column chromatograp...

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PUM

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Abstract

The invention discloses a method for preparing network interpenetrating functional aquagel through the click chemistry and the atom transfer radical polymerization (ATRP) synchronous reaction. The polymer network is generated through the click reaction of monomers A containing three or more than three end alkynyl radicals and monomers B at least containing two end laminated nitrogen radicals, and network interpenetrating polymers are obtained through the atom transfer radical polymerization (ATRP) by double-bond-containing monomers C with functional groups. The click chemistry and the atom transfer radical polymerization are synchronously carried out in the same catalytic system, and the network interpenetrating functional aquagel with the regular structure is obtained. The method of the invention has the advantages of the click chemistry and the ATRP, and also has the advantages of simple operation and fast reaction. The functional aquagel prepared by the method of the invention based on polyethyleneglycol has the characteristics of good biocompatibility, high tensile strength, high water absorption capacity, high swelling ratio, regular structure and the like.

Description

technical field [0001] The invention relates to a preparation method of a functional hydrogel, in particular to a preparation method of a network interpenetrating functional hydrogel. Background technique [0002] The application of polymer functional gels has attracted more and more attention, and its special properties have also attracted more and more people's interest. The so-called functional gel refers to a class of polymers that can perceive small stimuli or changes in the external environment (such as temperature, pH value, light, magnetism, electricity or pressure, etc.), and at the same time produce corresponding chemical properties and physical structure changes. gel. It is precisely because of the intelligence of this kind of polymer gel that it may be applied in many fields, especially in biomedical fields such as drug sustained release, protein separation and purification, and active enzyme embedding. . However, due to the low mechanical strength of the gel ...

Claims

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Application Information

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IPC IPC(8): C08F291/00C08F291/06C08F291/12
Inventor 付国东付蓉
Owner SOUTHEAST UNIV
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