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Preparation method of temperature, pH and ultraviolet multi-stimuli-responsive semi-interpenetrating network nanocomposite hydrogel

A semi-interpenetrating network and nano-composite technology, which is applied in the field of preparation of smart gels, can solve problems such as inability to compound, high hydrophilicity requirements, and difficulties in multi-response nano-composite gels.

Inactive Publication Date: 2014-11-26
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reason why it is difficult to prepare multi-response nanocomposite gels is that clay, as a hydrophilic substance, needs to be synthesized in a water solvent as a cross-linking agent, which requires high hydrophilicity of monomers, which is also a problem for some The synthesis of nanocomposite gels with functional monomers sets obstacles, such as lipophilic monomers, which cannot be complexed

Method used

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  • Preparation method of temperature, pH and ultraviolet multi-stimuli-responsive semi-interpenetrating network nanocomposite hydrogel
  • Preparation method of temperature, pH and ultraviolet multi-stimuli-responsive semi-interpenetrating network nanocomposite hydrogel
  • Preparation method of temperature, pH and ultraviolet multi-stimuli-responsive semi-interpenetrating network nanocomposite hydrogel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 3.6g of 4-(4-hydroxyphenylazo)benzoic acid in 100mL of anhydrous tetrahydrofuran, add 3.5mL of triethylamine, mix well, place in an ice-water bath to cool for 30 minutes, and slowly add 5mL of acryloyl chloride diluted with 60mL of anhydrous tetrahydrofuran, reacted at room temperature for 24h after dripping, added water to precipitate the product, filtered to obtain a crude product, washed with distilled water until neutral, and obtained a yellow powdery solid. Dissolve the yellow powdery solid in 120mL tetrahydrofuran, slowly adjust the pH of the system to 7 with aqueous sodium bicarbonate, stir at room temperature for 24 hours, precipitate with dilute aqueous hydrochloric acid, filter to obtain a yellow solid, wash with distilled water until neutral, and obtain a pure product , The yield is 92%. (back example all adopts this method to prepare this monomer)

[0031] Dissolve 4g of NIPA, 0.17g of 4-[(4-acryloyloxy)phenylazo]benzoic acid, 0.96g of lithium diat...

Embodiment 2

[0033] Dissolve 4g of NIPA, 0.22g of 4-[(4-acryloyloxy)phenylazo]benzoic acid, 1.22g of lithium diatomaceous earth, and 0.094g of sodium pyrophosphate in 40g of water and place it in a container at 0°C under nitrogen protection. Stir in an ice bath for 120 minutes until uniform and transparent, then add 0.6g of CMC, and continue stirring for 2 hours to obtain a uniform and transparent pre-polymerization solution; dissolve 0.04g of KPS and 0.03g of TEMED in 2g of water, stir well and add to the pre-polymerization solution, under nitrogen protection Stir rapidly for 2 minutes until uniform; then pour into a mold of a certain shape and react at 0°C for 24 hours, and then react at room temperature for 24 hours. After the obtained gel is taken out, the product is obtained by soaking and changing water repeatedly in deionized water.

Embodiment 3

[0035] 4.5g NIPA, 0.2g 4-[(4-acryloyloxy) phenyl azo] benzoic acid, 2.1g lithium diatomaceous earth, 0.161g sodium pyrophosphate were dissolved in 45g water and placed in a container, under nitrogen protection at 0 Stir in an ice bath for 120 minutes until uniform and transparent, then add 0.8g of CMC, and continue to stir for 2 hours to obtain a uniform and transparent pre-polymerization solution; dissolve 0.045g of KPS and 0.034g of TEMED into 2.25g of water, stir well and add to the pre-polymerization solution, nitrogen Stir quickly under protection for 2 minutes until uniform; then pour into a mold of a certain shape and react at 0°C for 24 hours, and then react at room temperature for 24 hours. After the obtained gel is taken out, the product is obtained by soaking and changing water repeatedly in deionized water.

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Abstract

The invention relates to a preparation method of a semi-interpenetrating network nanocomposite hydrogel which can respond to variations in temperature, pH and ultraviolet to realize volume transition. The preparation method of the gel is as follows: taking temperature-sensitive monomers, namely N-isopropylacrylamide and azo type water soluble monomers, namely 4-((4-acryloxy) phenyl azo) benzoic acid as copolymerization monomers, taking modified nano-clay as a cross-linking agent, dissolving the monomers and the cross-linking agent in a cellulose type macromolecular water solution, uniformly stirring, and then performing oxidation, reduction and catalytic free radical polymerization in an ice bath under the protection of nitrogen for preparation. The gel uses nano-laponite cross-linked monomers to constitute a framework of the gel and takes cellulose type macromolecules as semi-interpenetrating macromolecules. The obtained hydrogel has the advantages of excellent mechanical properties, high swelling rate and fast and controllable stimulus response. The gel has the potential to be applied to the field of sustained release of medicaments.

Description

technical field [0001] The invention belongs to a preparation method of an intelligent gel, in particular to a preparation method of an intelligent gel with excellent mechanical properties and responsiveness to multiple stimuli. Background technique [0002] Polymer gel refers to a system composed of a three-dimensional network structure of polymer compounds and a solvent, in which the polymers are connected by van der Waals force, chemical bond force, physical winding force, hydrogen bond force, etc. Since it is a three-dimensional network structure, it cannot be dissolved by solvents, but only swells. Responsive polymer gels are generally synthesized from responsive macromolecules, whose structure, physical properties, and chemical properties can change with changes in the external environment. When the gel is stimulated by the environment, its structure and properties (mainly volume) will respond accordingly, such as when the composition of the solvent, pH value, ionic s...

Claims

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Application Information

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IPC IPC(8): C08F251/02C08F220/54C08F220/36C08F2/48C08F2/44C08K9/02C08K3/34C08K3/32
Inventor 陈一
Owner HUNAN UNIV OF TECH
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