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Silver nano-particle hybrid supramolecular hydrogel based on cyclodextrin/PEG grafted polyacrylic acid, and preparation method and application thereof

A supramolecular hydrogel, grafted polyacrylic acid technology, applied to silver nanoparticle hybrid supramolecular hydrogel based on cyclodextrin/PEG grafted polyacrylic acid and the field of preparation and application, can solve the problem of gel performance, poor stability of silver nanoparticles, affecting antibacterial properties, etc., to achieve the effect of improving stability, simple preparation process, and solving agglomeration

Active Publication Date: 2018-02-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under normal conditions, the stability of silver nanoparticles is poor, and the agglomeration phenomenon is serious, which seriously affects its antibacterial performance.
Therefore, some small molecules, such as oleic acid, are needed to stabilize it. However, the incorporation of these compounds affects the performance of the gel to some extent.

Method used

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  • Silver nano-particle hybrid supramolecular hydrogel based on cyclodextrin/PEG grafted polyacrylic acid, and preparation method and application thereof
  • Silver nano-particle hybrid supramolecular hydrogel based on cyclodextrin/PEG grafted polyacrylic acid, and preparation method and application thereof
  • Silver nano-particle hybrid supramolecular hydrogel based on cyclodextrin/PEG grafted polyacrylic acid, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The structural formula of the anionic polyelectrolyte PPEGMA-co-PAA is:

[0035]

[0036] The synthetic method of polymer of the present invention, step is as follows:

[0037] PEGMA (2.2g, 2.3mmol), AA (82μL, 1.2mmol), CPADB (9.6mg, 0.03mmol), AIBN (1.5mg, 0.01mmol) were added to a Schlenk polymerization bottle, and the mixture was dissolved in 3mL of purified toluene, Freeze-thaw cycles deoxygenated and filled with nitrogen, and reacted in an oil bath at 60°C for 5 hours under the protection of nitrogen. After the reaction, the reaction bottle was placed in an ice-water bath, and the stopper was opened to expose to the air to terminate the polymerization. The mixture was precipitated in a mixed solvent of diethyl ether / n-hexane to remove unreacted monomers, centrifuged to obtain a pink solid, and dried under vacuum at 35°C. (Mn, GPC =10.2K, PDI=1.21)

[0038] Weigh the polymer PPEGMA-co-PAA (236.3 mg, 0.06 mmol AA unit) and dissolve it in 10 mL of high-purity w...

Embodiment 2

[0042] PEGMA (2.2g, 2.3mmol), AA (238μL, 3.5mmol), CPADB (9.6mg, 0.03mmol), AIBN (1.5mg, 0.01mmol) were added to a Schlenk polymerization bottle, and the mixture was dissolved in 3mL of purified toluene, Freeze-thaw cycles deoxygenated and filled with nitrogen, and reacted in an oil bath at 60°C for 7 hours under the protection of nitrogen. After the reaction, the reaction bottle was placed in an ice-water bath, and the stopper was opened to expose to the air to terminate the polymerization. The mixture was precipitated in a mixed solvent of diethyl ether / n-hexane to remove unreacted monomers, centrifuged to obtain a pink solid, and dried under vacuum at 35°C. (Mn, GPC =30.3K, PDI=1.19)

[0043] The polymer PPEGMA-co-PAA (78.8mg, 0.08mmol AA unit) was weighed and dissolved in 10mL of high-purity water, 0.025M silver nitrate aqueous solution (1mL) was added thereto, and stirred at room temperature for 0.5h at high speed. The freshly prepared 0.25M sodium borohydride aqueous ...

Embodiment 3

[0047] Add PEGMA (4.4 g, 4.6 mmol), AA (1.25 mL, 18.4 mmol), CPADB (9.6 mg, 0.03 mmol), AIBN (1.5 mg, 0.01 mmol) into a Schlenk polymerization flask, and dissolve the mixture in 10 mL of purified toluene , deoxygenated and nitrogen-filled by freeze-thaw cycles, and reacted in an oil bath at 60°C for 8 hours under the protection of nitrogen. After the reaction, the reaction bottle was placed in an ice-water bath, and the stopper was opened to expose to the air to terminate the polymerization. The mixture was precipitated in an excess of diethyl ether / n-hexane mixed solvent to remove unreacted monomers, and centrifuged to obtain a pink solid, which was vacuum-dried at 35°C. (Mn, GPC =600.1K, PDI=1.37)

[0048] The polymer PPEGMA-co-PAA (35.0mg, 0.08mmol AA unit) was weighed and dissolved in 10mL of high-purity water, 0.025M silver nitrate aqueous solution (1mL) was added thereto, and stirred at room temperature for 0.5h at high speed. The freshly prepared 0.25M sodium borohyd...

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Abstract

The invention relates to a silver nano-particle hybrid supramolecular hydrogel based on cyclodextrin / PEG grafted polyacrylic acid, and a preparation method and an application thereof. The supramolecular hydrogel is characterized in that the molecular weight of an anionic polyelectrolyte PPEGMA-co-PAA is 10-600 kDa; a molar ratio of the PPEGMA to the PAA in the polymer is 10:1 to 1:4; and the content of nano-silver in the supramolecular hydrogel is 0.05-5%. The preparation process is simple, uniformly dispersed spherical nano-silver particles are obtained, and the agglomeration problem of nano-silver is effectively solved. A pure polymer system which only can form hydrogel under an acidic condition, but the above silver hybrid system also can form hydrogel under neutral and alkaline conditionms, so the pH value range of the hydrogel is enlarged. The nano-silver hybrid supramolecular hydrogel has self-repairing property and injectable performance, and has good application prospects in the fields of antibacterial agents and wound healing.

Description

technical field [0001] The invention relates to the preparation of a silver nanoparticle hybrid supramolecular hydrogel, in particular to the synthesis of polyethylene glycol monoether methacrylate grafted polyacrylic acid by reversible addition-fragmentation chain transfer radical polymerization (RAFT) The random copolymer of PPEGMA-co-PAA (PPEGMA-co-PAA), using the PPEGMA-co-PAA anionic polyelectrolyte containing acrylic acid as a stabilizer to prepare silver nanoparticles in situ, prepared by supramolecular interaction with α-cyclodextrin has antibacterial properties Silver nanoparticles hybrid supramolecular hydrogels. Background technique [0002] Supramolecular hydrogels are physical gels whose formation depends on non-covalent supramolecular interactions between polymer chains. Common supramolecular interactions mainly include the following categories: van der Waals forces, hydrogen bond interactions, electrostatic interactions, hydrophobic interactions, and host-gue...

Claims

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Application Information

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IPC IPC(8): C08J3/075C08L5/16C08L33/14C08K3/08C08F220/28C08F220/06
CPCC08F220/28C08F220/286C08J3/075C08J2305/16C08J2433/14C08L5/16C08L33/14C08K3/08C08F220/06
Inventor 任丽霞乔亚平袁晓燕
Owner TIANJIN UNIV
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