Preparation method of antibacterial quaternized chitosan/Ag hybrid nano-hydrogel

A technology of quaternized chitosan and nano-hydrogel, which is applied in the field of preparation of antibacterial quaternized chitosan/Ag hybrid nano-hydrogel, can solve the problem that limits the wide application of Ag nanoparticles and is not enough to meet the Antibacterial requirements, Ag nanoparticles are easy to agglomerate, etc., to achieve excellent structural stability and antibacterial properties, improve bonding fastness, and good water dispersibility.

Active Publication Date: 2021-08-13
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The antibacterial ability of unmodified chitosan is often weak, which is not enough to meet the complex and changeable antibacterial requirements. The water solubility and antibacterial performance of chitosan modified by quaternization can be significantly improved [Carbohydrate Polymers, 2020, 247, 116754-116765.】
Ag nanoparticles are favored because of their broad-spectrum, high-efficiency, and low-drug-resistance antibacterial properties, but Ag nanoparticles are prone to agglomeration and difficult to process, which limits the wide application of Ag nanoparticles to a certain extent.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 2.5g of Ag nanoparticles (average size of 18nm) to a mixed solvent of 250g of water and 250g of ethylene glycol, and ultrasonically treat them for 20min at a power of 300W to obtain a dispersion of Ag nanoparticles, and then adjust the temperature to 30°C , adding an ethylene glycol solution containing 3.85 mg of 2-aminoethanethiol, and reacting for 2 hours to obtain surface amino-modified Ag nanoparticles, which are purified and dried for use. The amino-modified Ag nanoparticles were redispersed in deionized water, and the amino-modified Ag nanoparticles aqueous dispersion was obtained after ultrasonic treatment for 20 min at a power of 300 W.

[0042] 0.0125 g of emulsifier P(E / B)-PEO was weighed and dissolved in 12.5 g of isoparaffin (isopar M, Exxon Mobil) to obtain an emulsifier solution. 0.3g quaternized chitosan and 5mg NaBF 4 Dissolve in 2g of purified Ag nanoparticle aqueous dispersion (wherein the amino-modified Ag nanoparticle content is 3mg), the result...

Embodiment 2

[0047] Add 0.5g of Ag nanoparticles (average size is 15nm) to 250g of water and 250g of ethylene glycol, ultrasonic treatment at 450W for 10min to prepare Ag nanoparticles dispersion, then adjust the temperature to 30°C, add 1 mg of 2-aminomercaptopropionic acid in ethylene glycol solution was reacted for 12 hours to prepare Ag nanoparticles with surface amino-modification, and the product was purified and dried for use. The amino-modified Ag nanoparticles were redispersed in deionized water, and the amino-modified Ag nanoparticles aqueous dispersion was obtained after ultrasonic treatment for 10 min at a power of 450 W.

[0048] Weigh 1.5g emulsifier Tween 80 and 1.5g Span-80, dissolve in 30g toluene to obtain emulsifier solution. 0.42g quaternized chitosan and 8.3mg NaBF 4 Dissolve in 2.5g of purified Ag nanoparticle aqueous dispersion (wherein the amino-modified Ag nanoparticle content is 15mg), the resulting dispersion is added to the above emulsifier solution, stirred at...

Embodiment 3

[0053] Add 0.75g of Ag nanoparticles (average size is 20nm) to 250g of water and 250g of dimethyl sulfoxide, ultrasonically treat for 10min at a power of 500W to prepare Ag nanoparticles dispersion, then adjust the temperature to 30°C, A dimethyl sulfoxide solution containing 1.5 mg of 2-aminoethanethiol was added and reacted for 10 h to prepare Ag nanoparticles with surface amino-modification. The product was purified and dried before use. The amino-modified Ag nanoparticles were redispersed in deionized water, and the amino-modified Ag nanoparticles aqueous dispersion was obtained after ultrasonic treatment for 10 min at a power of 500 W.

[0054] Weigh 0.255g of emulsifier P(E / B)-PEO and dissolve it in 25.5g of n-hexadecane to obtain an emulsifier solution. 0.37g quaternized chitosan and 8.0mg Na 2 SO 4Dissolve in 2.0 g of purified Ag nanoparticle aqueous dispersion (wherein the amino-modified Ag nanoparticle content is 15 mg), add the obtained dispersion into the above e...

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Abstract

A preparation method of antibacterial quaternized chitosan/Ag hybrid nano-hydrogel comprises the following steps: (1) carrying out amino modification on Ag nano-particles to obtain an aqueous dispersion of the amino-modified Ag nano-particles; (2) modifying chitosan by using 2, 3-epoxypropyl trimethyl ammonium chloride, so as to obtain quaternized chitosan; (3) dissolving an emulsifier in a non-polar solvent to obtain a non-polar emulsifier solution; (4) dissolving a hydrophilic metal salt and quaternized chitosan in the amino-modified Ag nano-particle aqueous dispersion to obtain a dispersion A, adding the dispersion liquid A into a non-polar emulsifier solution, stirring and pre-emulsifying to obtain a crude emulsion, and performing ultrasonic treatment to prepare a reversed-phase miniemulsion; and (5) directly dropwise adding a cross-linking agent into the reversed-phase miniemulsion, reacting to prepare the quaternized chitosan/Ag hybrid nano-hydrogel, purifying, and dispersing in water to prepare the aqueous dispersion of the quaternized chitosan/Ag hybrid nano-hydrogel. The prepared hybrid nano-hydrogel has the advantages of good dispersity, controllable particle size, good colloidal stability, broad-spectrum antibacterial property and the like.

Description

[0001] (1) Technical field [0002] The invention relates to a preparation method of antibacterial quaternized chitosan / Ag hybrid nano hydrogel. [0003] (2) Background technology [0004] The variety and quantity of pathogenic bacteria and the emergence of drug-resistant bacteria caused by the abuse of antibiotics seriously threaten human health and safety. Therefore, there is an urgent need for safe, efficient, non-resistant and degradable antibacterial materials. [0005] Chitosan has the characteristics of wide source, good biocompatibility, and biodegradability, so it is a potential antibacterial candidate material. The antibacterial ability of unmodified chitosan is often weak, which is not enough to meet the complex and changeable antibacterial requirements. The water solubility and antibacterial performance of chitosan modified by quaternization can be significantly improved [Carbohydrate Polymers, 2020, 247, 116754-116765.]. Ag nanoparticles are favored because of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/075C08J3/24C08L5/08C08K9/04C08K3/08
CPCC08J3/075C08J3/24C08J2305/08C08K9/04C08K2003/0806
Inventor 曹志海高峰姚俊秘一芳郑思佳
Owner ZHEJIANG SCI-TECH UNIV
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