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Preparation method of quaternary ammonium salt polymer antibacterial agent and silver-loaded compound antibacterial agent thereof on basis of ATRP method

A technology of polymers and antibacterial agents, which is applied in the field of preparation of silver-loaded-quaternary ammonium salt polymer composite antibacterial agents, can solve the problems of expensive synthetic raw materials, high synthesis reaction temperature, and limited industrial applications, and achieve effective and controllable percentages. The effect of improving antibacterial efficiency and obvious antibacterial effect

Inactive Publication Date: 2016-07-27
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the antibacterial field, quaternary ammonium salt polymer materials have shown high value in use, but there are still some problems in practical applications: expensive synthetic raw materials; high synthesis reaction temperature and harsh conditions; partial synthesis intermediate / final The water solubility of the product is poor, and organic solvents need to be added to help dissolve it during use, which limits industrial application; some chloramine antibacterial agents use N-methylol as an active group, and there is still a problem of formaldehyde release during use

Method used

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  • Preparation method of quaternary ammonium salt polymer antibacterial agent and silver-loaded compound antibacterial agent thereof on basis of ATRP method
  • Preparation method of quaternary ammonium salt polymer antibacterial agent and silver-loaded compound antibacterial agent thereof on basis of ATRP method
  • Preparation method of quaternary ammonium salt polymer antibacterial agent and silver-loaded compound antibacterial agent thereof on basis of ATRP method

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Experimental program
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Effect test

Embodiment 1

[0042] (1) Take 0.2gATRP initiator It is recorded that PER-Br is completely dissolved in 5 mL of dimethyl sulfoxide (DMSO), and then 4.31 mL of glycidyl methacrylate (GMA) and 113 μL of pentamethyldiethylenetriamine (PMDETA) are dissolved in the solution 47 mg of cuprous bromide (CuBr) was added quickly after bubbling nitrogen gas for 5 minutes, and immediately sealed with a rubber stopper; the system was reacted at 27°C for 10 minutes under an oxygen-free nitrogen protection environment, and the cork was opened for 2-3 minutes , and then precipitated with methanol, and then washed twice with methanol to remove PMDETA, CuBr, and unreacted GMA and most of the solvent DMSO; after centrifugation, the supernatant was removed, and the residual methanol in the lower precipitate was dried, and then Then dissolve with 1-2mL DMSO, precipitate with deionized water and wash twice, remove the supernatant after centrifugation, add a small amount of pure water to freeze-dry, the product af...

Embodiment 2

[0046] Get the quaternary ammonium salt polymer antibacterial agent QPGDED-CH that 100mg embodiment 1 obtains 3 (or QPGDED-C 6 h 13 , or QPGDED / ED-CH 3 , or QPGDED / ED-C 6 h 13 ) was dissolved in 5 mL of deionized water, to which 600 mg of AgNO was added 3 , in a light-proof environment, after magnetic stirring for 48 hours, the reaction solution was dissolved in a small amount (30-40 mL) of pure water, and then dialyzed with a 3500 dialysis bag for 48 hours to remove unreacted AgNO 3 , and then take out the liquid in the dialysis bag and freeze-dry to obtain a yellow-brown flocculent product, which is the quaternary ammonium salt polymer silver-loaded composite antibacterial agent, which is respectively marked as QPGDED-CH 3 -Ag, QPGDED-C 6 h 13 -Ag, QPGDED / ED-CH 3 -Ag, QPGDED / ED-C 6 h 13 -Ag. Through thermogravimetric analysis, the silver-loaded amount of the four quaternary ammonium salt polymer silver-loaded composite antibacterial agents is all about 10wt%.

Embodiment 3

[0048] Get the antimicrobial agent polymer skeleton material PER-PGED that step 2 obtains in 100mg embodiment 1, be dissolved in the deionized water of 5mL, add the AgNO of 600mg wherein 3 , in a light-proof environment, after magnetic stirring for 48 hours, the reaction solution was dissolved in a small amount (30-40 mL) of pure water, and then dialyzed with a 3500 dialysis bag for 48 hours to remove unreacted AgNO 3 , and then take out the liquid in the dialysis bag and freeze-dry to obtain a yellow-brown flocculent product, which is the silver-loaded composite antibacterial agent, which is recorded as PER-PGED-Ag. The results of thermogravimetric analysis show that the silver loading is also about 10wt%.

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Abstract

The invention discloses a preparation method of a quaternary ammonium salt polymer antibacterial agent and a silver-loaded compound antibacterial agent thereof on the basis of an ATRP method. According to the method, various monomers are grafted onto initiation points of an initiator through atom transfer radical active polymerization, a high molecular polymer is obtained, ring-opening reacting is conducted on the high molecular polymer, and an antibacterial agent polymer framework material can be obtained; different modifications are conducted on the antibacterial agent polymer framework material, and a quaternary ammonium salt polymer antibacterial agent, a silver-loaded-quaternary ammonium salt polymer compound antibacterial agent and a silver-loaded polymer antibacterial agent are obtained respectively. The obtained antibacterial agents are low in antibacterial concentration and obvious in sterilizing effect and can be used for modifications of the surfaces of glass sheets, polystyrene and the like by combining the adsorption property of dopamine to form a surface antibacterial polymer brush. The antibacterial effect of the antibacterial agents is obvious, and high commercial potential is achieved.

Description

technical field [0001] The invention belongs to the technical field of preparation of antibacterial materials, in particular to a preparation method of a quaternary ammonium salt polymer antibacterial agent based on an ATRP method and a silver ion-modified silver-loaded-quaternary ammonium salt polymer composite antibacterial agent and its application in Application in the field of surface antibacterial. Background technique [0002] In recent years, antibacterial agents have been widely used in people's lives. The research on non-toxic and harmless antibacterial agents has also caused wave after wave of upsurge. Antibacterial agents are generally divided into inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents. [0003] Natural antibacterial agents are mainly derived from some extracts of animals and plants, such as chitosan, propolis, protamine and allicin, etc., which are the earliest antibacterial agents used by humans. Ultra-...

Claims

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Application Information

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IPC IPC(8): C08F120/32C08F8/00C08F8/44C09D5/14
CPCC08F120/32C08F8/44C09D5/14C08F8/00
Inventor 徐福建苑慧敏俞丙然
Owner BEIJING UNIV OF CHEM TECH
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