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Preparation method of silicon dioxide antibacterial microsphere

A technology of silicon dioxide and microspheres, applied in the field of antibacterial nanomaterials, can solve the problems of inability to achieve bacterial aggregation and adhesion, high quaternary ammonium salt addition, poor antibacterial effect, etc., and achieve efficient and long-lasting antibacterial performance and good antibacterial effect , Antibacterial performance, efficient and long-lasting effect

Active Publication Date: 2019-10-25
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN104472530A reports a preparation method of solid organosilicon quaternary ammonium salt, but the quaternary ammonium salt is simply adsorbed on the surface of silicon dioxide, there is still the problem of migration, and the amount of quaternary ammonium salt added is too high; and the quaternary ammonium salt Salt is grafted on the surface of silica, most of which require pretreatment of silica, such as treatment with silane coupling agent, and most of the quaternary ammonium salts used are short-chain quaternary ammonium salts, which cannot achieve the effect of preventing bacterial aggregation and adhesion. The process is complicated, the cost is high, and the antibacterial effect is not good

Method used

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  • Preparation method of silicon dioxide antibacterial microsphere
  • Preparation method of silicon dioxide antibacterial microsphere
  • Preparation method of silicon dioxide antibacterial microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0041] 100 parts of N,N-dimethyl-3-aminopropyltrimethoxysilane (Hangzhou Jessica Chemical Co., Ltd.), 120 parts of bromooctane (Aladdin), 0.1 part of p-hydroxyanisole (A Latin) was added to 200 parts of acetonitrile, reacted at 30°C for 8h, and the solution obtained by the reaction was rotary evaporated at 50°C for 2h, and the unreacted alkyl halide and solvent were removed to obtain Silicon-containing quaternary ammonium salt 1 , the structural formula is as follows:

[0042]

[0043] Mix 10 parts of tetramethoxysilane (Aladdin), 5 parts of 1mol / L sodium hydroxide aqueous solution (Chinese medicine), 5 parts Deionized water and 1 copy Silicon-containing quaternary ammonium salt 1 Prepared by dispersing in 200 parts of toluene (Sinopharm) and reacting at 35°C for 24 hours Silica Antibacterial Microspheres 1 . The antibacterial test was carried out according to relevant standards, and the results of the antibacterial rate test and the particle size of the microsphere...

Embodiment 2

[0045] 100 parts of N,N-dimethyl-3-aminopropyltrimethoxysilane (Hangzhou Jessica Chemical Co., Ltd.), 150 parts of bromodecane (Aladdin), 0.125 parts of 2-tert-butyl-p-phenyl Diphenol (Aladdin) was added to 250 parts of ethyl acetate, reacted at 45°C for 10h, and the solution obtained by the reaction was rotary evaporated at 60°C for 1.5h, and the unreacted alkyl halide and solvent were removed to obtain Silicon-containing quaternary ammonium salt 2 , the structural formula is as follows:

[0046]

[0047] Mix 10 parts of tetrapropoxysilane (Aladdin), 10 parts of 0.5mol / L potassium hydroxide aqueous solution (Chinese medicine), 5 parts deionization water and 1 copy Silicon-containing quaternary ammonium salt 2 Prepared by dispersing in 250 parts of acetonitrile (Sinopharm) and reacting at 75°C for 20 hours Silica antibacterial micro ball 2 . The antibacterial test was carried out according to relevant standards, and the results of the antibacterial rate test an...

Embodiment 3

[0049] 100 parts of N,N-dimethyl-3-aminopropyltrimethoxysilane (Hangzhou Jessica Chemical Co., Ltd.), 250 parts of bromododecane (Aladdin), 0.15 parts of p-hydroxyanisole ( Aladdin) was added to 300 parts of acetone, reacted at 60°C for 12h, and the solution obtained by the reaction was rotary evaporated at 70°C for 1h, and the unreacted alkyl halide and solvent were removed to obtain Silicon-containing quaternary ammonium salt 3 , the structural formula is as follows:

[0050]

[0051] Mix 10 parts of TEOS (Chinese medicine), 15 parts of ammonia water (Chinese medicine), 5 parts Deionized water Disperse in 300 parts of ethanol (Sinopharm), pre-react at 45°C for 4 hours, add 1 part of the above mixed solution dropwise Silicon-containing quaternary ammonium salt 3 , prepared by reacting at 50°C for 24h Silica antibacterial micro ball 3 . The antibacterial test was carried out according to relevant standards, and the results of the antibacterial rate test and the par...

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Abstract

The invention discloses a preparation method of a silicon dioxide antibacterial microsphere. A carrier, namely a silicon dioxide microsphere, and an antibacterial agent, namely a long-alkyl-chain silicon-containing quaternary ammonium salt are copolymerized, and the silicon-containing quaternary ammonium salt is directly bonded to the surface of the silicon dioxide microsphere, wherein the silicondioxide microsphere is prepared through a sol-gel method, and the volume ratio of a silicon source to the quaternary ammonium salt is 1:(0.1 to 1). According to the preparation method, a process is simple, reaction conditions are mild, the raw materials are easy to obtain, and the cost is low; and the obtained antibacterial microsphere is regular in sphere shape and uniform and controllable in particle size, antibacterial components on the microsphere do not migrate, the antibacterial property of the material is effectively improved, the contact-type antibacterial purpose is achieved, and thesilicon dioxide antibacterial microsphere is widely applied to the aspects of food packaging and clothing antibacterial coatings.

Description

technical field [0001] The invention relates to the technical field of antibacterial nanomaterials, and furthermore, relates to a preparation method of silicon dioxide antibacterial microspheres grafted with long alkyl chain silicon-containing quaternary ammonium salts on the surface. Background technique [0002] Bacteria are an important source of causing people's diseases, invading people's lives all the time, and their massive reproduction will threaten people's health. With the continuous advancement of science and technology and the improvement of people's living standards, people's self-health awareness is constantly strengthening, and the application of antibacterial materials has gradually attracted people's attention. In daily life, people first come into contact with all kinds of materials, such as daily necessities, food packaging, sanitary products, household appliances, public facilities, etc., the handrails encountered when taking the bus, the buttons encounte...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B33/18C01P2004/03C01P2004/62C01P2004/64
Inventor 东为富施申伟李婷丁重阳马丕明陈明清
Owner JIANGNAN UNIV
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