CN115590035A - Composite antibacterial agent and preparation method thereof - Google Patents
Composite antibacterial agent and preparation method thereof Download PDFInfo
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- CN115590035A CN115590035A CN202211265941.9A CN202211265941A CN115590035A CN 115590035 A CN115590035 A CN 115590035A CN 202211265941 A CN202211265941 A CN 202211265941A CN 115590035 A CN115590035 A CN 115590035A
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- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 201
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 68
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 67
- 239000005543 nano-size silicon particle Substances 0.000 claims description 62
- 235000012239 silicon dioxide Nutrition 0.000 claims description 62
- 238000003756 stirring Methods 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 34
- 239000006185 dispersion Substances 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 32
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 28
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 27
- 239000002105 nanoparticle Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000004599 antimicrobial Substances 0.000 claims description 15
- 239000011787 zinc oxide Substances 0.000 claims description 15
- SFVFIFLLYFPGHH-UHFFFAOYSA-M stearalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SFVFIFLLYFPGHH-UHFFFAOYSA-M 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 8
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 7
- 230000001699 photocatalysis Effects 0.000 claims description 7
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 claims description 6
- BKRJTJJQPXVRRY-UHFFFAOYSA-M dodecyl-(2-hydroxyethyl)-dimethylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CCO BKRJTJJQPXVRRY-UHFFFAOYSA-M 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229940049292 n-(3-(dimethylamino)propyl)octadecanamide Drugs 0.000 claims description 3
- MNAZHGAWPCLLGX-UHFFFAOYSA-N n-[3-(dimethylamino)propyl]docosanamide Chemical compound CCCCCCCCCCCCCCCCCCCCCC(=O)NCCCN(C)C MNAZHGAWPCLLGX-UHFFFAOYSA-N 0.000 claims description 3
- WWVIUVHFPSALDO-UHFFFAOYSA-N n-[3-(dimethylamino)propyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCCN(C)C WWVIUVHFPSALDO-UHFFFAOYSA-N 0.000 claims description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 36
- 230000001404 mediated effect Effects 0.000 abstract description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- Environmental Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Pest Control & Pesticides (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
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Abstract
The invention relates to a composite antibacterial agent, an antibacterial ceramic tile, an antibacterial dressing, an antibacterial plastic and a preparation method. The composite antibacterial agent comprises modified nano-silica, wherein the modified nano-silica is obtained by modifying with a cationic surfactant, so that the modified nano-silica has an antibacterial effect, and the obtained product has an internal antibacterial effect and a light-mediated antibacterial effect by compounding the modified nano-silica and the nano-titania, thereby realizing a long-acting antibacterial effect and good biological safety.
Description
Technical Field
The invention relates to the technical field of antibiosis, in particular to a composite antibacterial agent and a preparation method thereof.
Background
Healthy living environments are increasingly being the target of human pursuits. Microorganisms that are harmful to human health are ubiquitous, and thus combating harmful microorganisms is an important task for ensuring human health. The nano antibacterial material is a novel material with antibacterial property, is a nano preparation prepared by preparing an antibacterial agent or a substance without antibacterial property by a certain method, and has stronger antibacterial activity, wider antibacterial spectrum and higher safety than a common antibacterial agent. Currently, most of the antibacterial materials used in the field are single nanometer antibacterial materials, and the antibacterial effect of the antibacterial materials needs to be improved.
Disclosure of Invention
Based on the above, there is a need for a composite antibacterial agent and a preparation method thereof, so as to improve the antibacterial effect of the nano antibacterial material.
A composite antibacterial agent comprises modified nano-silica and photocatalytically active nanoparticles, wherein the modified nano-silica comprises nano-silica and a cationic surfactant, and the cationic surfactant is combined with negative charges on the surface of the nano-silica.
Compared with the prior scheme, the composite antibacterial agent has the following beneficial effects:
the composite antibacterial agent comprises modified nano-silica, wherein the modified nano-silica is obtained by modifying with a cationic surfactant, so that the modified nano-silica obtains an antibacterial effect and improves the adsorption force of the silica on bacteria, and meanwhile, the nano-silica modified by the cationic surfactant can be better combined with photocatalytic activity nano-particles, and the obtained product has an internal antibacterial effect and a light-mediated antibacterial effect, so that a long-acting antibacterial effect and good biological safety are realized.
In one embodiment, the photocatalytically active nanoparticles are selected from at least one of nano-titania and nano-zinc oxide.
In one embodiment, the mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 0.5-1: 4.
In one embodiment, the mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 1-1: 3.
In one embodiment, the mass ratio of the modified nano-silica to the photocatalytically active nano-particles is 1: 1 to 1: 5.
In one embodiment, the mass ratio of the modified nano-silica to the photocatalytically active nano-particles is 1: 2 to 1: 4.
In one embodiment, the nano-silica has a particle size of 20nm to 100nm.
In one embodiment, the photocatalytically active nanoparticles have a particle size of 25nm to 60nm.
In one embodiment, the cationic surfactant is selected from one or more of behenamidopropyl dimethylamine, hydroxyethyl lauryl dimethyl ammonium chloride, dimethyl diallyl ammonium chloride, stearamidopropyl dimethylamine, benzyltriethyl ammonium chloride, cetyl trimethyl ammonium bromide, and stearyl dimethyl benzyl ammonium chloride.
A preparation method of a composite antibacterial agent comprises the following steps:
step one, dispersing nano silicon dioxide in water to obtain a dispersion liquid;
adding a cationic surfactant into the dispersion liquid to modify the nano silicon dioxide to obtain a modified liquid;
and step three, adding the photocatalytic active nano particles into the modified solution, and stirring and mixing to obtain the composite antibacterial agent.
According to the preparation method of the composite antibacterial agent, the cationic surfactant is adopted to modify the nano-silica, and the cationic surfactant is combined with negative charges on the surface of the nano-silica, so that the modified nano-silica obtains an antibacterial effect, the adsorption force of the silica on bacteria is improved, meanwhile, the nano-silica modified by the cationic surfactant can be better combined with photocatalytic activity nano-particles, the obtained product has an internal antibacterial effect and a light-mediated antibacterial effect, and the long-acting antibacterial effect and good biological safety are realized.
In one embodiment, the reaction time of the second step is 1-4 h.
In one embodiment, the reaction time of the third step is 4-6 h.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The composite antibacterial agent comprises modified nano-silica and photocatalytic active nanoparticles, wherein the modified nano-silica comprises nano-silica and a cationic surfactant, and the cationic surfactant is combined with negative charges on the surface of the nano-silica.
The modified nano-silica is tested for potential by using a Zeta potentiometer, and the surface of the modified nano-silica is measured to be positively charged, so that the adsorption force of the silica on bacteria can be improved by modifying the silica by using the cationic surfactant.
Alternatively, the cationic surfactant may be selected from, but not limited to, one or more of behenamidopropyl dimethylamine, hydroxyethyl lauryl dimethyl ammonium chloride, dimethyl diallyl ammonium chloride, stearamidopropyl dimethylamine, benzyltriethyl ammonium chloride, cetyl trimethyl ammonium bromide, and stearyl dimethyl benzyl ammonium chloride.
In one example, the photocatalytically active nanoparticles are selected from at least one of nano-titania and nano-zinc oxide.
In one example, the mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 0.5-1: 4.
The above examples can achieve a better antibacterial effect by optimizing the mass ratio of the nanosilica to the cationic surfactant in the composite antibacterial agent.
Further, in one example, the mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 1 to 1: 3.
The above examples can achieve a better antibacterial effect by further preferably selecting the mass ratio of the nanosilica to the cationic surfactant in the composite antibacterial agent.
In one example, the mass ratio of the modified nano-silica to the photocatalytically active nano-particles is 1: 1 to 1: 5.
The above examples can achieve a better antibacterial effect by optimizing the mass ratio of the modified nano silica to the photocatalytically active nano particles in the composite antibacterial agent.
Further, in one example, the mass ratio of the modified nano-silica to the photocatalytically active nano-particles is 1: 2 to 1: 4.
The above examples can achieve a better antibacterial effect by further preferably selecting the mass ratio of the modified nano silica to the photocatalytically active nano particles in the composite antibacterial agent.
In one example, the nano-silica has a particle size of 20nm to 100nm. Further, in one example, the particle size of the nano-silica is 40nm to 60nm.
In one example, the photocatalytically active nanoparticles have a particle size of 25nm to 60nm. Further, in one example, the photocatalytically active nanoparticles have a particle size of 40nm to 50nm.
The composite antibacterial agent comprises modified nano-silica, wherein the modified nano-silica is obtained by modifying with a cationic surfactant, so that the modified nano-silica has an antibacterial effect and improves the adsorption force of the silica on bacteria.
Further, the present invention also provides a method for preparing the composite antibacterial agent exemplified in any one of the above, comprising the steps of:
step one, dispersing nano silicon dioxide in water to obtain a dispersion liquid.
And secondly, adding a cationic surfactant into the dispersion liquid to modify the nano silicon dioxide to obtain a modified liquid.
And step three, adding the photocatalytic active nano particles into the modified solution, and stirring and mixing to obtain the composite antibacterial agent.
According to the preparation method of the composite antibacterial agent, the cationic surfactant is adopted to modify the nano-silica, and the cationic surfactant is combined with negative charges on the surface of the nano-silica, so that the modified nano-silica obtains an antibacterial effect, the adsorption force of the silica on bacteria is improved, meanwhile, the nano-silica modified by the cationic surfactant can be better combined with the photocatalytic activity nano-particles, the obtained product has an internal antibacterial effect and a light-mediated antibacterial effect, and the long-acting antibacterial effect and good biological safety are realized.
The preparation method has the advantages of easy operation and high yield.
In one example, in the second step, stirring and mixing are performed, and the stirring speed is 500rpm to 800rpm.
In one example, the reaction time of the second step is 1-4 h. In some specific examples, the reaction time of step two is 1h, 2h, 3h, 4h, etc.
In one example, the reaction time of step three is 4h to 6h. In some specific examples, the reaction time of step three is 4h, 5h, 6h, etc.
The following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples, and it should be understood that the scope of the present invention is summarized by the appended claims, and a person skilled in the art should realize that certain changes made to the embodiments of the present invention, in light of the inventive concept, are intended to be covered by the spirit and scope of the claims of the present invention.
Example 1
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.025 g of a cationic surfactant solution (octadecyl dimethyl benzyl ammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 1. And stirring for about 2 hours, and modifying the nano-silica by using the cationic surfactant to obtain a modified solution containing the modified nano-silica.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 2
The present example prepares a composite antimicrobial agent, and the preparation method thereof includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charges, and the particle size is about 50nm.
Step 2, 0.05 g of a cationic surfactant solution (octadecyl dimethyl benzyl ammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 2. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 3
The present example prepares a composite antimicrobial agent, and the preparation method thereof includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, a cationic surfactant solution (octadecyl dimethyl benzyl ammonium chloride) of 0.075 is added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 3. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 4
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and a magnetic stirrer is used for stirring and dispersing at the speed of 550rpm, so that a dispersion liquid is obtained. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
And 2, adding 0.1 g of cationic surfactant solution (octadecyl dimethyl benzyl ammonium chloride) into the dispersion liquid obtained in the step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 4. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 5
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charges, and the particle size is about 50nm.
Step 2, 0.025 g of a cationic surfactant solution (dimethyldiallylammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 1. And stirring for about 2 hours, and modifying the nano-silica by using the cationic surfactant to obtain a modified solution containing the modified nano-silica.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 6
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.05 g of a cationic surfactant solution (dimethyldiallylammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 2. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 7
The present example prepares a composite antimicrobial agent, and the preparation method thereof includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.075 g of a cationic surfactant solution (dimethyldiallylammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 3. And stirring for about 2 hours, and modifying the nano-silica by using the cationic surfactant to obtain a modified solution containing the modified nano-silica.
And 3, adding 0.05 g of nano titanium dioxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano titanium dioxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano titanium dioxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 8
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.1 g of a cationic surfactant solution (dimethyldiallylammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 4. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.025 g of nano zinc oxide solution into the modification solution obtained in the step 2, wherein the particle size of the nano zinc oxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano zinc oxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 9
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and a magnetic stirrer is used for stirring and dispersing at the speed of 550rpm, so that a dispersion liquid is obtained. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.025 g of a cationic surfactant solution (hydroxyethyl lauryl dimethyl ammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 1. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano zinc oxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano zinc oxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano zinc oxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 10
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charges, and the particle size is about 50nm.
Step 2, 0.05 g of a cationic surfactant solution (hydroxyethyl lauryl dimethyl ammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 2. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano zinc oxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano zinc oxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano zinc oxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Example 11
This example prepares a composite antimicrobial agent, the preparation method of which includes the following steps:
step 1, 0.025 g of nano-silica is added into 120mL of water, and stirred and dispersed by using a magnetic stirrer at the speed of 550rpm to obtain a dispersion liquid. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.075 g of a cationic surfactant solution (hydroxyethyl lauryl dimethyl ammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 3. Stirring for about 2h, and modifying the nano silicon dioxide by the cationic surfactant to obtain a modified liquid containing the modified nano silicon dioxide.
And 3, adding 0.05 g of nano zinc oxide solution into the modified solution obtained in the step 2, wherein the particle size of the nano zinc oxide is about 50nm. The mass ratio of the modified nano silicon dioxide to the nano zinc oxide is 1: 2. Stirring for 5h to obtain the composite antibacterial agent.
Comparative example 1
This comparative example prepared an antibacterial agent, the preparation method of which included the steps of:
step 1, 0.025 g of nano-silica is added into 120mL of water, and a magnetic stirrer is used for stirring and dispersing at the speed of 550rpm, so that a dispersion liquid is obtained. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
Step 2, 0.025 g of a cationic surfactant solution (octadecyl dimethyl benzyl ammonium chloride) was added to the dispersion obtained in step 1. The mass ratio of the nano silicon dioxide to the cationic surfactant is 1: 1. Stirring for about 2h to obtain the antibacterial agent.
Comparative example 2
This comparative example prepared an antibacterial agent, the preparation method of which included the steps of:
step 1, 0.025 g of nano-silica is added into 120mL of water, and a magnetic stirrer is used for stirring and dispersing at the speed of 550rpm, so that a dispersion liquid is obtained. Wherein, the surface of the nano silicon dioxide has negative charge and the particle size is about 50nm.
And 2, adding 0.05 g of nano titanium dioxide into the dispersion liquid obtained in the step 1, wherein the particle size of the nano titanium dioxide is about 50nm. Stirring for 5h to obtain the antibacterial agent.
Comparative example 3
The comparative example prepared an antibacterial agent, the preparation method of which included the following steps:
step 1, add 0.025 grams of cationic surfactant solution (octadecyl dimethyl benzyl ammonium chloride) to 120mL of water. Stirring for about 2h.
And 2, adding 0.05 g of nano titanium dioxide into the solution, wherein the particle size of the nano titanium dioxide is about 50nm. Stirring for 5h to obtain the antibacterial agent.
The product of example 1 was centrifuged, redispersed in 30mL of water and stored in a 50mL centrifuge tube.
The products obtained in examples 1 to 13 and comparative examples 1 to 2 were subjected to an antibacterial test, and the Minimum Inhibitory Concentrations (MICs) of the products against escherichia coli and staphylococcus aureus were respectively tested. The test results are shown in table 1.
TABLE 1
The results show that the composite antibacterial agent prepared by the preparation method has good inhibition effect on escherichia coli and staphylococcus aureus.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A composite antibacterial agent, which is characterized by comprising modified nano-silica and photocatalytically active nanoparticles, wherein the modified nano-silica comprises nano-silica and a cationic surfactant, and the cationic surfactant is combined with negative charges on the surface of the nano-silica.
2. The composite antimicrobial agent of claim 1, wherein the photocatalytically active nanoparticles are at least one selected from the group consisting of nano titanium dioxide and nano zinc oxide.
3. The composite antibacterial agent according to claim 1, wherein the mass ratio of the nanosilica to the cationic surfactant is 1: 0.5 to 1: 4.
4. The composite antimicrobial agent of claim 1, wherein the mass ratio of the modified nanosilica to the photocatalytically active nanoparticles is from 1: 1 to 1: 5.
5. The composite antibacterial agent according to claim 1, wherein the mass ratio of the nanosilica to the cationic surfactant is 1: 1 to 1: 3.
6. The composite antimicrobial agent of claim 1, wherein the mass ratio of the modified nanosilica to the photocatalytically active nanoparticles is from 1: 2 to 1: 4.
7. The composite antibacterial agent according to any one of claims 1 to 6, wherein the nano silica has a particle size of 20nm to 100nm; and/or
The particle size of the photocatalytic activity nano particles is 20-100 nm.
8. The composite antimicrobial agent of any one of claims 1 to 6, wherein the cationic surfactant is selected from one or more of behenamidopropyl dimethylamine, hydroxyethyl lauryl dimethyl ammonium chloride, dimethyl diallyl ammonium chloride, stearamidopropyl dimethylamine, benzyl triethyl ammonium chloride, cetyl trimethyl ammonium bromide, and stearyl dimethyl benzyl ammonium chloride.
9. The preparation method of the composite antibacterial agent is characterized by comprising the following steps:
step one, dispersing nano silicon dioxide in water to obtain a dispersion liquid;
adding a cationic surfactant into the dispersion liquid to modify the nano silicon dioxide to obtain a modified liquid;
and step three, adding nano titanium dioxide into the modified solution, and stirring and mixing to obtain the composite antibacterial agent.
10. The method for preparing a composite antibacterial agent according to claim 9, wherein the reaction time of the second step is 1 to 4 hours; and/or
The reaction time of the third step is 4-6 h.
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