CN117378601A - Nano silver antibacterial agent and preparation method thereof - Google Patents
Nano silver antibacterial agent and preparation method thereof Download PDFInfo
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- CN117378601A CN117378601A CN202311292535.6A CN202311292535A CN117378601A CN 117378601 A CN117378601 A CN 117378601A CN 202311292535 A CN202311292535 A CN 202311292535A CN 117378601 A CN117378601 A CN 117378601A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title abstract description 25
- 239000003607 modifier Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 108
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 72
- 239000000243 solution Substances 0.000 claims description 44
- 239000011259 mixed solution Substances 0.000 claims description 36
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 25
- 229920000178 Acrylic resin Polymers 0.000 claims description 19
- 239000004925 Acrylic resin Substances 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 18
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 241000588724 Escherichia coli Species 0.000 abstract description 10
- 150000001450 anions Chemical class 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 9
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 8
- 229910052709 silver Inorganic materials 0.000 abstract description 8
- 239000004332 silver Substances 0.000 abstract description 8
- 230000001954 sterilising effect Effects 0.000 abstract description 8
- 230000002401 inhibitory effect Effects 0.000 abstract description 6
- 244000063299 Bacillus subtilis Species 0.000 abstract description 5
- 235000014469 Bacillus subtilis Nutrition 0.000 abstract description 5
- 241000607142 Salmonella Species 0.000 abstract description 5
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
- -1 re Species 0.000 abstract description 4
- 239000003814 drug Substances 0.000 description 19
- 230000001580 bacterial effect Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 229940079593 drug Drugs 0.000 description 7
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 5
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- 230000012010 growth Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 239000004599 antimicrobial Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002504 physiological saline solution Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 230000007928 solubilization Effects 0.000 description 2
- 238000005063 solubilization Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 description 1
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001332 colony forming effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 210000002919 epithelial cell Anatomy 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
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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
- 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
- A01N25/02—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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Zoology (AREA)
- Environmental Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Nanotechnology (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
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Abstract
The application provides a nano silver antibacterial agent and a preparation method thereof, and relates to the field of antibacterial agent preparation. The embodiment of the application provides a nano silver antibacterial agent, which belongs to an organic antibacterial agent, and not only can anions in a system stably exist, are uniformly dispersed in the system, but also have good sterilization effect, and have a Minimum Inhibitory Concentration (MIC) of less than 10 mug/ml for staphylococcus aureus, escherichia coli, salmonella and escherichia coli bacillus subtilis, and are suitable for wide control objects, but also have smaller required amount, so that the cost is saved. The preparation method is simple, the reaction conditions are not harsh, the processing modifier and the solubilizer are added in the preparation process, and the processing modifier and the solubilizer act synergistically in the system, so that nano silver and anions are uniformly dispersed in the system, the phenomenon of agglomeration can not occur, the utilization rate of silver is improved, and the antibacterial performance is more efficient.
Description
Technical Field
The application relates to the technical field of antibacterial agent preparation, in particular to a nano silver antibacterial agent and a preparation method thereof.
Background
Nano silver refers to silver nano by utilizing a front-edge nano technology, and the grain diameter of the nano silver is made into a nano-level metal silver simple substance. The particle size of the nano silver is smaller than 100nm and is generally between 25 and 50nm, the nano technology appears, so that the sterilizing capability of the silver in a nano state generates qualitative leap, very few nano silver can generate strong sterilizing effect, can kill 650 more bacteria in a few minutes, has small broad-spectrum sterilizing resistance, can promote wound healing, cell growth and damaged cell repair, has small toxic reaction, does not find any stimulating reaction on skin, opens up a wide prospect for widely applying the nano silver to perform sterilization, and is a new generation natural antibacterial agent. Meanwhile, it has the effect of promoting repair to damaged epithelial cells. It is worth mentioning that the product has increasingly enhanced antibacterial effect when meeting water, and is more beneficial to the treatment of diseases.
However, the use cost of nano silver is high, the required amount is large to achieve an ideal antibacterial effect, and anions in some inorganic silver-carrying antibacterial agents are not stable enough.
Disclosure of Invention
The aim of the application is to provide a nano silver antibacterial agent, which belongs to an organic antibacterial agent, so that anions in a system can exist stably, are uniformly dispersed in the system, have good sterilization effect, have Minimum Inhibitory Concentrations (MIC) of less than 10 mug/ml for staphylococcus aureus, escherichia coli, salmonella and escherichia coli bacillus subtilis, are suitable for wide control objects, have small required amount, and further save cost.
The preparation method is simple, the reaction conditions are not harsh, a processing modifier and a solubilizer are added in the preparation process, and the processing modifier and the solubilizer act synergistically in the system, so that nano silver and anions are uniformly dispersed in the system, the phenomenon of agglomeration is avoided, the silver utilization rate is improved, and the antibacterial performance is more efficient.
In order to solve the technical problems, the invention adopts the following technical scheme:
on one hand, the embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 0.3-1.3 parts of silver nitrate, 0.2-0.3 parts of nano silver particles, 80-100 parts of deionized water, 0.19-0.29 parts of sodium hydroxide, 0.8-2 parts of processing modifier, 0.2-1.5 parts of solubilizer and 0.2-0.3 part of zirconium phosphate.
On the other hand, the embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, adding a solubilizer and a mixed solution 1, adding a processing modifier, and stirring for 2-24 hours until the mixture is completely dissolved in water after stirring to obtain a mixed solution 2;
step C: filtering, drying, calcining and crushing the mixed solution 2, and then adding 75% alcohol by volume to obtain the nano silver antibacterial agent.
Compared with the prior art, the embodiment of the application has at least the following advantages or beneficial effects:
the embodiment of the application provides a nano silver antibacterial agent, which belongs to an organic antibacterial agent, and not only can anions in a system stably exist, are uniformly dispersed in the system, but also have good sterilization effect, and have a Minimum Inhibitory Concentration (MIC) of less than 10 mug/ml for staphylococcus aureus, escherichia coli, salmonella and escherichia coli bacillus subtilis, and are suitable for wide control objects, but also have smaller required amount, so that the cost is saved.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which is simple in preparation method, not harsh in reaction conditions, and adds a processing modifier and a solubilizer in the preparation process, and the processing modifier and the solubilizer act synergistically in the system, so that nano silver and anions are uniformly dispersed in the system, the phenomenon of agglomeration is avoided, the silver utilization rate is improved, and the antibacterial performance is more efficient.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail with reference to specific examples.
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 0.3-1.3 parts of silver nitrate, 0.2-0.3 parts of nano silver particles, 80-100 parts of deionized water, 0.19-0.29 parts of sodium hydroxide, 0.8-2 parts of processing modifier, 0.2-1.5 parts of solubilizer and 0.2-0.3 part of zirconium phosphate.
The solubilizer refers to a surfactant with solubilization capacity, and solubilization refers to a process of increasing solubility of a poorly soluble drug in a solvent and forming a solution under the action of the surfactant. The solubilizer is one of the surfactants, and the optimal hydrophilic-hydrophobic balance (HLB value) is l 5-l 8. The medicine can increase the solubility of the medicine, improve the content of main medicine in the preparation and has strong absorption effect. Thereby the medicine can reach the tissue part with a certain concentration to play a role in treatment and also can avoid toxic and side effects caused by long-term administration.
In some embodiments of the present application, the nano-silver particles have a particle size of 1-100nm.
In some embodiments of the present application, the concentration of the nano-silver particles is 20-300ppm.
In some embodiments of the present application, the processing modifier (ACR) is an acrylic resin copolymerized with acrylate and methacrylate monomers.
Acrylic resin synthesized by copolymerization of acrylic ester and methacrylic ester monomers is a thermoplastic resin. Can be repeatedly heated, softened, cooled and solidified. The polymer is a linear polymer compound, can be a homopolymer or a copolymer, has good physical and mechanical properties, and has excellent weather resistance, chemical resistance and water resistance, high light and color retention.
In some embodiments of the present application, the solubilizing agent is one or both of nonylphenol polyoxyethylene ether and octylphenol polyoxyethylene ether.
Octyl phenol polyoxyethylene ether is a chemical substance, is in the form of light yellow liquid, has high chemical stability, is not easily damaged by strong acid and strong alkali at high temperature, and has poor biodegradability. n=4, is readily soluble in oils and organic solvents; n >7, is soluble in water at room temperature. Has good emulsifying, dispersing and antistatic properties, can form a film on the surface of fruits and vegetables, has antibacterial properties, and plays roles in protection and fresh-keeping. Is nontoxic and harmless to human body.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, adding a solubilizer and a mixed solution 1, adding a processing modifier, and stirring for 2-24 hours until the mixture is completely dissolved in water after stirring to obtain a mixed solution 2;
step C: filtering, drying, calcining and crushing the mixed solution 2, and then adding 75% alcohol by volume to obtain the nano silver antibacterial agent.
In some embodiments of the present application, the conditions of the calcination process are: the temperature is 280-300 ℃ and the treatment time is 60-90min.
In some embodiments of the present application, the mesh number of the filtration is 80-120 mesh.
The features and capabilities of the present application are described in further detail below in connection with the examples.
Example 1
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 1.3 parts of silver nitrate, 0.3 part of nano silver particles, 100 parts of deionized water, 0.29 part of sodium hydroxide, 2 parts of acrylic resin, 1.5 parts of nonylphenol polyoxyethylene ether and 0.3 part of zirconium phosphate.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, then adding nonylphenol polyoxyethylene ether and the mixed solution 1, then adding acrylic resin, stirring for 24 hours until the mixture can be completely dissolved in water after stirring, and obtaining a mixed solution 2;
step C: filtering the mixed solution 2 through a 120-mesh sieve, drying, calcining at 300 ℃ for 60min, crushing, and adding 75% alcohol by volume fraction to obtain the nano silver antibacterial agent.
The processing modifier is an acrylic resin copolymerized from acrylate and methacrylate monomers.
Example 2
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 0.3 part of silver nitrate, 0.2 part of nano silver particles, 80 parts of deionized water, 0.19 part of sodium hydroxide, 0.8 part of acrylic resin, 0.2 part of nonylphenol polyoxyethylene ether and 0.2 part of zirconium phosphate.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, then adding nonylphenol polyoxyethylene ether and the mixed solution 1, then adding acrylic resin, stirring for 8 hours until the mixture can be completely dissolved in water after stirring, and obtaining a mixed solution 2;
step C: filtering the mixed solution 2 through a 80-mesh sieve, drying, calcining for 90min at the temperature of 280 ℃, crushing, and adding 75% alcohol by volume fraction to obtain the nano silver antibacterial agent.
The processing modifier is an acrylic resin copolymerized from acrylate and methacrylate monomers.
Example 3
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 0.8 part of silver nitrate, 0.25 part of nano silver particles, 90 parts of deionized water, 0.25 part of sodium hydroxide, 1.5 parts of acrylic resin, 1.0 part of octyl phenol polyoxyethylene ether and 0.28 part of zirconium phosphate.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, then adding octyl phenol polyoxyethylene ether and the mixed solution 1, then adding acrylic resin, stirring for 12 hours until the mixture can be completely dissolved in water after stirring, and obtaining a mixed solution 2;
step C: filtering the mixed solution 2 through a 100-mesh sieve, drying, calcining for 70min at the temperature of 290 ℃, crushing, and adding 75% alcohol by volume fraction to obtain the nano silver antibacterial agent.
The processing modifier is an acrylic resin copolymerized from acrylate and methacrylate monomers.
Example 4
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 1.1 parts of silver nitrate, 0.28 part of nano silver particles, 95 parts of deionized water, 0.26 part of sodium hydroxide, 1.8 parts of acrylic resin, 1.2 parts of octyl phenol polyoxyethylene ether and 0.23 part of zirconium phosphate.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, then adding octyl phenol polyoxyethylene ether and mixed solution 1, then adding acrylic resin, stirring for 2-24 hours until the mixture can be completely dissolved in water after stirring, and obtaining mixed solution 2;
step C: filtering the mixed solution 2 through a 110-mesh sieve, drying, calcining for 80min at the temperature of 295 ℃, crushing, and adding 75% alcohol by volume fraction to obtain the nano silver antibacterial agent.
The processing modifier is an acrylic resin copolymerized from acrylate and methacrylate monomers.
Comparative example 1
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 1.3 parts of silver nitrate, 0.3 part of nano silver particles, 100 parts of deionized water, 0.29 part of sodium hydroxide, 1.5 parts of nonylphenol polyoxyethylene ether and 0.3 part of zirconium phosphate.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, then adding nonylphenol polyoxyethylene ether and the mixed solution 1, and stirring for 24 hours until the mixture can be completely dissolved in water after stirring to obtain a mixed solution 2;
step C: filtering the mixed solution 2 through a 120-mesh sieve, drying, calcining at 300 ℃ for 60min, crushing, and adding 75% alcohol by volume fraction to obtain the nano silver antibacterial agent.
Comparative example 2
The embodiment of the application provides a nano silver antibacterial agent, which comprises the following raw materials in parts by weight: 1.3 parts of silver nitrate, 0.3 part of nano silver particles, 100 parts of deionized water, 0.29 part of sodium hydroxide, 2 parts of acrylic resin and 0.3 part of zirconium phosphate.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which comprises the following steps:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, then adding the mixed solution 1, adding acrylic resin, and stirring for 24 hours until the mixture can be completely dissolved in water after stirring to obtain a mixed solution 2;
step C: filtering the mixed solution 2 through a 120-mesh sieve, drying, calcining at 300 ℃ for 60min, crushing, and adding 75% alcohol by volume fraction to obtain the nano silver antibacterial agent.
The processing modifier is an acrylic resin copolymerized from acrylate and methacrylate monomers.
Experimental example
The minimum inhibitory concentration (minimal inhibit concentration, MIC) refers to the amount of drug contained in 1ml of the highest dilution tube that completely inhibits bacterial growth, i.e., the sensitivity of the bacteria being tested to the drug, as determined by tube dilution.
1. Principle of testing
The growth of the microorganism at different concentrations of the antimicrobial agent is measured by culturing the antimicrobial agent and the microorganism to be tested in a range of dilution, typically at a suspension concentration of 100 ten thousand Colony Forming Units (CFU) per milliliter (mL). The test system without antimicrobial activity shows turbidity due to the presence of microorganisms, while the absence of turbidity indicates that the growth of the microorganism to be tested is inhibited.
2. Bacterial content determination
(1) The bacterial solution was diluted 10-fold in a gradient with physiological saline (0.5 ml bacterial solution+4.5 ml physiological saline).
(2) And (3) dripping 0.1ml of each of three titer bacterial solutions of 10-5, 10-6 and 10-7 in the center of an agar plate, gently patting to uniformly spread the bacterial solutions without contacting the edge of the plate, making 2 plates for each gradient, and placing the plates into a 37 ℃ incubator for culturing for 16-24 hours.
(3) Counting the colony number: plates with 30-300 colonies were selected for counting. The results of the two plate counts were averaged to give a bacterial concentration, which required a growth turbidity of 9X 10 8 Personal-ml. Calculation example: the number of colonies grown on two plates of 10-6 is 68, 70, and the average of 69 colonies/0.1 ml, 1ml contains 6.90X10 of viable colony number 6 Each ml, i.e.the growth haze was 6.9X10 8 And each ml.
(4) The test bacterial liquid (prepared in step 3) is prepared by using broth as 1:10000 dilution (final turbidity 10).
3. Determination of bacteriostatic concentration
(1) 100 μl of blank broth containing TTC (5%) was added to each well of the first 3 rows (i.e., A, B, C rows) of 96-well plates.
(2) Adding 100 mu L of prepared liquid medicine (with the concentration of 512 mu g/ml) into a 1 st hole of A, B, C row, then carrying out double dilution on the medicine, namely adding the liquid medicine into the 1 st hole, fully blowing (at least 3 times) by a pipetting gun to fully mix the medicine with broth, then sucking 100 mu L of the medicine into the 2 nd hole, fully blowing to fully mix the medicine with broth, adding 100 mu L of the medicine into the 3 rd hole, repeating until the last hole is reached, and sucking 100 mu L of the medicine to be discarded; at this time, the concentration of the drug per well was 256, 128, 64, 32, 16, 8, 4, 2, 1, 0.5, 0.25, 0.125. Mu.g/ml in this order from left to right.
(3) 100. Mu.L of diluted bacteria solution was added to each well, and 3 replicates (A, B, C rows of samples) for determining MIC value of one drug were formed. At this time, the concentration of the drug per well, i.e., the final concentration of the drug, was 128, 64, 32, 16, 8, 4, 2, 1, 0, 0.5, 0.25, 0.125, 0.06 μg/ml in this order from left to right.
(4) A row of negative controls (blank broth alone without broth) and a row of positive controls (broth with broth without broth) were also made on the same plate.
(5) The 96-well culture plate is placed in a constant temperature incubator at 37 ℃ for 16-20 hours, and then the result is observed.
The nano silver antibacterial agents prepared in the examples 1-4 and the comparative examples were tested according to the test methods, and the minimum inhibitory concentrations (MIC, μg/ml) of the nano silver antibacterial agents prepared in the application against staphylococcus aureus, escherichia coli, salmonella and escherichia coli bacillus subtilis in broth are shown in Table 1:
TABLE 1 test results
As can be seen from Table 1, the antibacterial agents prepared in examples 1 to 4 all have high antibacterial effect, and the MIC values are very small, which means that the required amount is small and the cost is saved. The MIC values of the antibacterial agents prepared in comparative example 1 and comparative example 2 are larger than those of the antibacterial agents prepared in examples 1-4, and the effect of the antibacterial agents prepared in comparative example 1 is not good in example 1 with the same parameters because the acrylic resin serving as a processing modifier is not added in comparative example 1 and the polyoxyethylene nonylphenol ether serving as a solubilizer is not added in comparative example 2, so that the processing modifier and the solubilizer are indispensible and act synergistically in the system, and silver in the system is uniformly dispersed, so that the antibacterial agents can better exert the effect.
In summary, the embodiment of the application provides a nano silver antibacterial agent, which belongs to an organic antibacterial agent, and not only can anions in a system exist stably and are dispersed uniformly in the system, but also has good sterilization effect, and the Minimum Inhibitory Concentration (MIC) of staphylococcus aureus, escherichia coli, salmonella and escherichia coli bacillus subtilis is less than 10 mug/ml, so that suitable prevention and treatment objects are wide, the required amount is small, and the cost is saved.
The embodiment of the application provides a preparation method of a nano silver antibacterial agent, which is simple in preparation method, not harsh in reaction conditions, and adds a processing modifier and a solubilizer in the preparation process, and the processing modifier and the solubilizer act synergistically in the system, so that nano silver and anions are uniformly dispersed in the system, the phenomenon of agglomeration is avoided, the silver utilization rate is improved, and the antibacterial performance is more efficient.
The embodiments described above are some, but not all, of the embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
Claims (8)
1. The nano silver antibacterial agent is characterized by comprising the following raw materials in parts by weight: 0.3-1.3 parts of silver nitrate, 0.2-0.3 parts of nano silver particles, 80-100 parts of deionized water, 0.19-0.29 parts of sodium hydroxide, 0.8-2 parts of processing modifier, 0.2-1.5 parts of solubilizer and 0.2-0.3 part of zirconium phosphate.
2. The nano-silver antibacterial agent according to claim 1, wherein the nano-silver particles have a particle size of 1 to 100nm.
3. The nano-silver antibacterial agent according to claim 1, wherein the nano-silver particles concentration is 20-300ppm.
4. The nano-silver antibacterial agent according to claim 1, wherein the processing modifier (ACR) is an acrylic resin copolymerized with acrylate and methacrylate monomers.
5. The nano-silver antibacterial agent according to claim 1, wherein the solubilizing agent is one or both of nonylphenol polyoxyethylene ether and octylphenol polyoxyethylene ether.
6. A method for preparing the nano-silver antibacterial agent according to any one of claims 1 to 5, comprising the steps of:
step A: preparing silver nitrate into silver nitrate solution, preparing sodium hydroxide into sodium hydroxide solution, and mixing the silver nitrate solution with the sodium hydroxide solution to obtain mixed solution 1 for later use;
and (B) step (B): adding nano silver particles and zirconium phosphate into deionized water, adding a solubilizer and a mixed solution 1, adding a processing modifier, and stirring for 2-24 hours until the mixture is completely dissolved in water after stirring to obtain a mixed solution 2;
step C: filtering, drying, calcining and crushing the mixed solution 2, and then adding 75% alcohol by volume to obtain the nano silver antibacterial agent.
7. The method for preparing a nano-silver antibacterial agent according to claim 6, wherein the conditions of the calcination treatment are: the temperature is 280-300 ℃ and the treatment time is 60-90min.
8. The method for preparing a nano-silver antibacterial agent according to claim 6, wherein the mesh number of the filtration is 80-120 mesh.
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