CN116671515A - Nano silver antibacterial liquid and application thereof - Google Patents
Nano silver antibacterial liquid and application thereof Download PDFInfo
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- CN116671515A CN116671515A CN202310440110.9A CN202310440110A CN116671515A CN 116671515 A CN116671515 A CN 116671515A CN 202310440110 A CN202310440110 A CN 202310440110A CN 116671515 A CN116671515 A CN 116671515A
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- silver
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- antibacterial
- silver antibacterial
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 61
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000007788 liquid Substances 0.000 title claims abstract description 43
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 37
- 239000006185 dispersion Substances 0.000 claims abstract description 37
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 35
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003599 detergent Substances 0.000 claims abstract description 20
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000004359 castor oil Substances 0.000 claims description 15
- 235000019438 castor oil Nutrition 0.000 claims description 15
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 15
- 229920002749 Bacterial cellulose Polymers 0.000 claims description 13
- 239000005016 bacterial cellulose Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 10
- 229920002678 cellulose Polymers 0.000 claims description 10
- 239000001913 cellulose Substances 0.000 claims description 10
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 10
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 10
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 235000010980 cellulose Nutrition 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 3
- 150000001450 anions Chemical group 0.000 claims description 3
- 239000002736 nonionic surfactant Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- 125000003172 aldehyde group Chemical group 0.000 claims description 2
- 125000003368 amide group Chemical group 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000001413 amino acids Chemical class 0.000 claims description 2
- 229960003237 betaine Drugs 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims 1
- 239000011324 bead Substances 0.000 claims 1
- 239000003242 anti bacterial agent Substances 0.000 abstract description 5
- 229910052709 silver Inorganic materials 0.000 abstract description 5
- 239000004332 silver Substances 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- -1 silver ions Chemical class 0.000 description 9
- 229920001046 Nanocellulose Polymers 0.000 description 6
- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229960003500 triclosan Drugs 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OSDLLIBGSJNGJE-UHFFFAOYSA-N 4-chloro-3,5-dimethylphenol Chemical compound CC1=CC(O)=CC(C)=C1Cl OSDLLIBGSJNGJE-UHFFFAOYSA-N 0.000 description 2
- 229940123208 Biguanide Drugs 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000004283 biguanides Chemical class 0.000 description 2
- 239000003240 coconut oil Substances 0.000 description 2
- 235000019864 coconut oil Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229940116335 lauramide Drugs 0.000 description 2
- ILRSCQWREDREME-UHFFFAOYSA-N lauric acid amide propyl betaine Natural products CCCCCCCCCCCC(N)=O ILRSCQWREDREME-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- ZSBDPRIWBYHIAF-UHFFFAOYSA-N n-acetylacetamide Chemical compound CC(=O)NC(C)=O ZSBDPRIWBYHIAF-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 description 1
- 229940073507 cocamidopropyl betaine Drugs 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- A01P3/00—Fungicides
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/1206—Water-insoluble compounds free metals, e.g. aluminium grit or flakes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Organic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Plant Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Dentistry (AREA)
- Dispersion Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Toxicology (AREA)
- Molecular Biology (AREA)
- Emergency Medicine (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a nano silver antibacterial solution. The preparation method comprises the following steps: 1) Preparing an external structural agent dispersion liquid with the mass percentage content of 0.5-50%, and 2) uniformly adding silver-ammonia solution with the concentration of 0.01-0.25 mol/L into the external structural agent dispersion liquid; wherein, the mass ratio of the silver ammonia solution to the external structural agent is 1:30-1:5; 3) Adding a reducing agent into the mixed solution obtained in the step 2) to react so as to obtain nano silver antibacterial solution reduced on the surface of the external structural agent in situ; wherein the mass ratio of the reducing agent to the silver ammonia solution is 5:1-15:1, the reaction condition is heating to 40-80 ℃, and the reaction time is 0.5-12 hours. The nano silver antibacterial liquid is also disclosed as an antibacterial component for preparing a detergent. The invention can effectively solve the problem of unstable nano silver in silver antibacterial agent.
Description
Technical Field
The invention belongs to the technical field of detergents, and particularly relates to a nano silver antibacterial agent and application thereof.
Background
The components which can realize the sterilization and bacteriostasis effects in the detergent in the market at present are quaternary ammonium salts, biguanides, phenols and heavy metal silver ions. Because the general detergent formula is a compound system of anionic surfactant and nonionic surfactant, and quaternary ammonium salts and biguanides belong to cationic surfactant, when anions and cations coexist in the same system, flocculation can be generated through electrostatic attraction, and the situation of unstable formula can occur, so that certain formula limitation exists when the two antibacterial components are applied to the detergent. Commonly used phenolic antibacterial agents are triclosan, triclosan and 4-chloro-3, 5-dimethylphenol. Triclosan may be harmful to human bodies due to its toxicity and drug resistance, and has been limited by the U.S. FDA to enter the antibacterial washing product market, and the domestic "cosmetic safety technical Specification" (2015) also specifies the usage amount and scope of triclosan. Triclosan is safer than triclosan, but the antibacterial effect is relatively weak, and meanwhile, a certain color-changing risk exists, so that the appearance of the product is influenced. 4-chloro-3, 5-dimethylphenol has trace and extremely toxic effects on fish, and is discharged into natural water to influence the ecological system, and pseudomonas aeruginosa and a plurality of moulds have strong drug resistance.
Silver and its compounds have been used in various forms for a long time in various antibacterial products because of their advantages of safety, long-acting, broad-spectrum, sterile, and remarkable antibacterial effects. However, both silver ions and nano silver have the defects of instability and easy color change. Silver ions have strong photosensitive reaction and are easy to oxidize and change color when exposed to light or kept for a long time, and nano silver is used as a nano-scale product, has large specific surface area and high surface energy, is easy to agglomerate into large particles, and thus loses the characteristics of nano particles. Therefore, how to apply nano silver in detergent products more stably to achieve excellent antibacterial effect is still a problem to be solved by researchers in the field of detergents.
Disclosure of Invention
Based on the above, a first object of the present invention is to provide a nano silver antibacterial solution, so as to effectively solve the problem of instability of nano silver in the prior art.
A second object of the present invention is to provide an application of the above nano silver antibacterial solution.
In order to achieve the first object, the invention adopts the following technical scheme:
a nano silver antibacterial solution is prepared by the following method:
1) Preparing an external structural agent dispersion liquid with the mass percentage content of 0.5-50%,
2) Uniformly adding silver ammonia solution with the concentration of 0.01-0.25 mol/L into the external structural agent dispersion liquid; wherein, the mass ratio of the silver ammonia solution to the external structural agent is 1:30-1:5;
3) Adding a reducing agent into the mixed solution obtained in the step 2) to react so as to obtain nano silver antibacterial solution reduced on the surface of the external structural agent in situ; wherein the mass ratio of the reducing agent to the silver ammonia solution is 5:1-15:1, the reaction condition is heating to 40-80 ℃, and the reaction time is 0.5-12 hours.
Preferably, the external structurant in step 1) is one of nanocellulose, bacterial cellulose, microcrystalline cellulose, modified hydrogenated castor oil, modified cellulose, or a combination thereof. Wherein the nanocellulose can be prepared by physical, chemical or chemical plus physical methods. Further, both the modified hydrogenated castor oil and the modified cellulose are modified by anions. The main component of cellulose is a macromolecular compound formed by D-glucose with beta-1, 4 glycosidic bond, and because a large number of hydroxyl groups exist on a molecular chain, especially nano-scale cellulose, a large number of hydroxyl groups are exposed to cause the cellulose to display electronegativity in aqueous solution. And the silver ammonia solution shows positive charge, so silver ammonia ions can be adsorbed on the surface of cellulose fiber or modified castor oil through electrostatic attraction.
Preferably, the reducing agent is a surfactant having an aldehyde group, a hydroxyl group and/or an amide group. Further, the surfactant includes alkylamide betaine, alkylamide amine oxide, sodium alkenylsulfonate, lignin sulfonate, amide nonionic surfactant, and amino acid surfactant.
Preferably, in the step 1), the external structure agent is added to pure water, and then emulsified at a high speed of 2000 to 8000rpm for 5 to 15 minutes, so that the external structure agent is homogeneously dispersed in the pure water.
Preferably, the preparation method of the silver ammonia solution comprises the following steps: slowly dripping 2-10% ammonia water into 0.01-0.25 mol/L silver nitrate solution until the generated precipitate just disappears.
In order to achieve the second purpose, the invention adopts the following technical scheme:
the application of the nano silver antibacterial solution as described above is used as an antibacterial ingredient for preparing a detergent.
Preferably, the nano silver antibacterial solution is used in the detergent in a mass percentage of 0.1-10%.
Preferably, the detergent comprises a laundry detergent, a laundry gel, a floor cleaning agent and a glass cleaning agent.
Compared with the prior art, the invention has the following beneficial effects: (1) According to the invention, the external structural agent is used as a carrier, so that silver ammonia ions are adsorbed on the surface of the carrier, and when the reducing agent carries out reduction reaction on the silver ammonia ions adsorbed on the carrier, the generated particles are nano silver reduced on the surface of the external structural agent in situ, so that the silver ammonia ion nano silver has better stability compared with common nano silver. (2) The invention uses the external structuring agent as the carrier for in-situ reduction, and has a certain suspension effect, so that the nano silver loaded on the surface of the carrier is not easy to generate problems of precipitation and flocculation, and can achieve a more stable effect. (3) The reducing agent adopted by the invention is a surfactant molecule with weak reducibility, and can be used as the reducing agent in a formula system, and can also be used as the surfactant to play a role in the later stage when the nano silver antibacterial solution is applied to a detergent, so that the utilization rate of raw materials is greatly improved.
Detailed Description
The technical scheme of the present invention will be further described by specific examples, but the embodiments of the present invention are not limited thereto. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
The preparation of the nano silver antibacterial liquid comprises the following steps:
(1) 50g of bacterial cellulose was dispersed in 100g of water, and the dispersion was homogenized at 2000rpm for 15 minutes by a homogenizer to obtain a uniform bacterial cellulose dispersion.
(2) 2% ammonia water was slowly added dropwise to 5g of a silver nitrate solution having a molar concentration of 0.01mol/L until the resulting precipitate had just completely disappeared, to obtain a silver ammonia solution having a concentration of 0.01 mol/L. And adding the silver ammonia solution into the bacterial cellulose dispersion liquid, and uniformly stirring to obtain the bacterial fermentation cellulose silver ammonia ion loaded dispersion liquid.
(3) 25g of cocamidopropyl betaine is added into the dispersion liquid as a reducing agent, and the mixture is added to 60 ℃ and stirred for reaction for 2 hours in a dark place, so that the antibacterial liquid with nano silver loaded on the surface of bacterial cellulose is obtained.
Example 2
The preparation of the nano silver antibacterial liquid comprises the following steps:
(1) 2g of bacterial cellulose was dispersed in 100g of water, and the resulting solution was homogenized and dispersed at 8000rpm for 5 minutes by a homogenizer to obtain a uniform bacterial cellulose dispersion.
(2) 5% ammonia water was slowly added dropwise to 0.4g of a silver nitrate solution having a molar concentration of 0.20mol/L until the precipitate formed had just disappeared completely, to obtain a silver ammonia solution having a concentration of 0.20 mol/L. And adding the silver ammonia solution into the bacterial cellulose dispersion liquid, and uniformly stirring to obtain the bacterial cellulose silver ion loaded dispersion liquid.
(3) Adding 2g of coconut oil diacetyl amide as a reducing agent into the dispersion liquid, heating to 80 ℃, and stirring in a dark place for reaction for 0.5 hour to obtain the antibacterial liquid with the nano silver loaded on the surface of the bacterial cellulose.
Example 3
The preparation of the nano silver antibacterial liquid comprises the following steps:
(1) 0.5g of anionically modified hydrogenated castor oil was dispersed in 100g of water and homogeneously dispersed at a high speed of 5000rpm for 10 minutes by a homogenizer to obtain a uniform modified hydrogenated castor oil dispersion.
(2) 2% ammonia water was slowly added dropwise to 0.05g of a silver nitrate solution having a molar concentration of 0.25mol/L until the precipitate formed had just disappeared completely, to obtain a silver ammonia solution having a concentration of 0.25 mol/L. And adding the silver ammonia solution into the modified hydrogenated castor oil dispersion liquid, and uniformly stirring to obtain the modified hydrogenated castor oil silver ammonia ion loaded dispersion liquid.
(3) And adding 0.75g of alpha-sodium alkenyl sulfonate serving as a reducing agent into the dispersion liquid, heating to 40 ℃, and stirring for reaction for 12 hours in a dark place to obtain the antibacterial liquid with the nano silver loaded on the surface of the modified hydrogenated castor oil.
Example 4
The preparation of the nano silver antibacterial liquid comprises the following steps:
(1) 30g of anionically modified hydrogenated castor oil was dispersed in 100g of water and homogeneously dispersed at 6000rpm for 12 minutes by a homogenizer to obtain a uniform modified hydrogenated castor oil dispersion.
(2) 10% ammonia water was slowly added dropwise to 1g of a silver nitrate solution having a molar concentration of 0.1mol/L until the resulting precipitate had just completely disappeared, to obtain a silver ammonia solution having a concentration of 0.1 mol/L. And adding the silver ammonia solution into the modified hydrogenated castor oil dispersion liquid, and uniformly stirring to obtain the modified hydrogenated castor oil silver ammonia ion loaded dispersion liquid.
(3) 15g of sodium oleate is added into the dispersion liquid as a reducing agent, the mixture is heated to 45 ℃ and stirred for reaction for 4 hours in a dark place, and then the antibacterial liquid with nano silver loaded on the surface of the modified hydrogenated castor oil is obtained.
Example 5
The preparation of the nano silver antibacterial liquid comprises the following steps:
(1) 50g of microcrystalline cellulose was dispersed in 50g of water, and the dispersion was homogenized and dispersed at a high speed of 2000rpm for 15 minutes by a homogenizer to obtain a uniform microcrystalline cellulose dispersion.
(2) 2.5% ammonia water was slowly added dropwise to 5g of a silver nitrate solution having a molar concentration of 0.2mol/L until the precipitate formed had just disappeared completely, to obtain a silver ammonia solution having a concentration of 0.2 mol/L. Adding the silver ammonia solution into the microcrystalline cellulose dispersion liquid, and uniformly stirring to obtain the microcrystalline cellulose silver ammonia ion loaded dispersion liquid.
(3) And adding 25g of lauramide amine oxide serving as a reducing agent into the dispersion liquid, heating to 55 ℃, and stirring in a dark place for reaction for 6 hours to obtain the antibacterial liquid with the microcrystalline cellulose surface loaded with nano silver.
Example 6
The preparation of the nano silver antibacterial liquid comprises the following steps:
(1) 0.5g of nanocellulose was dispersed in 99.5g of water, and the dispersion was homogenized and dispersed at a high speed of 4000rpm for 8 minutes by a homogenizer to obtain a uniform nanocellulose dispersion.
(2) 5% ammonia water was slowly added dropwise to 0.05g of a silver nitrate solution having a molar concentration of 0.5mol/L until the precipitate formed had just disappeared completely, to obtain a silver ammonia solution having a concentration of 0.5 mol/L. Adding the silver ammonia solution into the nano cellulose dispersion liquid, and uniformly stirring to obtain the nano cellulose loaded silver ammonia ion dispersion liquid.
(3) And adding 0.25g of sodium lignin sulfonate serving as a reducing agent into the dispersion liquid, heating to 70 ℃, and stirring for reaction for 3 hours in a dark place to obtain the antibacterial liquid with nano-silver loaded on the surface of the nano-cellulose.
Comparative example 1
Preparation of a non-carrier nano silver antibacterial solution (no addition of bacterial cellulose, other amounts consistent with example 2):
(1) 5% ammonia water was slowly added dropwise to 0.4g of a silver nitrate solution having a molar concentration of 0.20mol/L until the precipitate formed had just disappeared completely, to obtain a silver ammonia solution having a concentration of 0.20 mol/L.
(2) 2g of coconut oil diacetyl amide is added into the silver ammonia solution as a reducing agent, and the silver ammonia solution is heated to 80 ℃ and stirred for reaction for 0.5 hour in a dark place, thus obtaining the antibacterial solution of nano silver.
Comparative example 2
Preparation of nano silver antibacterial solution (bacterial cellulose is added after silver ammonia solution is reduced, and other dosage is the same as that of example 5):
(1) 2.5% ammonia water was slowly added dropwise to 5g of a silver nitrate solution having a molar concentration of 0.2mol/L until the precipitate formed had just disappeared completely, to obtain a silver ammonia solution having a concentration of 0.2 mol/L.
(2) 25g of lauramide amine oxide is taken as a reducing agent, heated to 55 ℃ and stirred for reaction for 6 hours in the dark, and then the antibacterial solution of nano silver is obtained.
(3) 50g of microcrystalline cellulose was dispersed in 50g of water, and the dispersion was homogenized and dispersed at a high speed of 2000rpm for 15 minutes by a homogenizer to obtain a uniform microcrystalline cellulose dispersion.
(4) And (3) mixing the nano silver antibacterial solution obtained in the step (2) with the microcrystalline cellulose dispersion liquid to obtain a mixed solution.
The antibacterial solutions prepared in examples 1 to 6 and comparative examples 1 to 2 above were added to the same laundry detergent base material and stirred uniformly, and then the antibacterial agent-containing laundry detergent was tested for its antibacterial/bactericidal effect against staphylococcus aureus and escherichia coli, and for its appearance stability and antibacterial/bactericidal effect after storage at 45 ℃ for 3 months. The specific test method is as follows:
stability test
Taking a proper amount of laundry detergent containing an antibacterial agent, putting the laundry detergent into a 50ml transparent reagent bottle, putting a sample into a 45 ℃ oven for three months, taking out the sample, observing the appearance of the sample, and testing the bactericidal/bacteriostatic effect.
Test for killing/inhibiting bacteria
And (3) testing the killing/bacteriostasis rate according to a suspension quantitative method in QB/T2738-2012 daily chemical product antibacterial bacteriostasis effect evaluation method, wherein the test strains are escherichia coli and staphylococcus aureus. Assuming that the kill/inhibit ratio is not less than 90%, it means that the test passes the kill/inhibit test, and that the kill/inhibit ratio is less than 90%, and that the test does not pass the kill/inhibit test, and that the test is "X".
The test results of each example/comparative example are as follows:
TABLE 1
From the stability results and the killing/inhibiting results of examples 1 to 4, the nano-silver antibacterial liquid has good antibacterial effect, and the appearance and the antibacterial effect of the nano-silver antibacterial liquid are stable after being stored for 3 months in a baking oven at 45 ℃. Whereas comparative example 1 was oxidized and flocculated after a period of time at high temperature due to the lack of carrier and dispersion of the external structural agent, color change was generated, and antibacterial effect was weakened.
TABLE 2
From the external appearance and the antibacterial results of examples 5 and 6 and comparative example 2, it is apparent that the external structurant is added to the system after the silver-ammonia solution is reduced, so that the produced nano silver is difficult to be adsorbed on the surface of the external structurant, and the effect of stabilizing the nano silver is not strong. The benefit of the in situ reduction step of the present invention is demonstrated.
Claims (10)
1. The nano silver antibacterial liquid is characterized by being prepared by the following steps:
1) Preparing an external structural agent dispersion liquid with the mass percentage content of 0.5-50%,
2) Uniformly adding silver ammonia solution with the concentration of 0.01-0.25 mol/L into the external structural agent dispersion liquid; wherein, the mass ratio of the silver ammonia solution to the external structural agent is 1:30-1:5;
3) Adding a reducing agent into the mixed solution obtained in the step 2) to react so as to obtain nano silver antibacterial solution reduced on the surface of the external structural agent in situ; wherein the mass ratio of the reducing agent to the silver ammonia solution is 5:1-15:1, the reaction condition is heating to 40-80 ℃, and the reaction time is 0.5-12 hours.
2. The nano-silver antibacterial solution according to claim 1, wherein the external structurant in step 1) is one of nano-cellulose, bacterial cellulose, microcrystalline cellulose, modified hydrogenated castor oil, modified cellulose, or a combination thereof.
3. The nano-silver antibacterial solution according to claim 2, wherein both the modified hydrogenated castor oil and the modified cellulose are modified with anions.
4. The nano-silver antibacterial solution according to claim 1, wherein the reducing agent is a surfactant having aldehyde groups, hydroxyl groups and/or amide groups.
5. The nano-silver antibacterial solution according to claim 4, wherein the surfactant comprises alkylamide betaine, alkylamide amine oxide, sodium alkenylsulfonate, lignin sulfonate, amide nonionic surfactant and amino acid surfactant.
6. The nano-silver antibacterial solution according to claim 1, wherein in step 1), after the external structurant is added to the pure water, the external structurant is emulsified at a high speed of 2000 to 8000rpm for 5 to 15 minutes so as to be homogeneously dispersed in the pure water.
7. The nano-silver antibacterial solution according to claim 1, wherein the preparation method of the silver-ammonia solution is as follows: slowly dripping 2-10% ammonia water into 0.01-0.25 mol/L silver nitrate solution until the generated precipitate just disappears.
8. Use of the nano-silver antibacterial solution according to any one of claims 1 to 7 as antibacterial ingredient for the preparation of detergents.
9. The use according to claim 8, wherein the nano-silver antibacterial solution is used in the detergent in an amount of 0.1-10% by mass.
10. The use according to any one of claims 8 or 9, wherein the detergent comprises a laundry detergent, laundry gel beads, floor cleaning agent, glass cleaning agent.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007239077A (en) * | 2006-03-10 | 2007-09-20 | Mitsui Mining & Smelting Co Ltd | Method for producing particulate silver particle, and particulate silver particle obtained by the method |
| CN104399998A (en) * | 2014-10-22 | 2015-03-11 | 苏州正业昌智能科技有限公司 | Preparation method of graphene/nano-silver composite material |
| CN105033275A (en) * | 2015-06-15 | 2015-11-11 | 浙江理工大学 | Preparing method for synthesizing flake cellulose nanocrystalline/nano-silver hybridization particles through assistant reducing agent |
| CN108835125A (en) * | 2018-08-10 | 2018-11-20 | 湖州大本营科技有限公司 | A kind of preparation method and applications of micro-nano silver/chitosan compound anti-bacteria agent |
| CN111995799A (en) * | 2020-10-12 | 2020-11-27 | 江苏科技大学 | Preparation method of nano-silver/cellulose composite antibacterial material |
-
2023
- 2023-04-23 CN CN202310440110.9A patent/CN116671515A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007239077A (en) * | 2006-03-10 | 2007-09-20 | Mitsui Mining & Smelting Co Ltd | Method for producing particulate silver particle, and particulate silver particle obtained by the method |
| CN104399998A (en) * | 2014-10-22 | 2015-03-11 | 苏州正业昌智能科技有限公司 | Preparation method of graphene/nano-silver composite material |
| CN105033275A (en) * | 2015-06-15 | 2015-11-11 | 浙江理工大学 | Preparing method for synthesizing flake cellulose nanocrystalline/nano-silver hybridization particles through assistant reducing agent |
| CN108835125A (en) * | 2018-08-10 | 2018-11-20 | 湖州大本营科技有限公司 | A kind of preparation method and applications of micro-nano silver/chitosan compound anti-bacteria agent |
| CN111995799A (en) * | 2020-10-12 | 2020-11-27 | 江苏科技大学 | Preparation method of nano-silver/cellulose composite antibacterial material |
Non-Patent Citations (1)
| Title |
|---|
| JING CHEN ET AL: ""Microwave-assisted green synthesis of silver nanoparticles by carboxymethyl cellulose sodium and silver nitrate"", 《MATERILAS CHEMISTRY AND PHYSICS》, no. 108, pages 421 - 424 * |
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