CN114946877A - Nano antibacterial agent and preparation method thereof - Google Patents
Nano antibacterial agent and preparation method thereof Download PDFInfo
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- CN114946877A CN114946877A CN202210140496.7A CN202210140496A CN114946877A CN 114946877 A CN114946877 A CN 114946877A CN 202210140496 A CN202210140496 A CN 202210140496A CN 114946877 A CN114946877 A CN 114946877A
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- antibacterial agent
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- zirconium
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- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000011068 loading method Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000007709 nanocrystallization Methods 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- YHKRPJOUGGFYNB-UHFFFAOYSA-K sodium;zirconium(4+);phosphate Chemical compound [Na+].[Zr+4].[O-]P([O-])([O-])=O YHKRPJOUGGFYNB-UHFFFAOYSA-K 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052709 silver Inorganic materials 0.000 claims description 15
- 239000004332 silver Substances 0.000 claims description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000002539 nanocarrier Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000005342 ion exchange Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000011268 mixed slurry Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- -1 silver ions Chemical class 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 108091007643 Phosphate carriers Proteins 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 4
- 239000004599 antimicrobial Substances 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 3
- 229940039790 sodium oxalate Drugs 0.000 claims description 3
- RBWNDBNSJFCLBZ-UHFFFAOYSA-N 7-methyl-5,6,7,8-tetrahydro-3h-[1]benzothiolo[2,3-d]pyrimidine-4-thione Chemical compound N1=CNC(=S)C2=C1SC1=C2CCC(C)C1 RBWNDBNSJFCLBZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- 235000019445 benzyl alcohol Nutrition 0.000 claims description 2
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002114 nanocomposite Substances 0.000 claims description 2
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 claims description 2
- DAWBXZHBYOYVLB-UHFFFAOYSA-J oxalate;zirconium(4+) Chemical compound [Zr+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O DAWBXZHBYOYVLB-UHFFFAOYSA-J 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000011698 potassium fluoride Substances 0.000 claims description 2
- 235000003270 potassium fluoride Nutrition 0.000 claims description 2
- 239000011164 primary particle Substances 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 229940096017 silver fluoride Drugs 0.000 claims description 2
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000001308 synthesis method Methods 0.000 claims description 2
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 8
- 230000003287 optical effect Effects 0.000 abstract description 6
- 239000004033 plastic Substances 0.000 abstract description 5
- 229920003023 plastic Polymers 0.000 abstract description 5
- 239000000835 fiber Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 6
- 239000002609 medium Substances 0.000 description 6
- 239000004594 Masterbatch (MB) Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 239000001963 growth medium Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
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- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000006916 nutrient agar Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
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- 238000009501 film coating Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 231100000816 toxic dose Toxicity 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- 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 description 1
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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
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
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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
- A01N25/08—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 solids as carriers or diluents
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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
- A01N25/08—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 solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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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Abstract
The invention discloses a nano antibacterial agent and a preparation method thereof, and the specific process flow comprises the following steps: synthesis of a temperature-resistant carrier, nanocrystallization of the carrier, loading of an antibacterial component and calcination of an antibacterial agent. The antibacterial agent prepared by the method has the advantages of no toxicity, high-efficiency broad-spectrum antibacterial property, better color stability, excellent high-temperature stability, particularly better dispersity, simple and convenient preparation process, mild condition and low cost, and can be widely applied to the fields of plastics, fibers, ceramics, coatings and the like. The nano antibacterial powder prepared by the invention has the average size of less than 100nm and good dispersion performance, can not generate adverse effect on the optical performance of plastic products when being dispersed into solution or resin transparent solution or substrate, has the haze of not more than 5 percent, and can meet the antibacterial requirement in the strict field of optical performance.
Description
Technical Field
The invention relates to a preparation method of a nano antibacterial agent, belonging to the technical field of inorganic functional materials.
Background
Along with the improvement of science and technology and the improvement of living standard, the health consciousness of people is continuously enhanced, and urgent antibacterial demands are put forward for daily use, household appliances, bathrooms, building decoration materials, clothes, hats, clothes, medical materials and the like. Under such circumstances, it has become a general desire to improve the safety of production and living environments by using antibacterial materials for killing harmful bacteria and inhibiting their growth and reproduction.
The inorganic antibacterial agent is mainly prepared by utilizing the self-sterilization capability of metal, and has multiple advantages of excellent thermal stability, spectrum antibacterial property, long-acting antibacterial property, no drug resistance and the like. The silver has the most excellent antibacterial effect, and the toxic concentration or the minimum inhibitory concentration to unicellular organisms is more in the range of 0.1-20 mg/L.
NaZr 2 (PO 4 ) 3 Phosphate, a NASICON-configured phosphate, is the most commonly used antimicrobial carrier, and typically has a rhombohedral structure with a crystal structure consisting of PO 4 Tetrahedron and ZrO 6 Octahedrons are connected in a mode of sharing a vertex along the c axis to form a covalent bond network structure [ Zr ] 2 (PO 4 ) 3 ] - And repeating the steps to form a stable void structure, Na + The silver-loaded zirconium sodium phosphate antibacterial agent is positioned in the network cavities formed by the silver-loaded zirconium sodium phosphate antibacterial agent, can freely move through channels among the cavities, and is also easily exchanged by other external ions, so that the silver-loaded zirconium sodium phosphate antibacterial agent has extremely excellent ion exchange performance, and can be added into antibacterial plastics, antibacterial ceramics, antibacterial alloy and antibacterial fibers, so that the silver-loaded zirconium sodium phosphate antibacterial agent has a large market share in the field of antibacterial agents.
For example, in the preparation methods of the antibacterial agents disclosed in patents CN110934153A, CN102239887A, CN111387177A, CN112042639A and CN102763678A, cubic or flaky zirconium phosphate is used as a carrier, the particle size of the antibacterial agent is about 1 μm, and the finer carrier is added with a plurality of auxiliary agents such as template agents and introduction agents during the preparation process, or a complex ultrafiltration system is adopted, or ion exchange is performed for a plurality of times, so that the process is complex, and finer powder cannot be obtained.
Although silver-loaded antimicrobial agents currently in use have demonstrated excellent antimicrobial properties, they still suffer from a number of deficiencies. The first is that silver ions are released too quickly and the color stability of silver-based antibacterial agents is poor, which is not favorable for application in light-colored products. Secondly, the carrier size of the current commercially available antibacterial agent is large, the poor dispersibility not only can greatly reduce the antibacterial performance of the material, but also can greatly reduce the mechanical and optical properties of the matrix material by adding the antibacterial agent with larger size. As described above, reducing the particle size of the antibacterial material is an effective means for improving the dispersibility thereof and reducing the mechanical and optical properties of the base material.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art, and provides a nano antibacterial agent and a preparation method thereof, which can simultaneously solve the problems of temperature resistance of nano powder and the size of a nano carrier.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a preparation method of a nano antibacterial agent comprises the specific steps of synthesis of a temperature-resistant carrier, nanocrystallization of the carrier, loading of antibacterial components and calcination treatment of the antibacterial agent, wherein the size of the obtained nano carrier of the nano antibacterial agent is not more than 100nm, and the nano carrier is dispersed in a solution or film-forming resin to form a clear and transparent solution.
Preferably, the synthesis method of the temperature-resistant carrier comprises the following steps:
step 1: dissolving a mineralizer in deionized water, and stirring until the solid is completely dissolved, wherein the solution is marked as solution A; respectively dissolving a zirconium source and a phosphorus source in deionized water, and respectively marking as a solution B and a solution C;
step 2: dropwise adding the solution B into the solution A, stirring for at least 30min, uniformly mixing, then dropwise adding the solution C into the mixed solution to obtain mixed slurry, adjusting the pH value to be acidic by using a sodium hydroxide solution, and fully aging to obtain a precursor;
and step 3: and transferring the aged precursor into a high-pressure reaction kettle for heating, naturally cooling to room temperature after the reaction is finished, and filtering, washing and drying the obtained product to obtain the sodium zirconium phosphate nano temperature-resistant carrier with the primary particle size D90 being less than 200 nm.
Preferably, in the step 1, the phosphorus source compound: a zirconium source compound: the molar ratio of the mineralizer is (1-2): (2-4): (0.1 to 1);
preferably, in the step 2, the solid content refers to the mass ratio of the added materials to the total slurry mass, the solid content of the materials in the mixed slurry is 5-20 wt%, the pH of the mixed slurry is 1-6, the aging temperature is 20-70 ℃, and the aging time is 6-36 h; preferably, the solid content in the mixed slurry is 10-15 wt%. Preferably, the pH of the mixed slurry is 2-4. Preferably, the aging temperature is 50-70 ℃, and the aging time is 12-24 h.
Preferably, in the step 3, the hydrothermal reaction temperature is 100-210 ℃, and the reaction time is 1-24 h. Preferably, the reaction temperature is 150-180 ℃ and the reaction time is 3-12 h.
Preferably, the mineralizer is at least one of sodium oxalate, ammonium oxalate, potassium oxalate, oxalic acid and/or sodium fluoride, potassium fluoride and hydrofluoric acid; preferred are sodium oxalate and/or sodium fluoride.
Preferably, the zirconium source is at least one of zirconium oxychloride, zirconium sulfate, zirconium nitrate, zirconyl nitrate, zirconium oxalate; preferred is zirconium oxychloride.
Preferably, the phosphorus source is at least one of phosphoric acid, sodium monohydrogen phosphate, sodium dihydrogen phosphate and sodium polyphosphate. Sodium dihydrogen phosphate is preferred.
Preferably, the nanocrystallization adopts a wet sand-milling process, and the method comprises the following steps:
dispersing the sodium zirconium phosphate nanometer temperature-resistant carrier in water, sanding in a sand mill with a grinding medium to obtain slurry containing the sodium zirconium phosphate nanometer, and centrifuging and drying to obtain the sodium zirconium phosphate carrier with the average particle size of 20-100 nm.
Further preferably, the mass percent of the sodium zirconium phosphate in the slurry containing the nano sodium zirconium phosphate is 5-10%;
preferably, the sanding medium is zirconia balls with the average particle diameter of 0.1-0.5 mm, and the mixing ratio of the water to the ball milling medium calculated according to the volume ratio is (1-2): 1.
preferably, the sanding time is 6-24 h.
Preferably, the obtained nano zirconium sodium phosphate is used as a carrier, the loaded silver is used as an antibacterial component, and the loading method of the antibacterial component comprises the following steps:
dispersing a nano carrier in a solvent, adding soluble silver salt, fully performing adsorption or ion exchange, washing, and drying at normal pressure and low temperature;
and b, placing the dried nano carrier loaded with the silver ions into an electric furnace, and calcining to obtain the nano antibacterial agent.
The invention further takes the zirconium oxide microspheres as grinding media and adopts wet sanding to realize the nanocrystallization of the sodium zirconium phosphate. Obtaining the nano sodium zirconium phosphate with the average grain diameter of 20-100 nm.
Preferably, in the step a, the solid content is the mass percentage of sodium zirconium phosphate in the solvent, the solid content of the nano carrier calculated by mass percentage is 5-40 wt%, and the molar ratio of the soluble silver salt to the nano carrier is (0.1-1): 1, the pH value of ion exchange is 5-9, the temperature for carrying out ion exchange is 40-80 ℃, and the exchange time is 1-7 h; preferably, the solid content of the nano sodium zirconium phosphate is 10-20 wt%; preferably, the molar ratio of the soluble silver salt to the nano sodium zirconium phosphate is (0.25-0.5): 1; preferably, the pH value of the ion exchange is 6-8, the temperature for carrying out the ion exchange is 50-70 ℃, and the exchange time is 3-5 h.
Preferably, in the step a, the soluble silver salt compound is at least one selected from the group consisting of silver nitrate, silver perchlorate, chlorate, silver acetate, silver fluoride;
preferably, in the step a, the solvent for dispersing the sodium zirconium phosphate is at least one of water, ethanol, isopropanol, ethylene glycol, ethyl acetate and benzyl alcohol; water is preferred;
preferably, in the step b, the temperature for heat treatment of the nano composite silver-carrying powder is 400-900 ℃, and the heat preservation time is 1-10 h. Preferably, the calcination temperature is 500-700 ℃, and the heat preservation time is 3-5 h.
The invention relates to a nano antibacterial agent, which is prepared by the preparation method of the nano antibacterial agent.
Preferably, the antibacterial agent takes nano sodium zirconium phosphate as a carrier, the loading amount of silver in the nano antibacterial agent powder is 2-15 wt% according to the mass percentage, and the particle size of the antibacterial agent is 20-100 nm.
The antibacterial agent prepared by the invention has excellent discoloration resistance, the whiteness is kept above 90% after the antibacterial agent is continuously irradiated for 48 hours under ultraviolet light, meanwhile, the antibacterial agent prepared by the invention has good stability and better slow release performance, and the antibacterial rate of 1 wt% of antibacterial powder to escherichia coli and staphylococcus aureus can still reach 98% after the antibacterial powder is soaked in deionized water for 30 days.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the preparation method of the nano sodium zirconium phosphate carrier has the advantages of easily available raw materials, low cost, simple process and equipment, large flexibility of process parameters, short preparation period and mild conditions, and is suitable for large-area production;
2. the method adopts simple wet sanding to realize the nanocrystallization of the sodium zirconium phosphate, has low equipment requirement, effectively reduces the use of various auxiliary agents, and has high raw material utilization rate because the grinding medium and water can be recycled;
3. the nano zirconium sodium phosphate carrier prepared by the invention has many ion active sites and large ion exchange capacity, and can flexibly regulate and control the silver carrying capacity of the antibacterial agent by changing the adding amount of silver salt, thereby preparing the antibacterial agent meeting various requirements. Meanwhile, the prepared antibacterial agent has good slow release performance and can effectively realize long-acting antibiosis;
4. the nano silver-loaded sodium zirconium phosphate antibacterial powder prepared by the method is white, has good discoloration resistance and small average size, has small influence on the mechanical property of a matrix material, and can meet the antibacterial requirement of a light-colored fiber product;
5. the average size of the prepared nano antibacterial powder is less than 100nm, the dispersion performance is good, the nano antibacterial powder can be dispersed into a solution or resin such as PE, PA, PET, PMMA and other transparent solutions or substrates, the optical performance of a plastic product cannot be adversely affected, the haze of the obtained solution or film is less than 5%, and the antibacterial requirement in the field with strict optical performance can be met;
6. the method is simple and easy to implement, low in cost and suitable for popularization and application.
Drawings
FIG. 1 is an SEM image of sodium zirconium phosphate prior to sanding.
FIG. 2 is an SEM image of a nano antimicrobial.
FIG. 3 is a graph of the particle size distribution of sodium zirconium phosphate after sanding.
FIG. 4 is a graph showing the results of the nano-antimicrobial TG test.
FIG. 5 is a graph showing the antibacterial effect of the nano silver-loaded antibacterial agent prepared by the method.
Detailed Description
The present invention will be described in further detail with reference to examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this embodiment, a method for preparing a nano-antibacterial agent includes the following steps:
step 1: according to ZrOCl 2 ·8H 2 O：NaH 2 PO 4 : weighing the raw materials respectively in deionized water according to the molar ratio of 2:3.6:1, uniformly mixing, adjusting the pH to 3 by using a sodium hydroxide solution, aging at 50 ℃ for 12h, carrying out hydrothermal reaction at 180 ℃ for 24h, naturally cooling to room temperature after the reaction is finished, centrifuging and washing; then wet sanding, centrifuging and drying to obtain nano sodium zirconium phosphate;
step 2: dispersing nano sodium zirconium phosphate in deionized water by ultrasonic treatment to obtain 10 wt% suspension according to the weight ratio of NaZr 2 (PO 4 ) 3 ：AgNO 3 In a molar ratio of 1: 1, adding AgNO to the suspension 3 Stirring at 70 deg.C in dark for 5h, washing, and drying at normal pressure and low temperature; then fully grinding, and calcining for 5 hours at 500 ℃ in an electric furnace to obtain the nano antibacterial agent.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for preparing a nano-antibacterial agent includes the following steps:
step 1: according to ZrOCl 2 ·8H 2 O：NaH 2 PO 4 ：H 2 C 2 O 4 ·2H 2 Weighing raw materials according to the molar ratio of 2:3:0.5, respectively dissolving the raw materials in deionized water, uniformly mixing, adjusting the pH value to 3 by using a sodium hydroxide solution to obtain mixed slurry, ageing at normal temperature for 12 hours, carrying out hydrothermal reaction at 150 ℃ for 8 hours, naturally cooling to room temperature after the reaction is finished, centrifuging and washing; then wet sanding and drying are carried out to prepare the nano sodium zirconium phosphate;
step 2: dispersing nano sodium zirconium phosphate in deionized water by ultrasonic treatment to obtain 10 wt% suspension according to the weight ratio of NaZr 2 (PO 4 ) 3 ：AgNO 3 Is 0.25: 1 adding AgNO to the suspension 3 Stirring at 60 ℃ in a dark place for 3h, washing, and drying at normal pressure and low temperature; then fully grinding, and calcining for 5 hours at 500 ℃ in an electric furnace to obtain the nano antibacterial agent.
EXAMPLE III
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, the silver salt: the molar ratio of the carriers is different, other process conditions are consistent, and the Ag is + The loading results are shown in table 1.
Table 1. for different silver salts: table of Ag + ion loading mass percentage of carrier (molar ratio)
| Silver salt: carrier (molar ratio) | 0.25 | 0.3 | 0.4 | 0.5 | 0.6 | 0.75 | 0.8 | 1 |
| Ag + Mass percent | 4.49 | 5.67 | 6.72 | 8.61 | 10.04 | 11.95 | 11.89 | 13.05 |
Example four
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, the nano antibacterial agent prepared in the above example of the present invention was added to the PE master batch, and blown into a film.
Mixing the low-density polyethylene resin master batch, the nano antibacterial agent and the white oil according to the mass ratio of 100: 20: 0.05 stirring uniformly, then adding the mixture into a double-screw extruder for extrusion granulation, drying at low temperature after the first granulation is finished, and granulating again to obtain the antibacterial master batch. Mixing low-density polyethylene master batch and antibacterial master batch according to a mass ratio of 90: 10, then adding the mixed PE material into a film blowing machine to form a film, preparing an antibacterial PE film with the thickness of 20 mu m, and measuring the haze of the film to be 4%.
EXAMPLE five
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, the nano-antibacterial agent prepared by the present invention was added to the aqueous polyurethane to prepare a coating solution, and the coating solution was coated on the PET surface.
Mixing deionized water, the aqueous polyurethane emulsion and the nano antibacterial agent according to the mass ratio of 10:90:0.5, and adding a proper amount of film-forming auxiliary agent, defoaming agent, thickening agent and flatting agent to perform ultrasonic dispersion uniformly to prepare a film coating liquid. Then coated on the surface of clean PET to form an antibacterial coating with the thickness of about 20 μm, and the haze of the antibacterial coating is measured to be 3%.
EXAMPLE six
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, the antibacterial performance of the sodium zirconium phosphate nanoparticle prepared in the first example was measured by a filter paper method.
The nano antibacterial agent prepared in the first example is dispersed into 5mg/mL suspension by ultrasonic. Pouring in a sterilized plate with a diameter of 90mmAdding 15-20 ml of sterilized nutrient agar culture medium solution, solidifying, and transferring 100 μ L of culture medium solution with concentration of about 10 8 CFU/ml of Escherichia coli suspension, and coating uniformly. Then, three dry sterilized filter paper sheets with a diameter of 6mm were gently stuck on the medium with tweezers, 20. mu.L of the sample suspension was dropped on each filter paper sheet, 20. mu.L of sterilized distilled water was dropped on each blank control sheet, and Staphylococcus aureus was tested in the same manner. And after drying, inverting the mixture in a constant temperature and humidity incubator, culturing the mixture for 24 hours under the conditions that the T is 37 +/-0.5 ℃ and the RH is more than or equal to 90 percent, and observing the condition of the bacteriostatic ring around the filter paper sheet.
Comparative example
This embodiment is substantially the same as the above embodiment, and is characterized in that:
in this example, a commercially available antibacterial agent produced by a certain manufacturer was used as a comparative sample, and its antibacterial property was measured by a filter paper sheet method.
The commercially available antibacterial agent used in the comparative example was dispersed by sonication to a suspension of 5 mg/mL. Pouring 15-20 ml of sterilized nutrient agar culture medium solution into a sterilized plate with the diameter of 90mm, solidifying, and transferring 100 mu L of culture medium solution with the concentration of about 10 by using a liquid transfer gun 8 CFU/ml of Escherichia coli suspension, and coating uniformly. Then, three dry sterilized filter paper sheets with a diameter of 6mm were gently stuck on the medium with tweezers, 20. mu.L of the sample suspension was dropped on each filter paper sheet, 20. mu.L of sterilized distilled water was dropped on each blank control sheet, and Staphylococcus aureus was tested in the same manner. Drying, placing the filter paper upside down in a constant temperature and humidity incubator, culturing for 24h under the conditions that T is 37 +/-0.5 ℃ and RH is more than or equal to 90%, and observing the bacteriostatic ring condition around the filter paper sheet.
In summary, the specific process flow of the method for preparing the nano antibacterial agent according to the above embodiment of the present invention includes: synthesis of a temperature-resistant carrier, nanocrystallization of the carrier, loading of an antibacterial component and calcination of an antibacterial agent. The invention adopts a preparation method of a nano carrier, a phosphorus source and a zirconium source compound with a certain proportion are added into a solution containing a mineralizer, the pH value is adjusted to a proper value, the mixture is fully aged to obtain a precursor, and then the nano carrier is obtained through hydrothermal reaction. The antibacterial agent prepared by the method has the advantages of no toxicity, high-efficiency broad-spectrum antibacterial property, good color stability, excellent high-temperature stability, particularly good dispersibility, simple and convenient preparation process, mild conditions and low cost, and can be widely applied to the fields of plastics, fibers, ceramics, coatings and the like.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.
Claims (10)
1. A method for preparing a nano antibacterial agent is characterized by comprising the following steps: the method comprises the specific steps of synthesis of a temperature-resistant carrier, nanocrystallization of the carrier, loading of antibacterial components and calcination treatment of the antibacterial agent, wherein the size of the obtained nano antibacterial agent is not more than 100nm, and the nano antibacterial agent is dispersed in a solution or film-forming resin to form a clear and transparent solution.
2. The preparation method of the nano antibacterial agent according to claim 1, wherein the synthesis method of the temperature-resistant carrier comprises the following steps:
step 1: dissolving a mineralizer in deionized water, and stirring until the solid is completely dissolved, wherein the solution is marked as solution A; respectively dissolving a zirconium source and a phosphorus source in deionized water, and respectively marking as a solution B and a solution C;
and 2, step: dropwise adding the solution B into the solution A, stirring for at least 30min, uniformly mixing, then dropwise adding the solution C into the mixed solution to obtain mixed slurry, adjusting the pH value to be acidic by using a sodium hydroxide solution, and fully aging to obtain a precursor;
and step 3: and (3) transferring the aged precursor into a high-pressure reaction kettle for heating treatment, naturally cooling to room temperature after the reaction is finished, and filtering, washing and drying the obtained product to obtain the zirconium sodium phosphate nano temperature-resistant carrier with the primary particle size D90 being less than 200 nm.
3. The method for preparing nano antibacterial agent according to claim 2, characterized in that: in the step 1, the phosphorus source compound: a zirconium source compound: the molar ratio of the mineralizer is (1-2): (2-4): (0.1 to 1);
in the step 2, the solid content of the materials in the mixed slurry is 5-20 wt%, the pH of the mixed slurry is 1-6, the aging temperature is 20-70 ℃, and the aging time is 6-36 h;
in the step 3, the hydrothermal reaction temperature is 100-210 ℃, and the reaction time is 1-24 h.
4. The method for preparing nano antibacterial agent according to claim 2, characterized in that: the mineralizer is at least one of sodium oxalate, ammonium oxalate, potassium oxalate, oxalic acid and/or sodium fluoride, potassium fluoride and hydrofluoric acid;
the zirconium source is at least one of zirconium oxychloride, zirconium sulfate, zirconium nitrate, zirconyl nitrate and zirconium oxalate;
the phosphorus source is at least one of phosphoric acid, sodium monohydrogen phosphate, sodium dihydrogen phosphate and sodium polyphosphate.
5. The method for preparing the nano antibacterial agent according to claim 2, wherein the nano treatment adopts a wet sand grinding process, and the method comprises the following steps:
dispersing the sodium zirconium phosphate nanometer temperature-resistant carrier in water, sanding in a sand mill with a grinding medium to obtain slurry containing the sodium zirconium phosphate nanometer, and centrifuging and drying to obtain the sodium zirconium phosphate carrier with the average particle size of 20-100 nm.
6. The method for preparing nano antibacterial agent according to claim 5, characterized in that: the mass percent of the sodium zirconium phosphate in the slurry containing the nano sodium zirconium phosphate is 5-10 wt%;
the sanding medium is zirconia balls with the average particle size of 0.1-0.5 mm, and the mixing ratio of water and the ball milling medium calculated according to the volume ratio is (1-2): 1.
the sanding time is 6-24 h.
7. The preparation method of the nano antibacterial agent according to claim 5, characterized in that the obtained nano zirconium sodium phosphate is used as a carrier, and the loaded silver is used as an antibacterial component, and the loading method of the antibacterial component comprises the following steps:
dispersing a nano carrier in a solvent, adding soluble silver salt, fully performing adsorption or ion exchange, washing, and drying at normal pressure and low temperature;
and b, placing the dried nano carrier loaded with the silver ions into an electric furnace, and calcining to obtain the nano antibacterial agent.
8. The method for preparing nano antibacterial agent according to claim 7, characterized in that: in the step a, the solid content of the nano carrier is 5-40 wt%, and the molar ratio of the soluble silver salt to the nano carrier is (0.1-1): 1, the pH value of ion exchange is 5-9, the temperature for carrying out ion exchange is 40-80 ℃, and the exchange time is 1-7 h;
in the step a, the soluble silver salt compound is at least one selected from silver nitrate, silver perchlorate, chlorate, silver acetate and silver fluoride;
in the step a, the solvent for dispersing the sodium zirconium phosphate is at least one of water, ethanol, isopropanol, ethylene glycol, ethyl acetate and benzyl alcohol;
in the step b, the heat treatment temperature of the nano composite silver-carrying powder is 400-900 ℃, and the heat preservation time is 1-10 h.
9. A nano-antimicrobial agent characterized by: the nano antibacterial agent is prepared by the preparation method of the nano antibacterial agent as claimed in any one of claims 1 to 8.
10. The nano-antimicrobial agent according to claim 9, wherein: the antibacterial agent takes nano sodium zirconium phosphate as a carrier, the silver loading amount in the nano antibacterial agent powder is 2-15 wt% according to the mass percentage, and the particle size of the antibacterial agent is 20-100 nm.
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Application publication date: 20220830 |