CN114831122A - Antibacterial particles and preparation method thereof - Google Patents
Antibacterial particles and preparation method thereof Download PDFInfo
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- CN114831122A CN114831122A CN202110144341.6A CN202110144341A CN114831122A CN 114831122 A CN114831122 A CN 114831122A CN 202110144341 A CN202110144341 A CN 202110144341A CN 114831122 A CN114831122 A CN 114831122A
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- chitosan
- metal salt
- particles
- antibacterial
- solution
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- 239000002245 particle Substances 0.000 title claims abstract description 91
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 104
- 239000002184 metal Substances 0.000 claims abstract description 104
- 150000003839 salts Chemical class 0.000 claims abstract description 89
- 229920001661 Chitosan Polymers 0.000 claims abstract description 52
- 239000000243 solution Substances 0.000 claims abstract description 40
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 24
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000007863 gel particle Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 18
- 239000012046 mixed solvent Substances 0.000 claims abstract description 18
- 150000007524 organic acids Chemical class 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 150000004676 glycans Chemical class 0.000 claims abstract description 10
- 239000008187 granular material Substances 0.000 claims abstract description 10
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 10
- 239000005017 polysaccharide Substances 0.000 claims abstract description 10
- 230000000845 anti-microbial effect Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000004088 foaming agent Substances 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 8
- 239000004599 antimicrobial Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 21
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical group O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 229910001923 silver oxide Inorganic materials 0.000 claims description 10
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 5
- 239000005751 Copper oxide Substances 0.000 claims description 5
- 229910000431 copper oxide Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 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 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims 1
- 150000003751 zinc Chemical class 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 230000005764 inhibitory process Effects 0.000 description 18
- 238000010586 diagram Methods 0.000 description 16
- 239000000499 gel Substances 0.000 description 15
- 230000003385 bacteriostatic effect Effects 0.000 description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 230000006196 deacetylation Effects 0.000 description 4
- 238000003381 deacetylation reaction Methods 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 239000013384 organic framework Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 239000003361 porogen Substances 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 150000001556 benzimidazoles Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 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
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
-
- 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
-
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
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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
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
-
- 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
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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
- A01N59/20—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2248—Oxides; Hydroxides of metals of copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2286—Oxides; Hydroxides of metals of silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/415—Amides of aromatic carboxylic acids; Acylated aromatic amines
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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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- Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to an antibacterial particle and a preparation method thereof. An antimicrobial granule comprising a polysaccharide phase and a metal oxide phase, the polysaccharide phase having an organic backbone and the metal oxide phase being located within the organic backbone; the polysaccharide phase is chitosan. The preparation method of the antibacterial particles comprises the following steps: dissolving metal salt and chitosan in a mixed solvent of organic acid and water to form a chitosan-metal salt solution; adding a pore-foaming agent and a cross-linking agent into the chitosan-metal salt dissolving solution to form chitosan-metal salt gel; preparing the chitosan-metal salt gel into a plurality of chitosan-metal salt gel particles; soaking the chitosan-metal salt gel particles in a treating agent; drying the chitosan-metal salt gel particles soaked by the treating agent. The metal salt-chitosan two-phase antibacterial system is used for achieving a good antibacterial effect, and meanwhile, the particles are more environment-friendly by reducing the metal ion using amount and the characteristic that chitosan can be naturally degraded, is nontoxic and harmless.
Description
Technical Field
The invention relates to the technical field of antibacterial products, and particularly relates to antibacterial particles and a preparation method thereof.
Background
The antibacterial material is a functional material with sterilization and antibacterial properties, and the antibacterial effect is achieved mainly by adding an antibacterial agent. Among them, antibacterial particles are commonly used in the field of washing because of their advantages such as easy storage and transportation. The antibacterial particles are mainly classified into natural antibacterial particles, organic antibacterial particles and inorganic antibacterial particles.
The natural antibacterial particles are safe, environment-friendly and good in antibacterial property, but are difficult to realize industrialization due to poor heat resistance, short drug effect period and limited production conditions.
The organic antibacterial agent takes organic matters such as organic acids, phenols, quaternary ammonium salts, benzimidazoles and the like as antibacterial components, can effectively inhibit the propagation of harmful bacteria and mould, but has poor stability, easy decomposition and generally higher toxicity.
The inorganic antibacterial agent is prepared by adding metal or its ion with antibacterial ability into porous material such as zeolite and silica gel or glass. Compared with organic antibacterial particles, the inorganic antibacterial material has the characteristics of good persistence, broad-spectrum antibacterial property, good heat resistance and good safety, but is not as environment-friendly as natural antibacterial particles.
Therefore, how to consider environmental friendliness on the premise of ensuring antibacterial performance is a difficult problem to be solved urgently in the field of washing.
Disclosure of Invention
The invention mainly aims to provide antibacterial particles, which utilize a metal salt-chitosan two-phase antibacterial system to achieve a good antibacterial effect, and simultaneously, the particles are more environment-friendly by reducing the metal ion dosage and the characteristics of natural degradation, no toxicity and no harm of chitosan.
The invention also aims to provide a preparation method of the antibacterial particles, which can stably adsorb or coat the metal oxide in an organic framework formed by chitosan, and improves the stability and bacteriostasis rate of the particles.
In order to achieve the above purpose, the invention provides the following technical scheme:
an antimicrobial particle comprising a polysaccharide phase and a metal oxide phase, the polysaccharide phase having an organic backbone, the metal oxide phase having a metal oxide therein, the metal oxide being located in the organic backbone; the polysaccharide phase is chitosan.
A method of making antimicrobial granules, comprising:
dissolving metal salt and chitosan in a mixed solvent of organic acid and water to form a chitosan-metal salt solution;
adding a pore-foaming agent and a cross-linking agent into the chitosan-metal salt dissolving solution to form chitosan-metal salt gel;
preparing the chitosan-metal salt gel into a plurality of chitosan-metal salt gel particles;
soaking the chitosan-metal salt gel particles in a treating agent;
and drying the chitosan-metal salt gel particles soaked by the treating agent to obtain the chitosan-metal salt antibacterial particles.
Compared with the prior antibacterial particles, the two-phase antibacterial particles have the following technical effects.
1. Double antibacterial effect: the polysaccharide such as chitosan has strong antibacterial performance and wide antibacterial spectrum; meanwhile, the polysaccharide such as chitosan also has the characteristic of adsorbing heavy metal ions, so that the metal oxide can be stably adsorbed on the surface of the chitosan skeleton after being converted into metal ions in a solution environment, and the antibacterial effect is continuously exerted.
2. The chitosan is a degradable, nontoxic and environment-friendly material, so that the prepared antibacterial particles have high application value in the fields of washing, coating and the like.
3. Because the antibacterial particles have double antibacterial effects, the service life of the antibacterial particles can be prolonged compared with the existing antibacterial particles under the condition of the same content of antibacterial metal ions.
In some embodiments, the two-phase antibacterial particles provided by the present invention, the metal oxide includes silver oxide, and other metal oxides having antibacterial effect in practical sense, including but not limited to at least one of copper oxide, zinc oxide, etc., may be added.
In some embodiments, the product of the invention comprises chitosan having a degree of deacetylation of 80% to 90% to form shape-stable particles.
In some embodiments, the metal oxide comprises silver oxide, and the mass ratio of the silver oxide to the mass of the entire metal oxide phase is 10% or more, so as to achieve a higher antibacterial effect.
In some embodiments, the chitosan-metal salt bi-phase antimicrobial particles further comprise a cross-linking agent, wherein the cross-linking agent is glutaraldehyde, and the structural stability is increased by cross-linking.
In some embodiments, the chitosan phase and the metal oxide phase in the chitosan-metal salt dual-phase antibacterial particles are 90 to 96 percent and 4 to 10 percent respectively by mass.
In some embodiments, the metal oxide comprises silver oxide, copper oxide and zinc oxide, wherein the mass percentages of the chitosan, the silver oxide, the copper oxide and the zinc oxide are respectively 90-97%, 1.0-2.2%, 0-2% and 0-2%.
In some embodiments, the mass ratio of the silver salt in the total amount of all metal salts is above 10% to ensure that the particles have sufficient antimicrobial properties. The anionic form of the metal salt is not limited and includes, but is not limited to, typical nitrate, acetate, chloride salts and the like.
In some embodiments, the organic acid may be formic acid, acetic acid, propionic acid, butyric acid, etc., and the volume ratio of the organic acid in the mixed solvent is 3.5 to 4.5%.
In some embodiments, the dissolving the metal salt and the chitosan in a mixed solvent of an organic acid and water to form a chitosan-metal salt dissolved solution includes:
putting metal salt into a container filled with a mixed solvent of organic acid and water, and stirring to form a metal salt solution;
and (3) putting the chitosan into a container filled with the metal salt dissolving solution, and stirring to form the chitosan-metal salt dissolving solution.
In some embodiments, the amount of the mixed solvent used is 5 to 10g of chitosan dissolved per 100 mL.
In some embodiments, the agitation may be ultrasonic agitation, and more preferably, the water bath is heated during the agitation.
In some embodiments, dibutyl phthalate is used as a pore-forming agent, and 3-3.5 mL of pore-forming agent is added per 10g of chitosan.
In some embodiments, the crosslinking agent may be a glutaraldehyde solution with a concentration of 0.2% to 0.3%.
In some embodiments, the porogen and cross-linking agent may be added in steps, the porogen is added first, stirred for a certain time, then glutaraldehyde is added, and stirring is continued to form a stable framework structure.
In some embodiments, after the gel is formed, the gel is dispersed into a particulate form with a dropper or an automated extrusion device. When the antibacterial particles are used in the field of washing, the particle size is preferably 0.5-1.5 cm, so that the antibacterial particles can be conveniently taken and placed.
In some embodiments, the treating agent includes, but is not limited to, inorganic strong bases such as sodium hydroxide, potassium hydroxide, and the like. In some embodiments, the inorganic strong base solution is 1.5 to 2.5 wt% sodium hydroxide solution.
In some embodiments, in order to reduce the content of impurities in the particles so as not to cause inconvenience to the use, the method further comprises, after the soaking and before the drying: washing with ethanol solution and/or distilled water.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic diagram of a method for preparing an antibacterial granule according to the present invention;
fig. 2 is a schematic diagram of a method for preparing an antibacterial granule according to an embodiment of the present invention;
FIG. 3 is a diagram illustrating the morphology of a chitosan-metal salt gel according to an embodiment of the present invention;
FIG. 4 is a diagram illustrating the morphology of chitosan-metal salt gel particles provided in an embodiment of the present invention;
fig. 5 is a diagram of an initial bacteriostatic effect of chitosan-metal salt antibacterial particles provided by an embodiment of the present invention;
FIG. 6 is a diagram of the bacteriostatic effect of a ceramic silver ion antibacterial ball in the prior art;
fig. 7 is a diagram of the bacteriostatic effect of the antibacterial particles after 5 times of machine washing;
FIG. 8 is a diagram of the bacteriostatic effect of the antibacterial particles after 10 machine washes according to the embodiment of the present invention;
fig. 9 is a bacteriostatic effect diagram of the antibacterial particles after being washed by a machine 60 times according to the embodiment of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The raw materials, reagents or instruments used are not indicated by manufacturers, and all the raw materials, the reagents or the instruments are conventional products which can be obtained by commercial purchase or can be prepared according to the prior art. According to the invention, the metal oxide is stably adsorbed or coated in the organic framework formed by chitosan to obtain the metal salt-chitosan two-phase antibacterial particles, and a series of problems of unobvious antibacterial effect, environmental friendliness and the like of the existing antibacterial particles are solved. Fig. 1 is a schematic diagram of a method for preparing an antibacterial granule according to an embodiment of the present invention. As shown in fig. 1, the preparation method of the antibacterial granules comprises:
dissolving metal salt and chitosan in a mixed solvent of organic acid and water to form a chitosan-metal salt solution;
adding a pore-foaming agent and a cross-linking agent into the chitosan-metal salt dissolving solution to form chitosan-metal salt gel;
preparing the chitosan-metal salt gel into a plurality of chitosan-metal salt gel particles;
soaking the chitosan-metal salt gel particles in a treating agent;
and drying the chitosan-metal salt gel particles soaked by the treating agent to obtain the chitosan-metal salt antibacterial particles.
Specifically, firstly, metal salt and chitosan are mixed and dissolved in a mixed solvent of organic acid and water, and an emulsification system is obtained by means of dispersion means such as stirring; then adding a cross-linking agent and a pore-forming agent into the chitosan skeleton to obtain a chitosan skeleton with a certain porosity, wherein the metal salt is coated or adsorbed in the chitosan skeleton through electrostatic interaction or coordination bonds (chitosan coordinates chelated silver ions) in the cross-linking process, and finally the obtained phase is gelatinous; and dispersing the gel into particles with a certain particle size, soaking in an inorganic strong alkali solution, and drying to convert the metal salt into metal oxide, thereby obtaining the chitosan-metal salt antibacterial particles. The antibacterial particles obtained by the method have the characteristics of dual antibacterial effects, porosity, degradability, no toxicity, environmental friendliness, long service life and the like.
In various embodiments, the type and amount of raw materials, operating temperature and time, etc. variables in the above-described processes can be varied to obtain particles with different properties.
For example, the metal salt may be a nitrate, acetate, chloride, or the like of a metal element such as silver, gold, copper, or the like. In a preferred embodiment, at least a silver salt is included. The mass ratio of the silver salt in the total amount of all metal salts is 10% or more, more preferably 40% or more, to ensure sufficient antibacterial property of the particles.
The chitosan is preferably chitosan with a degree of deacetylation of 80% to 90% to form shape stable particles, more preferably with a degree of deacetylation of 85%.
The proportion of the chitosan and the metal salt is determined according to the ratio of the compounds in the final particles, and the proportion of the mass of the silver oxide in the mass of the whole metal oxide phase is preferably more than 10 percent so as to achieve higher antibacterial effect. In some preferred embodiments, the mass percentages of the chitosan phase and the metal oxide phase in the antibacterial particles are 90-96% and 4-10%, respectively. More preferably, the mass percentages of the chitosan, the silver oxide, the copper oxide and the zinc oxide are respectively 90-97%, 1.0-2.2%, 0-2% and 0-2%.
The organic acid used in the method can be formic acid, acetic acid, propionic acid, butyric acid and the like, and a better emulsification effect can be obtained when the volume ratio of the organic acid in the mixed solvent is 3.5-4.5%, and the volume ratio can be 3.5%, 3.6%, 3.7%, 3.8%, 3.9%, 3.5%, 4.1%, 4.3%, 4.5% and the like, and is optional within the range. The amount of the mixed solvent is preferably 5 to 10g of chitosan per 100mL of the mixed solvent. When the solution is dissolved, it may be appropriately heated, for example, in a water bath at 60 ℃ for 8min or more while stirring.
The dissolving manner of the metal salt and the chitosan in the mixed solvent is various, including but not limited to the following manners:
putting metal salt into a container filled with a mixed solvent of organic acid and water, and stirring to form a metal salt solution;
and (3) putting the chitosan into a container filled with the metal salt dissolving solution, and stirring to form the chitosan-metal salt dissolving solution.
Wherein, the stirring can be ultrasonic stirring, and more preferably, the water bath is heated during the stirring process.
The pore-foaming agent used in the invention can adopt a typical pore-foaming compound, and the addition amount of the pore-foaming agent should comprehensively consider factors such as porosity, particle strength, stability and the like. Taking dibutyl phthalate as an example of a pore-forming agent, 3-3.5 mL of the pore-forming agent is added into every 10g of chitosan to achieve better comprehensive performance.
The cross-linking agent used in the present invention may be any cross-linking agent which can cross-link chitosan to form an organic skeleton, such as glutaraldehyde, and is preferably added in the form of a 0.2% to 0.3% concentration solution.
The pore-foaming agent and the cross-linking agent glutaraldehyde can be added step by step to form a stable skeleton structure, and the preferable mode is as follows: adding pore-foaming agent, stirring for a certain time, then adding glutaraldehyde, and continuing stirring. Glutaraldehyde is added as a solution at a concentration of 0.2% to 0.3%, more preferably 0.25%, to form chitosan microspheres of regular and uniform shape.
After the gel is formed, the gel is dispersed into a pellet form by any means, for example, by extrusion into a pellet form using a dropper or an automatic extrusion device. The type of automatic extrusion device is generally determined according to the particle size. When the antibacterial particles are directly used for washing, the antibacterial particles are more suitable for large particles of cm grade, and a cutting type device is preferably selected; when the antibacterial particles are used for products such as paint, the antibacterial particles are suitably prepared into particles, and devices such as atomization and dispersion devices are suitably selected.
When the antibacterial particles are used in the field of washing, the particle size is preferably 0.5-1.5 cm, so that the antibacterial particles can be conveniently taken and placed.
The treating agent mainly has the function of oxidizing metal, the soaking time is preferably more than 3 hours, and the selected strong base comprises but is not limited to inorganic strong bases such as sodium hydroxide, potassium hydroxide and the like. In some preferred embodiments, the inorganic strong alkali solution is 1.5 to 2.5 wt% sodium hydroxide solution. The treatment mode and practice are preferably as follows: and soaking the chitosan-metal salt particles in 1.5-2.5 wt% of sodium hydroxide solution for more than 3 hours.
In order to reduce the impurity content in the particles so as not to cause inconvenience to the use, the method further comprises the following steps after the soaking and before the drying: washed with an ethanol solution (e.g., a typical 50% ethanol solution) and/or distilled water.
The main principle of the two-phase antibacterial particle prepared by the preparation method of the invention is as follows: mixing and dissolving metal salt and chitosan in a mixed solvent of organic acid and water, and performing dispersion processes such as stirring to obtain an emulsification system; then adding a cross-linking agent and a pore-forming agent into the chitosan skeleton to obtain a chitosan skeleton with a certain porosity, wherein the metal salt is coated or adsorbed in the chitosan skeleton through electrostatic interaction or coordination bonds (chitosan coordinates chelated silver ions) in the cross-linking process, and finally the obtained phase is gelatinous; then dispersing the gel into particles with certain particle size, and then soaking and drying the particles in an inorganic strong alkali solution to convert the metal salt into metal oxide. In conclusion, the invention adopts the processes of emulsification, crosslinking and oxidation to prepare the metal salt-chitosan two-phase antibacterial particles without complex equipment.
Fig. 2 is a schematic diagram of another method for preparing antibacterial particles according to an embodiment of the present invention. As shown in fig. 2, the preparation method of the antibacterial granules includes:
dissolving 0.5g of metal salt (composed of mixed silver nitrate and copper acetate, wherein the mass ratio of the silver nitrate can be 10%, 20%, 30%, 40% and 50%) in 100mL of 4% acetic acid, carrying out ultrasonic treatment for 5min to completely dissolve the metal salt, then adding 8g of chitosan (deacetylation degree of about 85%), stirring until no large insoluble particles exist, then placing the mixture in a water bath kettle, heating at 60 ℃ for 8min, and continuing stirring until complete dissolution is achieved to form the chitosan-metal salt dissolving solution.
Adding 5mL dibutyl phthalate into the dissolved chitosan-metal salt solution, stirring for 5min, adding 10mL glutaraldehyde solution, and continuing stirring for 10min to form chitosan-metal salt gel, as shown in FIG. 3. In the embodiment, a glutaraldehyde solution is used as a cross-linking agent, the concentration of glutaraldehyde is 0.2-0.3%, the cross-linking agent is too little, and the mechanical strength of particles is poor; too high content, high gel strength during preparation, difficult control of particle morphology, and possibly influence silver release. The chitosan-metal salt gel is kneaded into particles, or in order to obtain chitosan-metal salt gel particles with uniform size, the chitosan-metal salt gel can be placed into a dropper with a certain diameter and then dropped into particles through the dropper, preferably, the diameter of the chitosan-metal salt gel particles is controlled to be about 1cm, as shown in fig. 4.
Soaking the obtained chitosan-metal salt gel particles in 2 wt% sodium hydroxide solution (the surface is not smooth and becomes smooth in about 10 min) for 3h, washing with distilled water, then placing in 50% ethanol solution, sealing and soaking for 2h (completely soaking), washing with distilled water to neutrality, and taking out. Drying in an oven to obtain chitosan-metal salt dual-phase bacteriostatic particles (with a diameter of about 0.5cm), as shown in fig. 5 as particles 501. Fig. 5 is a schematic diagram of a zone of inhibition generated by the chitosan-metal salt dual-phase bacteriostatic particles obtained in this example in a petri dish (tap water is filled in the petri dish), and as shown in fig. 5, the chitosan-metal salt dual-phase bacteriostatic particles obtained in this example generate a zone of inhibition 502 of about 0.7cm in the tap water. For comparison, fig. 6 is a schematic diagram of a zone of inhibition generated by a ceramic silver ion antibacterial ball 601 in a petri dish (containing tap water in the petri dish) in the prior art, and as shown in fig. 6, the ceramic silver ion antibacterial ball in the prior art generates a zone of inhibition 602 of about 0.2cm in the tap water.
Fig. 7 is a schematic diagram of a zone of inhibition generated in a culture dish after 5 times of machine washing of the chitosan-metal salt dual-phase bacteriostatic particles in fig. 5, fig. 8 is a schematic diagram of a zone of inhibition generated in a culture dish after 10 times of machine washing of the chitosan-metal salt dual-phase bacteriostatic particles in fig. 5, and fig. 9 is a schematic diagram of a zone of inhibition generated in a culture dish after 60 times of machine washing of the chitosan-metal salt dual-phase bacteriostatic particles in fig. 5. Comparing the sizes of the inhibition zone 502 in fig. 5(0 time of machine washing), the inhibition zone 702 in fig. 7(5 time of machine washing), the inhibition zone 802 in fig. 8(10 time of machine washing), and the inhibition zone 902 in fig. 9(60 time of machine washing), it can be seen that the size of the inhibition zone after 60 times of machine washing of the chitosan-metal salt dual-phase inhibition particles is almost the same as the size of the inhibition zone after 5 times of machine washing, which indicates that the chitosan-metal salt dual-phase inhibition particles prepared by the embodiment of the present application still maintain a high inhibition effect after multiple times of washing, i.e., the chitosan-metal salt dual-phase inhibition particles prepared by the embodiment of the present application maintain a good inhibition effect for a long time, and have a longer service cycle.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (18)
1. An antimicrobial granule comprising a polysaccharide phase having an organic backbone and a metal oxide phase located within the organic backbone; the polysaccharide phase is chitosan.
2. The antimicrobial particles of claim 1, wherein the metal oxide comprises one or a combination of two or more of silver oxide, copper oxide, and zinc oxide.
3. The antibacterial particle according to claim 1, wherein the metal oxide phase contains silver oxide, and the proportion of the mass of the silver oxide to the mass of the entire metal oxide phase is 10% or more.
4. The antimicrobial particles of claim 1, further comprising a cross-linking agent, wherein the cross-linking agent is glutaraldehyde.
5. The antibacterial particle according to claim 1, wherein the mass percentages of the chitosan phase and the metal oxide phase in the antibacterial particle are 90-96% and 4-10%, respectively.
6. A method of making the antimicrobial granules of claim 1, comprising:
dissolving metal salt and chitosan in a mixed solvent of organic acid and water to form a chitosan-metal salt solution;
adding a pore-foaming agent and a cross-linking agent into the chitosan-metal salt dissolving solution to form chitosan-metal salt gel;
preparing the chitosan-metal salt gel into a plurality of chitosan-metal salt gel particles;
soaking the chitosan-metal salt gel particles in a treating agent;
and drying the chitosan-metal salt gel particles soaked by the treating agent to obtain the chitosan-metal salt antibacterial particles.
7. The method for preparing antibacterial granules according to claim 6, wherein the dissolving of the metal salt and chitosan in the mixed solvent of organic acid and water to form a chitosan-metal salt dissolved solution comprises:
putting metal salt into a container filled with a mixed solvent of organic acid and water, and stirring to form a metal salt solution;
and (3) putting the chitosan into a container filled with the metal salt dissolving solution, and stirring to form the chitosan-metal salt dissolving solution.
8. The method of claim 7, wherein the stirring in the solution of forming the chitosan-metal salt comprises ultrasonic stirring.
9. The method of claim 7 or 8, wherein the stirring comprises water bath heating stirring.
10. The preparation method according to claim 6, wherein the pore-forming agent is dibutyl phthalate, and the cross-linking agent is glutaraldehyde.
11. The method according to claim 6, wherein the treating agent is 1.5 to 2.5 wt% sodium hydroxide solution.
12. The method according to claim 11, wherein the chitosan-metal salt gel particles are soaked in 1.5-2.5 wt% sodium hydroxide solution for more than 3 hours.
13. The method of claim 6, wherein after the chitosan-metal salt gel particles are soaked in the treatment agent and before the chitosan-metal salt gel particles soaked in the treatment agent are dried, the method further comprises:
washing the chitosan-metal salt gel particles with an ethanol solution and/or distilled water.
14. The method of claim 13, wherein the ethanol solution is a 50% ethanol solution, and the 50% ethanol solution completely immerses the chitosan-metal salt gel particles.
15. The preparation method according to claim 6, wherein 3-3.5 mL of pore-forming agent is added per 10g of chitosan.
16. The method according to claim 6, wherein the volume ratio of the organic acid in the mixed solvent is 3.5 to 4.5%.
17. The method according to claim 6, wherein the metal salt includes a silver salt, a zinc salt, and a copper salt, and the mass ratio of the silver salt is 10% or more in the total amount of all the metal salts.
18. The method of claim 10, wherein the glutaraldehyde is added in the form of a 0.2-0.3% strength solution.
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