CN114573015B - Nanometer zinc oxide composite antibacterial agent dispersion liquid and preparation method thereof - Google Patents
Nanometer zinc oxide composite antibacterial agent dispersion liquid and preparation method thereof Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 62
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 239000006185 dispersion Substances 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 241000411851 herbal medicine Species 0.000 claims abstract description 30
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 239000011701 zinc Substances 0.000 claims abstract description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008139 complexing agent Substances 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- 239000001509 sodium citrate Substances 0.000 claims abstract description 6
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 11
- 229920002472 Starch Polymers 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 235000019698 starch Nutrition 0.000 claims description 8
- 239000008107 starch Substances 0.000 claims description 8
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000000084 colloidal system Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- WPUMTJGUQUYPIV-JIZZDEOASA-L disodium (S)-malate Chemical compound [Na+].[Na+].[O-]C(=O)[C@@H](O)CC([O-])=O WPUMTJGUQUYPIV-JIZZDEOASA-L 0.000 claims description 3
- 235000019265 sodium DL-malate Nutrition 0.000 claims description 3
- 239000001394 sodium malate Substances 0.000 claims description 3
- 241000205585 Aquilegia canadensis Species 0.000 claims description 2
- 241000037740 Coptis chinensis Species 0.000 claims description 2
- 229920002774 Maltodextrin Polymers 0.000 claims description 2
- 239000005913 Maltodextrin Substances 0.000 claims description 2
- 241000972673 Phellodendron amurense Species 0.000 claims description 2
- 235000005187 Taraxacum officinale ssp. officinale Nutrition 0.000 claims description 2
- 239000002526 disodium citrate Substances 0.000 claims description 2
- 235000019262 disodium citrate Nutrition 0.000 claims description 2
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 claims description 2
- 229940035034 maltodextrin Drugs 0.000 claims description 2
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 claims description 2
- 239000001433 sodium tartrate Substances 0.000 claims description 2
- 229960002167 sodium tartrate Drugs 0.000 claims description 2
- 235000011004 sodium tartrates Nutrition 0.000 claims description 2
- 235000019263 trisodium citrate Nutrition 0.000 claims description 2
- 241000245665 Taraxacum Species 0.000 claims 1
- 229940124350 antibacterial drug Drugs 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000011068 loading method Methods 0.000 abstract description 4
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 abstract description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 10
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 239000003814 drug Substances 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 241000628997 Flos Species 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 210000002421 cell wall Anatomy 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- RZLVQBNCHSJZPX-UHFFFAOYSA-L zinc sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Zn+2].[O-]S([O-])(=O)=O RZLVQBNCHSJZPX-UHFFFAOYSA-L 0.000 description 3
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 244000000010 microbial pathogen Species 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 208000035473 Communicable disease Diseases 0.000 description 1
- 241000218202 Coptis Species 0.000 description 1
- 235000002991 Coptis groenlandica Nutrition 0.000 description 1
- 208000004232 Enteritis Diseases 0.000 description 1
- QQILFGKZUJYXGS-UHFFFAOYSA-N Indigo dye Chemical compound C1=CC=C2C(=O)C(C3=C(C4=CC=CC=C4N3)O)=NC2=C1 QQILFGKZUJYXGS-UHFFFAOYSA-N 0.000 description 1
- 241000972672 Phellodendron Species 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 240000004534 Scutellaria baicalensis Species 0.000 description 1
- 235000017089 Scutellaria baicalensis Nutrition 0.000 description 1
- 241000607764 Shigella dysenteriae Species 0.000 description 1
- 241000194017 Streptococcus Species 0.000 description 1
- 240000001949 Taraxacum officinale Species 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 239000010231 banlangen Substances 0.000 description 1
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 description 1
- 229940093265 berberine Drugs 0.000 description 1
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 231100000463 ecotoxicology Toxicity 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 208000006750 hematuria Diseases 0.000 description 1
- 230000004957 immunoregulator effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- 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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- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/12—Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a nano zinc oxide antibacterial agent and a preparation method thereof, belonging to the technical field of nano powder. The zinc source is added into sodium hydroxide solution to be directly precipitated to obtain nano zinc oxide, but the morphology controllability is affected by too fast reaction, so that a certain amount of urea is added to regulate the nano zinc oxide; in addition, complexing agents are added to prepare nano zinc oxide with different particle sizes, and preferably trisodium citrate is used as the complexing agent. The nano zinc oxide composite antibacterial agent is prepared by nano-forming the Chinese herbal medicine and compositing the nano zinc oxide. The nanometer zinc oxide and the nanometer Chinese herbal medicine are combined through polycarboxylic acid, and then the inorganic layered silicate dispersing agent is used for loading the nanometer zinc oxide and the nanometer Chinese herbal medicine, so that the composite antibacterial agent is formed. The nano zinc oxide composite antibacterial agent dispersion liquid with small particle size, uniform particle size distribution and small stability is prepared by a nano homogenization technology.
Description
Technical Field
The invention relates to the technical field of nano powder, in particular to a nano zinc oxide antibacterial agent and a preparation method thereof.
Background
Among the nano material antibacterial agents, nano zinc oxide has strong inhibition or killing effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus, salmonella and the like, and nano zinc oxide is used as a novel zinc source, has the characteristics of selective toxicity, good biocompatibility, higher bioactivity, good immunoregulatory capability, high absorptivity and the like, and is further researchedAttention of the researcher. The antibacterial mechanism is mainly composed of free Zn 2+ In addition, the nano zinc oxide particles have photocatalysis, can generate optical toxicity under the irradiation of visible light or ultraviolet rays and can generate lethal effect on bacteria. However, the use of nano zinc oxide increases the chance of zinc oxide being exposed to the body, which inevitably enters the environment and life, thus posing a hazard to human health and ecosystem safety, and thus the biosafety and ecotoxicology issues of nano zinc oxide have raised general attention (Journal of Biomedical Nanotechnology,2021,17,2420-2432). Therefore, reducing the dosage of nano zinc oxide and improving the effect of nano zinc oxide are hot research points.
The Chinese herbal medicine has good antibacterial effect, can inhibit growth and reproduction of pathogenic microorganisms, and can improve organism resistance, and can be used for treating infectious diseases. The antibacterial Chinese herbal medicine contains effective components such as alkaloid, flavonoid, coumarone extract and the like, and can inhibit and kill various pathogenic microorganisms. The Chinese herbal medicines with broad-spectrum antibacterial effect comprise flos Lonicerae, fructus forsythiae, folium Isatidis, radix Isatidis, indigo naturalis, coptidis rhizoma, cortex Phellodendri, scutellariae radix, herba Violae, herba Taraxaci, etc. For example, coptis chinensis and phellodendron bark have berberine as main components, have broad-spectrum antibacterial effect, and have inhibiting effect on various gram-negative bacteria and positive bacteria such as bacillus dysenteriae, pneumococcus, staphylococcus aureus, streptococcus and the like. It is commonly used for enteritis, pneumonia, hematuria, pyocutaneous disease, and swelling and toxicity. At present, the Chinese herbal medicine extract is used as an antibacterial preparation, so that a good effect is achieved.
The nanometer Chinese herbal medicine is applied to the field of Chinese herbal medicine, and after the Chinese herbal medicine is prepared into nanometer particles, the particles of the Chinese herbal medicine become very small, so that the contact area with a solvent is increased, and the dissolution rate and the dissolution amount of the components of the Chinese herbal medicine can be improved. The cell wall of the conventional traditional Chinese medicine is not damaged, and many effective components in the cells are difficult to penetrate the cell wall and cannot be extracted and utilized. If the traditional Chinese medicine is nanocrystallized, the cell wall is broken completely, and almost all the components in the cell can be extracted and utilized or directly taken and absorbed by human body. The bioavailability of insoluble drugs such as mineral drugs can be improved after the drugs are prepared into nano particles.
If the nano zinc oxide and the nano Chinese herbal medicine are used in a combined way, the antibacterial performance of the nano zinc oxide and the nano Chinese herbal medicine can be fully exerted, and the biological risk of the nano zinc oxide is reduced. Therefore, it is particularly important to develop a preparation process in which both are mixed. The organic matter is modified on the surface of the inorganic nano-particles, and common methods are surface modification, including physical modification and chemical modification. At present, physical modification is most commonly used, but the physical modification is combined through non-covalent bonds, so that the charge transfer efficiency between the physical modification and the non-covalent bonds is low, and the synergistic effect is not obvious.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a nano zinc oxide antibacterial agent with controllable morphology and particle size, and simultaneously provides a nano zinc oxide composite antibacterial agent dispersion liquid with extremely high dispersity.
The invention provides a preparation method of a nanometer zinc oxide antibacterial agent with controllable morphology and particle size, which comprises the following steps:
adding a zinc source into a mixed solution of sodium hydroxide and urea, adding a complexing agent, and reacting at 40-90 ℃.
Further, the molar ratio of sodium hydroxide to urea in the mixed solution of sodium hydroxide and urea is 0.032: (0.00-0.04), wherein the mole number of urea is not 0.
Further, the molar ratio of the sodium hydroxide to the zinc source in the mixed solution of the sodium hydroxide and the urea is 4:1.
Further, the complexing agent comprises one of disodium citrate, trisodium citrate, sodium malate or sodium tartrate, and the molar amount of the complexing agent is 5-50% of that of the zinc source.
The second object of the invention is to provide a nano zinc oxide prepared by the preparation method.
The invention provides a preparation method of nano zinc oxide composite antibacterial agent dispersion liquid prepared from the nano zinc oxide antibacterial agent, which comprises the following steps:
adding water-soluble polycarboxylic acid into water for dissolution, dividing the water-soluble polycarboxylic acid into 2 parts by volume, adding nano zinc oxide into one part of the water-soluble polycarboxylic acid, adding nano Chinese herbal medicine powder with equal mass, and simultaneously adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS) to obtain a first solution; adding the inorganic layered silicate dispersing agent into another part, homogenizing until all the inorganic layered silicate dispersing agent is fully contacted with water to form transparent colloid, and obtaining a second solution; finally, mixing the first solution with the second solution, and homogenizing; the water-soluble polycarboxylic acid accounts for 5-50wt%, the nano zinc oxide antibacterial agent accounts for 0.5-5wt%, EDC and NHS account for 0.5-5wt%, the inorganic layered silicate dispersant accounts for 0-10wt%, and the balance is water, wherein the total amount is 100wt%.
Further, the Chinese herbal medicine is one or more of dandelion, honeysuckle, coptis, phellodendron, scutellaria baicalensis or fructus forsythiae.
Further, the preparation method of the nano Chinese herbal medicine powder comprises the following steps: mixing the Chinese medicinal powder with soluble starch or maltodextrin, and grinding at low temperature for 2-10 min.
The invention discloses the following technical effects:
1. the invention prepares the nano zinc oxide with the grain diameter below 50nm by adopting a direct precipitation method. The key technology is as follows: the zinc source is added into the sodium hydroxide solution to directly precipitate to obtain nano zinc oxide, but the appearance controllability is affected by too fast reaction, so that a certain amount of urea is added to regulate the nano zinc oxide; in addition, complexing agents are added to prepare nano zinc oxide with different particle sizes, and preferably trisodium citrate is used as the complexing agent.
2. The invention prepares the nano zinc oxide composite antibacterial agent by nanocrystallizing Chinese herbal medicines and compositing the Chinese herbal medicines with nano zinc oxide. The key technology is as follows: the nanometer zinc oxide and the nanometer Chinese herbal medicine are combined through polycarboxylic acid, and then the inorganic layered silicate dispersing agent is used for loading the nanometer zinc oxide and the nanometer Chinese herbal medicine, so that the composite antibacterial agent is formed.
3. The invention prepares the nano zinc oxide composite antibacterial agent dispersion liquid with small particle size, uniform particle size distribution and good stability by the nano homogenization technology.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
0.008mol of zinc sulfate heptahydrate is added into a mixed solution of 0.032mol of sodium hydroxide and 0.04mol of urea, 0.004mol of trisodium citrate and 40g of deionized water are added, the reaction is carried out for 1h at 40 ℃, after the reaction is completed, the nano zinc oxide is obtained after washing with clear water for several times and drying.
Loading herba Taraxaci and Coptidis rhizoma and soluble starch into cell-grade superfine pulverizer (total mass of herba Taraxaci and Coptidis rhizoma is equal to that of soluble starch), and grinding at 10deg.C for 5 min to obtain nanometer Chinese herbal medicine powder.
5% of a water-soluble polycarboxylic acid was added to water for dissolution, and the mixture was divided into 2 parts by volume. Adding nano zinc oxide with the mass ratio of 0.5% into one part of the nano zinc oxide, adding nano Chinese herbal medicine powder with the same mass, and simultaneously adding 0.5% EDC and 0.5% NHS to obtain a first solution; adding 10% inorganic layered silicate dispersant into the other part, homogenizing until all inorganic layered silicate dispersants are in contact with water to fully and completely form transparent colloid, and obtaining a second solution; finally, the first solution and the second solution are mixed and homogenized. Preparing nano zinc oxide composite antibacterial agent dispersion liquid.
The antibacterial rate of the nano zinc oxide composite antibacterial agent dispersion liquid on the escherichia coli for 1 minute is 99.5 percent.
Example 2
0.008mol of zinc sulfate heptahydrate is added into a mixed solution of 0.032mol of sodium hydroxide and 0.03mol of urea, 0.024mol of trisodium citrate and 40g of deionized water are added, the reaction is carried out for 1h at 50 ℃, after the reaction is completed, the nano zinc oxide is obtained after washing with clear water for several times and drying.
Loading flos Lonicerae and soluble starch into cell-level superfine pulverizer (the mass of flos Lonicerae is equal to that of soluble starch), grinding at 10deg.C for 5 min, and making into nanometer Chinese herbal medicine powder.
10% of a water-soluble polycarboxylic acid was added to water for dissolution, and the mixture was divided into 2 parts by volume. Adding nano zinc oxide with the mass ratio of 1% into one part of the nano zinc oxide, adding nano Chinese herbal medicine powder with the same mass, and simultaneously adding 1% EDC and 1% NHS to obtain a first solution; adding 10% inorganic layered silicate dispersant into the other part, homogenizing until all inorganic layered silicate dispersants are in contact with water to fully and completely form transparent colloid, and obtaining a second solution; finally, the first solution and the second solution are mixed and homogenized. Preparing nano zinc oxide composite antibacterial agent dispersion liquid.
The antibacterial rate of the nano zinc oxide composite antibacterial agent dispersion liquid on the escherichia coli for 1 minute is 99.9 percent.
Example 3
0.008mol of zinc sulfate heptahydrate is added into a mixed solution of 0.032mol of sodium hydroxide and 0.02mol of urea, 0.032mol of sodium malate and 40g of deionized water are added, the reaction is carried out for 1h at 80 ℃, after the reaction is completed, the nano zinc oxide is obtained after washing with clear water for several times and drying.
Putting radix Scutellariae and fructus forsythiae and soluble starch into a cell-grade superfine pulverizer (the total mass of radix Scutellariae and fructus forsythiae is equal to that of soluble starch), grinding at 10deg.C for 5 min, and making into nanometer Chinese herbal medicine powder.
10% of a water-soluble polycarboxylic acid was added to water for dissolution, and the mixture was divided into 2 parts by volume. Adding nano zinc oxide with the mass ratio of 1% into one part of the nano zinc oxide, adding nano Chinese herbal medicine powder with the same mass, and simultaneously adding 1% EDC and 1% NHS to obtain a first solution; adding 5% inorganic layered silicate dispersant into the other part, homogenizing until all inorganic layered silicate dispersants are in contact with water to fully and completely form transparent colloid, and obtaining a second solution; finally, the first solution and the second solution are mixed and homogenized. Preparing nano zinc oxide composite antibacterial agent dispersion liquid.
The antibacterial rate of the nano zinc oxide composite antibacterial agent dispersion liquid on the escherichia coli for 1 minute is 99.0 percent.
Claims (4)
1. The preparation method of the nano zinc oxide composite antibacterial agent dispersion liquid is characterized by comprising the following steps:
adding water-soluble polycarboxylic acid into water for dissolution, dividing the water-soluble polycarboxylic acid into 2 parts by volume, adding nano zinc oxide into one part of the water-soluble polycarboxylic acid, adding nano Chinese herbal medicine powder with the same mass, and simultaneously adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide to obtain a first solution; adding the inorganic layered silicate dispersing agent into another part, homogenizing until all the inorganic layered silicate dispersing agent is fully contacted with water to form transparent colloid, and obtaining a second solution; finally, mixing the first solution with the second solution, and homogenizing; the water-soluble polycarboxylic acid accounts for 5-50wt%, the nano zinc oxide antibacterial agent accounts for 3-20wt%, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide account for 0.5-5wt%, the inorganic layered silicate dispersant accounts for 0-10wt%, and the balance is water, wherein the total amount is 100wt%;
the preparation method of the nano zinc oxide comprises the following steps: adding a zinc source into a mixed solution of sodium hydroxide and urea, adding a complexing agent, and reacting at 40-90 ℃, wherein the molar ratio of the sodium hydroxide to the zinc source in the mixed solution of sodium hydroxide and urea is 4:1, and the complexing agent is one of disodium citrate, trisodium citrate, sodium malate or sodium tartrate, and the molar amount is 5-50% of that of the zinc source.
2. The method for preparing nano zinc oxide composite antibacterial agent dispersion liquid according to claim 1, wherein the Chinese herbal medicine is one or more of dandelion, honeysuckle, coptis chinensis, phellodendron bark, radix scutellariae and fructus forsythiae.
3. The method for preparing the nano zinc oxide composite antibacterial agent dispersion liquid according to claim 1, which is characterized in that the nano Chinese herbal medicine preparation method comprises the following steps: mixing the Chinese medicinal powder with soluble starch or maltodextrin, and grinding at low temperature for 2-10 min.
4. The use of the nano zinc oxide composite antibacterial agent dispersion liquid prepared by the preparation method of any one of claims 1 to 3 in the preparation of antibacterial drugs.
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