CN106106522A - A kind of nano zine oxide carries silver chitosan compound anti-bacteria agent and preparation method thereof - Google Patents
A kind of nano zine oxide carries silver chitosan compound anti-bacteria agent and preparation method thereof Download PDFInfo
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- CN106106522A CN106106522A CN201610482787.9A CN201610482787A CN106106522A CN 106106522 A CN106106522 A CN 106106522A CN 201610482787 A CN201610482787 A CN 201610482787A CN 106106522 A CN106106522 A CN 106106522A
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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
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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
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Abstract
The invention discloses a kind of nano zine oxide and carry silver chitosan compound anti-bacteria agent and preparation method thereof, preparation method is: under the conditions of stirring at normal temperature, chitosan is dissolved in acetic acid aqueous solution or aqueous formic acid, it is sequentially added into Polyethylene Glycol and hydroxyethyl cellulose, stir, add silver nitrate aqueous solution, stir, react under 100 115 DEG C of microwave conditions, it is naturally cooling to room temperature, adding nano zine oxide, it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide carries silver chitosan compound anti-bacteria agent.Utilizing the reproducibility hydroxyl of chitosan body as silver ion reducing agent, be not re-introduced into new reducing agent, one-step method prepares and carries silver chitosan solution；Utilizing microwave to synthesize, be greatly shortened the response time, reaction system is prepared mostly under normal temperature condition, and the nanometer silver even particle size distribution obtained, and reunion situation is substantially reduced；Anti-microbial property is excellent；Biological safety is high；Method is simple, and production cost is relatively low.
Description
Technical field
The present invention relates to silver-colored chitosan compound anti-bacteria agent of a kind of nano zine oxide-loads and preparation method thereof, belong to inorganic-have
The preparation of machine hydridization anti-biotic material and applied technical field thereof.
Background technology
Antibacterial refers within a certain period of time, makes certain micro-organisms (antibacterial, fungus, yeast, algae and virus
Deng) growth or breeding be maintained at the chemical substance of below certain level.Antibacterial be generally divided into silver, zinc, copper etc. be main
The mineral-type of raw material, the organic with esters, alcohols, phenols as primary raw material and with animal class, plant, mineral substance extract
Natural class for primary raw material.Wherein, inorganic antiseptic has good stability, has a broad antifungal spectrum, is not likely to produce the advantages such as drug resistance,
But it is subjected to query at anelasticity and the biological safety of body surface；Organic antibacterial agent thermostability is relatively poor, and the Yishui River
Solve, effect duration short；The biological safety of natural antibacterial agent is higher, but its antibacterial ability is relatively weak.
Chitosan, as a kind of antibacterial, has good biocompatibility, and has no side effect, but its anti-microbial property phase
To more weak, both can effectively eliminate the deficiency that chitosan anti-bacteria performance is not enough, it is also possible to aobvious by compounding with inorganic antiseptic
Write the biological safety improving composite.
Silver, as a kind of typical inorganic antiseptic raw material, has the advantages such as wide, the acting duration length of scope of restraining fungi, and
Silver ion is easily reduced agent, forms nanometer silver as the reproducibility hydroxyl on chitosan reduces, after being combined with chitosan, and can be uniform
Stable is distributed in chitosan gel rubber body, and the composite of formation can slowly discharge silver ion, it is possible to reaches the most antibacterial
Effect, and there is the features such as good antibacterial activity, avirulence.But, at present, uniform and stable it is distributed in chitosan for preparing
In nanometer silver, how exchanged by physical absorption, ion, external source adds the methods such as reducing agent and carries out, and the many needs of reaction system
Carrying out long-time heating process, preparation method is relative complex, easily affects the stability of chitosan solution, and needs to add boron hydrogen
Change the reducing agent that sodium or sodium citrate etc. are new, reduce biological safety and the system stability of composite.
Additionally, nano zine oxide is as a kind of antibacterial nano active oxidation material, it is possible to by light-catalyzed reaction, generation
Active oxygen and Nano-Zinc body is antibacterial etc. that multiple action mode plays antibacterial action, and there is low bio-toxicity, easily obtain
Etc. feature, but, the antibacterial activity of nano zine oxide is the highest.At present, nano zine oxide is combined with chitosan-nanometer silver
Not yet report.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of nano zine oxide-load silver chitosan is combined
Antibacterial.
Second object of the present invention is to provide the preparation side of a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent
Method.
Technical scheme is summarized as follows:
The preparation method of a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent, comprises the steps: in stirring at normal temperature
Under the conditions of, in proportion 0.1g chitosan is dissolved in acetic acid aqueous solution that 15-25mL volumetric concentration is 0.5%-1% or formic acid is water-soluble
In liquid, it is sequentially added into 0.5-2.5mL Polyethylene Glycol and 0.01-0.06g hydroxyethyl cellulose, stirs, add 0.5-2mL dense
Degree is the silver nitrate aqueous solution of 0.5-2M, stirs, and reacts 30-60s, be naturally cooling under 100-115 DEG C of microwave condition
Room temperature, adds 0.01-0.8g nano zine oxide, and it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide-load silver chitosan
Complex antimicrobials.
Preferably: the viscosity of chitosan is 20-300cps, deacetylation is more than 75%.
Preferably: Polyethylene Glycol is Polyethylene Glycol-200 or PEG-4000.
Nano zine oxide prepared by said method-load silver chitosan compound anti-bacteria agent.
The invention have the advantages that
1, utilize the reproducibility hydroxyl of chitosan body as silver ion reducing agent, be not re-introduced into new reducing agent, a step
Legal system must carry silver chitosan solution；
2, utilizing microwave synthesis method, be greatly shortened the response time, reaction system is prepared mostly under normal temperature condition, and obtains
The nanometer silver even particle size distribution obtained, reunion situation is substantially reduced；
3, chitosan is organically combined with nanometer silver, the compound nano zine oxide that adds, anti-microbial property excellence；
4, the composite antibacterial material biological safety of preparation is high；
5, preparation method of the present invention is simple, and production cost is relatively low.
Accompanying drawing explanation
Fig. 1 is the particle size distribution measuring result of nano zine oxide.
Fig. 2 is for carrying silver chitosan transmission electron microscope photo.
Fig. 3 is that nano zine oxide-load silver chitosan compound anti-bacteria agent is to escherichia coli antibacterial effect.
Fig. 4 is that nano zine oxide-load silver chitosan compound anti-bacteria agent is to staphylococcus aureus antibacterial effect.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.Based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise
Embodiment, broadly falls into protection scope of the present invention.
Chitosan used by each embodiment be viscosity be 20-300cps, deacetylation be more than 75%.
Embodiment 1
The preparation of nano zine oxide:
Prepare 0.2M zinc acetate solution with methanol for solvent, take 50mL zinc acetate solution, add the NaOH aqueous solution of 0.8M,
Adjusting pH value is 8.7；Zinc acetate solution after adjusting pH is transferred to, in polyfluortetraethylene pipe, seal, and being placed in cavity is
150 DEG C catch up with 6h in acid device, stand after 12h, after confirming that polyfluortetraethylene pipe is down to room temperature, open upper cover, add proper amount of methanol
Rinse, then flushing liquor is transferred in glass, be dried to pulverulence in being placed in 60 DEG C of aeration cabinets, nanometer can be obtained
Zinc oxide particles.
The pH value substituting the present embodiment with pH=10.6 is 8.7, other same the present embodiment；
PH can also select 8,9,11；
Fig. 1 is the particle size distribution measuring result of the nano zine oxide of preparation；
Fig. 1 a be pH terminal be the nano granular of zinc oxide particle size determination result of 8.7, particle diameter is 8.900nm；
Fig. 1 b be pH terminal be the nano granular of zinc oxide particle size determination result of 10.6, particle diameter is 3.681nm.Show preparation
Nano granular of zinc oxide meet the requirements, and in preparation process, the particle diameter of nano granular of zinc oxide product is had an impact by pH terminal,
PH is the biggest, and nano particle diameter is the least.
Embodiment 2
The preparation method of a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent, comprises the steps:
Under the conditions of stirring at normal temperature, 0.1g chitosan is dissolved in the acetic acid aqueous solution that 20mL volumetric concentration is 1%, successively
Add 1mL PEG-4000 and 0.03g hydroxyethyl cellulose, stir, add the silver nitrate that 0.5mL concentration is 1M water-soluble
Liquid (existing now join), stirs, and reacts 30s, be naturally cooling to room temperature under 115 DEG C of microwave conditions, must carry silver-colored chitosan；
Adding 0.05g nano zine oxide, it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide-load silver chitosan
Complex antimicrobials.
Embodiment 3
The preparation method of a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent, comprises the steps:
Under the conditions of stirring at normal temperature, 0.1g chitosan is dissolved in the acetic acid aqueous solution that 20mL volumetric concentration is 1%, successively
Add 0.5mL PEG-4000 and 0.01g hydroxyethyl cellulose, stir, add the silver nitrate water that 0.5mL concentration is 2M
Solution (existing now join), stirs, and reacts 60s, be naturally cooling to room temperature under 100 DEG C of microwave conditions, must carry silver-colored chitosan；
Adding 0.01g nano zine oxide, it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide-load silver chitosan
Complex antimicrobials.
Embodiment 4
The preparation method of a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent, comprises the steps:
Under the conditions of stirring at normal temperature, 0.1g chitosan is dissolved in the acetic acid aqueous solution that 15mL volumetric concentration is 1%, successively
Add 2.5mL PEG-4000 and 0.06g hydroxyethyl cellulose, stir, add the silver nitrate that 1mL concentration is 1M water-soluble
Liquid (existing now join), stirs, and reacts 45s, be naturally cooling to room temperature under 110 DEG C of microwave conditions, must carry silver-colored chitosan；
Adding 0.01g nano zine oxide, it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide-load silver chitosan
Complex antimicrobials.
Embodiment 5
The preparation method of a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent, comprises the steps:
Under the conditions of stirring at normal temperature, 0.1g chitosan is dissolved in the aqueous formic acid that 25mL volumetric concentration is 0.5%, depends on
Secondary addition 1mL Polyethylene Glycol-200 and 0.03g hydroxyethyl cellulose, stir, and adds the silver nitrate water that 2mL concentration is 0.5M
Solution (existing now join), stirs, and reacts 30s, be naturally cooling to room temperature under 100 DEG C of microwave conditions, must carry silver-colored chitosan；
Adding 0.8g nano zine oxide, it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide-load silver chitosan is multiple
Close antibacterial.
The preferred 150W of microwave synthesizer used by each embodiment microwave.
Prepared by each embodiment carries structural characterization and the nano zine oxide-load silver chitosan compound anti-bacteria agent of silver chitosan
Anti-microbial property result as follows:
2. carry silver chitosan transmission electron microscope results
Fig. 2 a is the load silver chitosan transmission electron microscope picture of embodiment 2 preparation, and visible nano-Ag particles in figure, particle diameter is about 3-
10nm；
Fig. 2 b is the load silver chitosan transmission electron microscope picture of embodiment 3 preparation, and visible nano-Ag particles in figure, particle diameter is about
15-21nm。
Under the conditions of two kinds, the nano-Ag particles particle diameter of preparation is less, and particle diameter is relatively uniform, and distribution of particles ratio is more uniform, without bright
Aobvious agglomeration.
3. carry silver chitosan and nano zine oxide-load silver chitosan compound anti-bacteria agent anti-escherichia coli effectiveness comparison, see figure
3, result display nano zine oxide-load silver its antibacterial activity of chitosan compound anti-bacteria agent and antibacterial ability are higher than carrying silver chitosan.
Carry silver chitosan and nano zine oxide-load silver chitosan compound anti-bacteria agent anti-Staphylococcus aureus effectiveness comparison,
See that Fig. 4, result display nano zine oxide-load silver its antibacterial activity of chitosan compound anti-bacteria agent and antibacterial ability gather higher than carrying silver shell
Sugar.
Claims (4)
1. a preparation method for nano zine oxide-load silver chitosan compound anti-bacteria agent, is characterized in that comprising the steps: often
Under temperature stirring condition, in proportion 0.1g chitosan is dissolved in acetic acid aqueous solution or the first that 15-25mL volumetric concentration is 0.5%-1%
In aqueous acid, it is sequentially added into 0.5-2.5mL Polyethylene Glycol and 0.01-0.06g hydroxyethyl cellulose, stirs, add
0.5-2mL concentration is the silver nitrate aqueous solution of 0.5-2M, stirs, and reacts 30-60s under 100-115 DEG C of microwave condition, from
So being cooled to room temperature, add 0.01-0.8g nano zine oxide, it is transparent that room temperature continues stirring until system, it is thus achieved that nano zine oxide-load
Silver chitosan compound anti-bacteria agent.
Method the most according to claim 1, is characterized in that the viscosity of described chitosan is 20-300cps, and deacetylation is big
In 75%.
Method the most according to claim 1, it is characterized in that described Polyethylene Glycol be Polyethylene Glycol-200 or Polyethylene Glycol-
400。
4. the nano zine oxide that prepared by the method for one of claim 1-3-load silver chitosan compound anti-bacteria agent.
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| CN106978721A (en) * | 2017-03-22 | 2017-07-25 | 广西科技大学 | A kind of preparation method of long-acting antibiotic textile |
| CN106977990A (en) * | 2017-04-06 | 2017-07-25 | 长沙理工大学 | A kind of antibacterial modification nano zine oxide/fluoropolymer ultraviolet-curing paint and preparation method thereof |
| CN107258774A (en) * | 2017-06-23 | 2017-10-20 | 华南农业大学 | A kind of antibacterial material with slow-releasing and controlled-releasing action and preparation method and application |
| CN107970133A (en) * | 2017-11-28 | 2018-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Antiseptic toothpaste preparation method and products thereof and application |
| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
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| CN106978721A (en) * | 2017-03-22 | 2017-07-25 | 广西科技大学 | A kind of preparation method of long-acting antibiotic textile |
| CN106857658A (en) * | 2017-03-30 | 2017-06-20 | 安徽省银锂子生物科技发展有限公司 | It is a kind of carry with, the Nano Silver table-ware disinfection liquid of efficient quick sterilization |
| CN106977990A (en) * | 2017-04-06 | 2017-07-25 | 长沙理工大学 | A kind of antibacterial modification nano zine oxide/fluoropolymer ultraviolet-curing paint and preparation method thereof |
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| CN107970133A (en) * | 2017-11-28 | 2018-05-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Antiseptic toothpaste preparation method and products thereof and application |
| CN109169706A (en) * | 2018-07-19 | 2019-01-11 | 大美泰康（天津）生态科技有限公司 | Complex antimicrobials and antibacterial bacteriostatic type multifunctional inorganic ecologic coating obtained |
| CN110038528A (en) * | 2019-04-25 | 2019-07-23 | 广西科技大学 | A kind of preparation method of Cellulose/Chitosan composite antibacterial adsorbent |
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| CN112538666A (en) * | 2020-12-23 | 2021-03-23 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Reusable nano-fiber film for antibacterial biological protective mask and manufacturing method thereof |
| CN114456396A (en) * | 2022-01-28 | 2022-05-10 | 广东粤港澳大湾区国家纳米科技创新研究院 | Polymer modified zinc oxide and preparation method and application thereof |
| CN114456396B (en) * | 2022-01-28 | 2023-09-19 | 广东粤港澳大湾区国家纳米科技创新研究院 | Polymer modified zinc oxide and preparation method and application thereof |
| CN114575042A (en) * | 2022-03-01 | 2022-06-03 | 浙江盛纺纳米材料科技有限公司 | Antibacterial non-woven fabric and preparation method thereof |
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| CN115672702B (en) * | 2022-10-26 | 2023-11-10 | 青岛美中建材机械有限公司 | Decorative board and processing technology thereof |
| CN116199800A (en) * | 2023-02-08 | 2023-06-02 | 中国林业科学研究院林产化学工业研究所 | Preparation method of chitosan-citral-calcium salt compound with vibrio resistance activity |
| CN116199800B (en) * | 2023-02-08 | 2024-02-27 | 中国林业科学研究院林产化学工业研究所 | Preparation method of chitosan-citral-calcium salt compound with vibrio resistance activity |
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