CN106342887A - Chitosan packed nano-silver and graphene oxide composite antibacterial material - Google Patents
Chitosan packed nano-silver and graphene oxide composite antibacterial material Download PDFInfo
- Publication number
- CN106342887A CN106342887A CN201610736602.2A CN201610736602A CN106342887A CN 106342887 A CN106342887 A CN 106342887A CN 201610736602 A CN201610736602 A CN 201610736602A CN 106342887 A CN106342887 A CN 106342887A
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- CN
- China
- Prior art keywords
- graphene oxide
- carboxymethyl chitosan
- nanometer silver
- composite antibacterial
- antibacterial material
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—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
-
- 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
-
- 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
Abstract
A chitosan packed nano-silver and graphene oxide composite antibacterial material is formed by mixing O-carboxymethyl chitosan packed nano-silvers with graphene oxide, wherein each O-carboxymethyl chitosan packed nano-silver consists of a nano-silver core and an O-carboxymethyl chitosan shell adsorbed on the surface of the nano-silver core; and the O-carboxymethyl chitosan packed nano-silvers are uniformly loaded on the surface of the graphene oxide. The antibacterial effect is optimized by changing the ratio of the various O-carboxymethyl chitosan packed nano-silvers to the graphene oxide, the minimal inhibitory concentration to colibacillus is 0.25 mu/mL, the minimal inhibitory concentration to staphylococcus aureus is 1 mu/mL, and the minimal inhibitory concentrations reach the minimum concentration limit of existing domestic and overseas like optimal products, used materials are harmless to human bodies, and the chitosan packed nano-silver and graphene oxide composite antibacterial material is low in price and is an environmentally friendly novel composite antibacterial agent.
Description
Technical field
The present invention relates to a kind of graphene oxide-nano silver composite antibacterial agent, especially a kind of antibacterial modified for material
The o- carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material of blending.
Background technology
, in daily life accidentally often in contact with various antibacterials and virus, these microorganisms are in suitable humidity for people
Can breed rapidly with the growing environments such as temperature, and pass through contact transmission disease, impact people are physically and mentally healthy.Therefore research side
Just practical, easily realize the long-acting low toxicity antibacterial of antibiotic and sterilizing function, the living and working environment creating health has weight
The meaning wanted.
Nanometer silver is the nano material of a class most prospect, has the bactericidal property being significantly better than silver iron compound, but
The characteristic that nanometer silver is easily reunited makes its range of application be very limited, and typically need to add a large amount of protective agents in preparation process.
For example, " one kind complexation nanometer silver aggressiveness liquid antibacterial agent and its preparation side twice of Publication No. cn103371182
The patent of invention of method ", this patent with nanometer argentiferous double salt, with polyvinyl alcohol, as dispersion, protect, surely by Polyvinylpyrrolidone
Determine film former, with hypo as complexation and reducing agent, be prepared for the nanometer silver fine particle that particle diameter is 3-5 nanometer.But nanometer
Silver protecting agent does not typically have antibiotic property, and protectant addition in a large number limits the performance of nanometer silver antimicrobial performance.
Graphene is by the tightly packed bi-dimensional cellular shape lattice structure becoming of monolayer carbon atom, the Graphene tool after oxidation
There is quasi- two-dimensional structure, a large amount of oxy radicals that its surface exists, the combination for other granules provides effective site.Work as nanometer silver
Granule and graphene oxide compound tense, these sites and this absorption can effectively stop nano-Ag particles from being reunited.Therefore, with oxygen
Graphite alkene is prepared antimicrobial composite material for matrix load silver nanoparticle Argent grain and is always study hotspot.Simultaneous oxidation Graphene with
There is synergistic antibacterial in nanometer silver, antibacterial effect is better than with concentration graphene oxide or nanometer silver.
For example, publication No. is that cn104068058a is disclosed " a kind of preparation method of graphene oxide antibacterial composite material "
With glucose as reducing agent, starch is prepared for graphene oxide antibacterial composite material for stabilizer using a stage reduction method, its work
Skill is simple, easy to operate, and reaction condition is gentle, and production efficiency is high, green, environmental friendliness；The graphene oxide of preparation is antibacterial multiple
In condensation material, nano-Ag particles equably adsorb on graphene oxide, are effectively improved the bacteriostasis property of graphene oxide,
But this invention cannot illustrate that graphene oxide whether there is Synergistic antimicrobial effect with nanometer silver.
Content of the invention
The present invention is intended to provide a kind of graphene oxide of low toxicity, safe and stable property and good dispersion-nanometer silver antimicrobial material
Material, and inquire into the ratio between o- carboxymethyl chitosan and graphene oxide and Synergistic antimicrobial effect.
Above-mentioned purpose is achieved through the following technical solutions.
A kind of shitosan parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described composite antibacterial material
Material is to be made up of o- carboxymethyl chitosan parcel nanometer silver and graphene oxide blending, and described o- carboxymethyl chitosan wraps up nanometer
Silver is that the o- carboxymethyl chitosan shell on nanometer galactic nucleus surface is constituted by nanometer galactic nucleus and its absorption, o- carboxymethyl chitosan bag
Wrap up in nanometer silver uniform load in surface of graphene oxide, o- carboxymethyl chitosan parcel nanometer silver is with graphene oxide in mass ratio
For 1:5-5:1.
Wherein, described o- carboxymethyl chitosan parcel nanometer silver is by silver nitrate and o- carboxymethyl chitosan mixed solution warp
Prepared by ultraviolet light；Described o- carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material is by o- carboxymethyl shell
Polysaccharide parcel nanometer silver and graphene oxide are prepared by self-assembly method in aqueous；Described o- carboxymethyl chitosan molecular weight
For 30000- 2000000；The a diameter of 0.7-1.2 nm micron of described graphene oxide, monolayer rate is more than 95%；Described o- carboxylic first
Base enclosure polysaccharide parcel nanometer silver particle diameter is 2-20nm；Described o- carboxymethyl chitosan wraps up nanometer silver graphene oxide composite antibacterial
Material preservation state is the powder after aqueous solution or lyophilization.
A kind of above-mentioned shitosan wraps up nanometer silver graphene oxide composite antibacterial material, with respect to the master of traditional anti-biotic material
Want feature and be advantageous in that:
The special quasi- two-dimensional structure of graphene oxide can effectively prevent nanometer silver from reuniting, a large amount of presence of surface of graphene oxide
Reproducibility hydroxyl can effectively slow down the oxidation of silver-colored simple substance, and simultaneous oxidation Graphene and nanometer silver have synergistic antibacterial, antibacterial effect
Better than with concentration graphene oxide or nanometer silver, through micro meat soup method testing inspection: o- carboxymethyl chitosan parcel nanometer silver oxygen
Graphite alkene composite antibacterial material is 0.25/ml to colibacillary minimal inhibitory concentration, the minimum to gold-coloured staphylococci
Mlc is 1/ml, has reached the least concentration limit that similar best product can reach both at home and abroad at present.
Brief description
Fig. 1 is the shitosan parcel antibacterial reality of the micro broth dilution method of nanometer silver graphene oxide composite antibacterial material of the present invention
Test result, test strain is escherichia coli.
Fig. 2 is the shitosan parcel antibacterial reality of the micro broth dilution method of nanometer silver graphene oxide composite antibacterial material of the present invention
Test result, test strain is gold-coloured staphylococci.
Specific embodiment
To further describe the specific embodiment of the present invention below by specific embodiment.
Comparative example 1
Contrast experiment's example 1 is not carry out the o- carboxymethyl chitosan parcel nanometer silver of self assembly, its preparation side with graphene oxide
Method is as follows:
0.1%wt silver nitrate solution is added agitator, room for 5:95 by volume with 0.1%wt o- carboxymethyl chitosan solution
It is placed in 4ml quartz colorimetric utensil after temperature lower stirring 0.5h, logical nitrogen 20s eliminates air and seals.Quartz colorimetric utensil is placed in
Exposing to solution at 272nm uviol lamp 5cm is in golden yellow.
Above-mentioned solution high speed centrifugation is taken precipitation, and obtains o- carboxymethyl chitosan parcel twice with 50%wt washing with alcohol
Nanometer silver.Precipitation is dispersed again in ultra-pure water, and ultrasonic 10min, obtains final product o- carboxymethyl chitosan parcel nanometer silver antimicrobial material
Material.
Micro broth dilution method minimal inhibitory concentration test:
The strain of escherichia coli (atcc11229) and staphylococcus aureuses (atcc6538) is inoculated into method of scoring respectively and joins
On the Nutrient agar put, be placed in constant incubator lower culture after, take typical bacterium colony subcultivation to nutrient broth medium
In, cultivate again, with nutrient broth, bacteria suspension is diluted, be configured to 105Cfu/ml bacterial suspension is standby.
Choose eight holes side by side in 96 hole polystyrene plates of sterilizing, every hole sequentially adds the sterilizing mh of double concentration
(b) complete medium 100 μ l, 105The o- carboxymethyl chitosan of variable concentrations after cfu/ml bacterial suspension 50 μ l and doubling dilution
Parcel nano silver antibacterial material 50 μ l.Now the 1st hole to the 8th hole drug level be respectively 16,8,4,2,1,0.5,0.25,
0.125μg/ml.96 hole polystyrene plates are placed in 37oCulture 24h in incubator, detects the od in each hole at 630nm with microplate reader
Value.
Result of the test is shown in accompanying drawing 1, accompanying drawing 2, o- carboxymethyl chitosan parcel nano silver antibacterial material to colibacillary
Little Mlc is 1/ml, and the minimal inhibitory concentration to gold-coloured staphylococci is 2/ml.
Embodiment 1
Implement the technical scheme that a kind of o- carboxymethyl chitosan wraps up nanometer silver graphene oxide composite antibacterial material, its described o-
Carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material is wrapped up with o- carboxymethyl chitosan by graphene oxide
Nanometer silver self assembly preparation in aqueous.Its described o- carboxymethyl chitosan parcel nanometer silver preparation method is with contrast experiment's example
1.Subsequently o- carboxymethyl chitosan parcel nanometer silver is dissolved in ultra-pure water for 5:1 in mass ratio with graphene oxide, supersound process
10min, obtains o- carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material.
With respect to comparative example 1, embodiment 1 adds graphene oxide can effectively prevent nanometer silver from reuniting, and dispersibility is more
Good.
Micro broth dilution method minimal inhibitory concentration is tested with comparative example 1.
Result of the test is shown in accompanying drawing 1, accompanying drawing 2, and the present embodiment o- carboxymethyl chitosan parcel nanometer silver graphene oxide is combined
Anti-biotic material is 1/ml to colibacillary minimal inhibitory concentration, be 2 to the minimal inhibitory concentration of gold-coloured staphylococci/
Ml, fungistatic effect is identical with comparative example 1.
Embodiment 2
According to the process preparation of embodiment 1, the difference of embodiment 2 is: o- carboxymethyl chitosan parcel nanometer silver and oxygen
Graphite alkene is 3:3 in mass ratio.
With respect to embodiment 1, embodiment 3 graphene oxide accounting improves, and dispersibility is more preferable.
Micro broth dilution method minimal inhibitory concentration is tested with comparative example 1.
Result of the test is shown in accompanying drawing 1, accompanying drawing 2, and the present embodiment o- carboxymethyl chitosan parcel nanometer silver graphene oxide is combined
Anti-biotic material is 4/ml to colibacillary minimal inhibitory concentration, be 4 to the minimal inhibitory concentration of gold-coloured staphylococci/
Ml, fungistatic effect is unsuitable excessive not as good as embodiment 1, comparative example 1, therefore graphene oxide accounting.
Embodiment 3
According to the process preparation of embodiment 1, the difference of embodiment 2 is: o- carboxymethyl chitosan parcel nanometer silver and oxygen
Graphite alkene is 2:4 in mass ratio.
The present embodiment o- carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material dispersibility is between enforcement
Between example 1 and embodiment 2.
Micro broth dilution method minimal inhibitory concentration is tested with comparative example 1.
Result of the test is shown in accompanying drawing 1, accompanying drawing 2, and o- carboxymethyl chitosan wraps up nanometer silver graphene oxide composite antibacterial material
It is 0.25/ml to colibacillary minimal inhibitory concentration, the minimal inhibitory concentration to gold-coloured staphylococci is 1/ml, antibacterial
Effect is better than embodiment 1, comparative example 1, o- carboxymethyl chitosan parcel nanometer silver is described with graphene oxide in mass ratio
There is significant Synergistic antimicrobial effect both during 2:4.
Claims (7)
1. a kind of shitosan parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described composite antibacterial material
It is to be made up of o- carboxymethyl chitosan parcel nanometer silver and graphene oxide blending, described o- carboxymethyl chitosan wraps up nanometer silver
It is that the o- carboxymethyl chitosan shell on nanometer galactic nucleus surface is constituted by nanometer galactic nucleus and its absorption, o- carboxymethyl chitosan wraps up
In surface of graphene oxide, o- carboxymethyl chitosan wraps up nanometer silver and with graphene oxide is in mass ratio nanometer silver uniform load
1:5-5:1.
2. shitosan as claimed in claim 1 parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described
O- carboxymethyl chitosan parcel nanometer silver is to be prepared through ultraviolet light with o- carboxymethyl chitosan mixed solution by silver nitrate.
3. shitosan as claimed in claim 1 parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described
O- carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material be by o- carboxymethyl chitosan wrap up nanometer silver and
Graphene oxide is prepared by self assembly in aqueous.
4. shitosan as claimed in claim 1 parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described
The molecular weight of o- carboxymethyl chitosan is 30000- 2000000.
5. shitosan as claimed in claim 1 parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described
The diameter of graphene oxide is 0.7-1.2 nm micron, and monolayer rate is more than 95%.
6. shitosan as claimed in claim 1 parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described
O- carboxymethyl chitosan parcel nanometer silver particle diameter is 2-20nm.
7. shitosan as claimed in claim 1 parcel nanometer silver graphene oxide composite antibacterial material it is characterised in that: described
After o- carboxymethyl chitosan parcel nanometer silver graphene oxide composite antibacterial material preservation state is aqueous solution or lyophilization
Powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610736602.2A CN106342887A (en) | 2016-08-29 | 2016-08-29 | Chitosan packed nano-silver and graphene oxide composite antibacterial material |
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| CN201610736602.2A CN106342887A (en) | 2016-08-29 | 2016-08-29 | Chitosan packed nano-silver and graphene oxide composite antibacterial material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108977151A (en) * | 2018-08-11 | 2018-12-11 | 安徽华祺汽车装饰有限公司 | A kind of preferable automobile interior decoration adhesive of antibacterial effect and preparation method thereof |
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| CN102224819A (en) * | 2011-04-02 | 2011-10-26 | 中国科学院海洋研究所 | Nano silver loaded graphene oxide composite bactericide, and its preparation and application |
| CN103191464A (en) * | 2013-04-07 | 2013-07-10 | 西南交通大学 | Method for preparing antibacterial porous oxidized graphene/chitosan composite bracket |
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Patent Citations (4)
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| CN101223887A (en) * | 2008-01-31 | 2008-07-23 | 吴继贤 | Nano silver antimicrobial solution and preparing method thereof |
| CN102224819A (en) * | 2011-04-02 | 2011-10-26 | 中国科学院海洋研究所 | Nano silver loaded graphene oxide composite bactericide, and its preparation and application |
| CN103191464A (en) * | 2013-04-07 | 2013-07-10 | 西南交通大学 | Method for preparing antibacterial porous oxidized graphene/chitosan composite bracket |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108977151A (en) * | 2018-08-11 | 2018-12-11 | 安徽华祺汽车装饰有限公司 | A kind of preferable automobile interior decoration adhesive of antibacterial effect and preparation method thereof |
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