CN106106522B - A kind of nano zine oxide-load silver chitosan compound anti-bacteria agent and preparation method thereof - Google Patents
A kind of nano zine oxide-load silver chitosan compound anti-bacteria agent and preparation method thereof Download PDFInfo
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- CN106106522B CN106106522B CN201610482787.9A CN201610482787A CN106106522B CN 106106522 B CN106106522 B CN 106106522B CN 201610482787 A CN201610482787 A CN 201610482787A CN 106106522 B CN106106522 B CN 106106522B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- 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-load silver chitosan compound anti-bacteria agents and preparation method thereof, the preparation method comprises the following steps: under the conditions of stirring at normal temperature, chitosan is dissolved in acetic acid aqueous solution or aqueous formic acid, sequentially add polyethylene glycol and hydroxyethyl cellulose, it stirs evenly, silver nitrate aqueous solution is added, it stirs evenly, it is reacted under 100-115 DEG C of microwave condition, it is naturally cooling to room temperature, nano zine oxide is added, it is transparent that room temperature continues stirring until system, obtains nano zine oxide-load silver chitosan compound anti-bacteria agent.Using the reproducibility hydroxyl of chitosan ontology as silver ion reducing agent, it is not re-introduced into new reducing agent, one-step method, which is made, carries silver-colored chitosan solution；It is synthesized using microwave, greatly shortens the reaction time, reaction system is prepared under normal temperature conditions mostly, and the nano silver particle diameter distribution obtained is uniform, and reunion situation substantially reduces；Anti-microbial property is excellent；Biological safety is high；Method is simple, lower production costs.
Description
Technical field
The present invention relates to a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent and preparation method thereof, belong to it is inorganic-have
The preparation of machine hydridization anti-biotic material and its applied technical field.
Background technique
Antibacterial agent is to refer within a certain period of time, make certain micro-organisms (bacterium, fungi, saccharomycete, algae and virus
Deng) growth or breeding be maintained at certain level chemical substance below.It is main that antibacterial agent, which is generally divided into silver, zinc, copper etc.,
The inorganic of raw material, using esters, alcohols, phenols as the organic of primary raw material and with animal class, plant, mineral substance extract
For the natural class of primary raw material.Wherein, inorganic antiseptic has many advantages, such as that stability is good, has a broad antifungal spectrum, is not likely to produce drug resistance,
But it is subjected to query in the anelasticity and biological safety of body surface；Organic antibacterial agent heat resistance is relatively poor, and the Yishui River
Solution, validity period are short；The biological safety of natural antibacterial agent is higher, but its antibacterial ability is relatively weak.
Chitosan has good biocompatibility as a kind of antibacterial agent, and has no toxic side effect, but its anti-microbial property phase
To weaker, it can both can effectively eliminate the insufficient deficiency of chitosan anti-bacteria performance by being compounded with inorganic antiseptic, can also show
Write the biological safety for improving composite material.
Silver is used as a kind of typical inorganic antiseptic raw material, has many advantages, such as that scope of restraining fungi is wide, acting duration is long, and
Silver ion is easy to be reduced agent, if the reproducibility hydroxyl on chitosan restores to form nano silver, with chitosan it is compound after, can be uniform
Stable is distributed in chitosan gel rubber body, the composite material of formation can slow release silver ion, can reach permanent antibacterial
Effect, and have the characteristics that good antibacterial activity, nontoxicity.But currently, uniform and stable chitosan is distributed in prepare
In nano silver, multi-pass crosses physical absorption, ion exchange, external source are added the methods of reducing agent and carry out, and reaction system needs more
Long-time heating processing is carried out, preparation method is relative complex, is easy to influence the stability of chitosan solution, and need to be added boron hydrogen
Change the new reducing agent such as sodium or sodium citrate, reduces the biological safety and system stability of composite material.
In addition, nano zine oxide can pass through light-catalyzed reaction, generation as a kind of antibacterial nano active oxidation material
The multiple actions mode such as active oxygen and Nano-Zinc ontology antibacterial plays antibacterial action, and has low bio-toxicity, easily obtains
The features such as, still, the antibacterial activity of nano zine oxide is not high.Currently, nano zine oxide and chitosan-nano silver progress is compound
It has not been reported.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of nano zine oxide-load silver chitosan is compound
Antibacterial agent.
A second object of the present invention is to provide a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent preparation sides
Method.
Technical solution of the present invention is summarized as follows:
A kind of preparation method of nano zine oxide-load silver chitosan compound anti-bacteria agent, includes the following steps: in stirring at normal temperature
Under the conditions of, it is water-soluble for the acetic acid aqueous solution or formic acid of 0.5%-1% that 0.1g chitosan is dissolved in 15-25mL volumetric concentration in proportion
In liquid, 0.5-2.5mL polyethylene glycol and 0.01-0.06g hydroxyethyl cellulose are sequentially added, is stirred evenly, it is dense that 0.5-2mL is added
Degree is the silver nitrate aqueous solution of 0.5-2M, stirs evenly, reacts 30-60s under 100-115 DEG C of microwave condition, be naturally cooling to
0.01-0.8g nano zine oxide is added in room temperature, and it is transparent that room temperature continues stirring until system, obtains nano zine oxide-load silver chitosan
Complex antimicrobials.
Preferably: the viscosity of chitosan is 20-300cps, and deacetylation is greater than 75%.
Preferably: polyethylene glycol is polyethylene glycol -200 or polyethylene glycol-400.
Nano zine oxide-load silver chitosan compound anti-bacteria agent of above method preparation.
The invention has the following advantages that
1, using the reproducibility hydroxyl of chitosan ontology as silver ion reducing agent, new reducing agent, a step are not re-introduced into
Legal system must carry silver-colored chitosan solution；
2, using microwave synthesis method, the reaction time is greatly shortened, reaction system is prepared under normal temperature conditions mostly, and is obtained
The nano silver particle diameter distribution obtained is uniform, and reunion situation substantially reduces；
3, chitosan and nano silver are organically combined, compound addition nano zine oxide, anti-microbial property is excellent；
4, the composite antibacterial material biological safety prepared is high；
5, preparation method of the present invention is simple, lower production costs.
Detailed description of the invention
Fig. 1 is the particle size distribution measuring result of nano zine oxide.
Fig. 2 is to carry silver-colored chitosan transmission electron microscope photo.
Fig. 3 is nano zine oxide-load silver chitosan compound anti-bacteria agent to Escherichia coli antibacterial effect.
Fig. 4 is nano zine oxide-load silver chitosan compound anti-bacteria agent to staphylococcus aureus antibacterial effect.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, and but the scope of the present invention is not limited thereto.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment belongs to protection scope of the present invention.
Chitosan used in each embodiment is that viscosity is 20-300cps, and deacetylation is greater than 75%.
Embodiment 1
The preparation of nano zine oxide:
0.2M zinc acetate solution is prepared by solvent of methanol, 50mL zinc acetate solution is taken, the NaOH aqueous solution of 0.8M is added,
Adjusting pH value is 8.7；Zinc acetate solution after adjustment pH is transferred in polyfluortetraethylene pipe, is sealed, being placed in cavity is
150 DEG C are caught up with 6h in sour device, and after standing 12h, confirmation polyfluortetraethylene pipe is cooled to room temperature, and opens upper cover, proper amount of methanol is added
It rinses, then flushing liquor is transferred in glass, be placed in 60 DEG C of aeration cabinets and dry to pulverulence, can be obtained nanometer
Zinc oxide particles.
It is 8.7 with the pH value that pH=10.6 substitutes the present embodiment, 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 8.7 nano granular of zinc oxide particle size determination as a result, partial size is 8.900nm；
Fig. 1 b be pH terminal be 10.6 nano granular of zinc oxide particle size determination as a result, partial size is 3.681nm.Show to prepare
Nano granular of zinc oxide meet the requirements, and pH terminal has an impact to the partial size of nano granular of zinc oxide product in preparation process,
PH is bigger, and nano particle diameter is smaller.
Embodiment 2
A kind of preparation method of nano zine oxide-load silver chitosan compound anti-bacteria agent, includes the following 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
1mL polyethylene glycol-400 and 0.03g hydroxyethyl cellulose is added, stirs evenly, it is water-soluble that the silver nitrate that 0.5mL concentration is 1M is added
Liquid (existing now to match), stirs evenly, and reacts 30s under 115 DEG C of microwave conditions, is naturally cooling to room temperature, must carry silver-colored chitosan；
0.05g nano zine oxide is added, it is transparent that room temperature continues stirring until system, obtains nano zine oxide-load silver chitosan
Complex antimicrobials.
Embodiment 3
A kind of preparation method of nano zine oxide-load silver chitosan compound anti-bacteria agent, includes the following 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
0.5mL polyethylene glycol-400 and 0.01g hydroxyethyl cellulose is added, stirs evenly, the silver nitrate water that 0.5mL concentration is 2M is added
Solution (existing now to match), stirs evenly, and reacts 60s under 100 DEG C of microwave conditions, is naturally cooling to room temperature, must carry silver-colored chitosan；
0.01g nano zine oxide is added, it is transparent that room temperature continues stirring until system, obtains nano zine oxide-load silver chitosan
Complex antimicrobials.
Embodiment 4
A kind of preparation method of nano zine oxide-load silver chitosan compound anti-bacteria agent, includes the following 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
2.5mL polyethylene glycol-400 and 0.06g hydroxyethyl cellulose is added, stirs evenly, it is water-soluble that the silver nitrate that 1mL concentration is 1M is added
Liquid (existing now to match), stirs evenly, and reacts 45s under 110 DEG C of microwave conditions, is naturally cooling to room temperature, must carry silver-colored chitosan；
0.01g nano zine oxide is added, it is transparent that room temperature continues stirring until system, obtains nano zine oxide-load silver chitosan
Complex antimicrobials.
Embodiment 5
A kind of preparation method of nano zine oxide-load silver chitosan compound anti-bacteria agent, includes the following 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%, according to
Secondary addition 1mL polyethylene glycol -200 and 0.03g hydroxyethyl cellulose, stir evenly, and the silver nitrate water that 2mL concentration is 0.5M is added
Solution (existing now to match), stirs evenly, and reacts 30s under 100 DEG C of microwave conditions, is naturally cooling to room temperature, must carry silver-colored chitosan；
0.8g nano zine oxide is added, it is transparent that room temperature continues stirring until system, and it is multiple to obtain nano zine oxide-load silver chitosan
Close antibacterial agent.
The preferred 150W of microwave synthesizer used in each embodiment microwave.
The structural characterization and nano zine oxide-load silver chitosan compound anti-bacteria agent of the silver-colored chitosan of load of each embodiment preparation
Anti-microbial property result it is as follows:
2. carrying silver-colored chitosan transmission electron microscope results
Fig. 2 a is load silver chitosan transmission electron microscope picture prepared by embodiment 2, and visible nano-Ag particles in figure, partial size is about 3-
10nm；
Fig. 2 b is load silver chitosan transmission electron microscope picture prepared by embodiment 3, visible nano-Ag particles in figure, and partial size is about
15-21nm。
The nano-Ag particles partial size prepared under the conditions of two kinds is smaller, and partial size is relatively uniform, and distribution of particles is relatively uniform, without bright
Aobvious agglomeration.
3. carrying silver-colored chitosan compared with the anti-Escherichia coli effect of nano zine oxide-load silver chitosan compound anti-bacteria agent, figure is seen
3, nano zine oxide-its antibacterial activity of load silver chitosan compound anti-bacteria agent and antibacterial ability, which are higher than, as the result is shown carries silver-colored chitosan.
Silver-colored chitosan is carried compared with nano zine oxide-load silver chitosan compound anti-bacteria agent anti-Staphylococcus aureus effect,
See Fig. 4, it is poly- to be higher than the silver-colored shell of load for nano zine oxide-its antibacterial activity of load silver chitosan compound anti-bacteria agent and antibacterial ability as the result is shown
Sugar.
Claims (4)
1. a kind of nano zine oxide-load silver chitosan compound anti-bacteria agent preparation method, it is characterized in that including the following steps: normal
Under warm stirring condition, 0.1g chitosan is dissolved in the acetic acid aqueous solution or first that 15-25mL volumetric concentration is 0.5%-1% in proportion
In aqueous acid, 0.5-2.5mL polyethylene glycol and 0.01-0.06g hydroxyethyl cellulose are sequentially added, is stirred evenly, is added
0.5-2mL concentration is the silver nitrate aqueous solution of 0.5-2M, stirs evenly, reacts 30-60s under 100-115 DEG C of microwave condition, from
It is so cooled to room temperature, is added 0.01-0.8g nano zine oxide, it is transparent that room temperature continues stirring until system, obtains nano zine oxide-load
Silver-colored chitosan compound anti-bacteria agent.
2. according to the method described in claim 1, deacetylation is big it is characterized in that the viscosity of the chitosan is 20-300cps
In 75%.
3. according to the method described in claim 1, it is characterized in that the polyethylene glycol is polyethylene glycol -200 or polyethylene glycol -
400。
4. nano zine oxide prepared by the method for one of claim 1-3-load silver chitosan compound anti-bacteria agent.
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