CN104126611A - Preparation method of nano-silver composite antibacterial agent - Google Patents
Preparation method of nano-silver composite antibacterial agent Download PDFInfo
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- CN104126611A CN104126611A CN201410355274.2A CN201410355274A CN104126611A CN 104126611 A CN104126611 A CN 104126611A CN 201410355274 A CN201410355274 A CN 201410355274A CN 104126611 A CN104126611 A CN 104126611A
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Abstract
The invention discloses a preparation method of a nano-silver composite antibacterial agent. The invention is characterized in that the nano-silver composite antibacterial agent is formed by combining a nano-silver solution and an organic antibacterial agent which have synergistic effect and adduction effect according to a certain ratio. The structure and performance of the antibacterial agent after combination are stable, and the antibacterial agent has more rapid, efficient and broad-spectrum antibacterial performance. The minimal inhibitory concentration (MIC) of the antibacterial agent for inhibiting escherichia coli, Enterobacter hormaechei, staphylococcus aureus, bacillus subtilis, Rhodotorula mucilaginosa, penicillium and Aspergillus niger is only 1-10 microgram/ml. The preparation method of the nano-silver composite antibacterial agent is characterized in that the nano-silver in the nano-silver composite antibacterial agent has monodispersity and there is no agglomeration phenomenon. The preparation method has advantages of ingenious conception, simple experimental operation, high operationality and short period, and is suitable for large-scale production.
Description
Technical field
The invention belongs to nano anti-biotic material technical field, be specifically related to the preparation method of a kind of anti-microbial property wide spectrum, efficient and stable nano silver composite antibacterial agent.
Background technology
Nano anti-biotic material is the class new material growing up on inorganic antibacterial material and nano material basis.Wherein, it is efficient that Nano Silver has anti-microbial property, and good heat resistance is difficult for developing immunity to drugs and the advantage such as safety height, the focus of anti-biotic material area research and application especially.In recent years, the existing multiple inorganic antibacterial material that contains Nano Silver comes out, some of them are used in commercialization, the antibacterial effect of Nano Silver can match in excellence or beauty and even be better than any efficient antibiotic (Roy R., Hoover M. R. and Bhalla, A. S., et al. Ultradilute Ag-aquasols with extraordinary bactericidal properties:role of the system Ag-O-H
2o [J]. Materials research innovations 2007,11 (1): 3-11.).
Because nano silver particles has great specific surface area, belong to thermodynamic unstable system, and there are a large amount of blemish and dangling bonds, this makes very easily to reunite between particle, form larger-size aggregate, cause losing while finally application the due physical property of nano particle and function, thereby affect the Application and Development of its product.In order to reduce the generation of Nano Silver agglomeration, usually by nano-silver loaded on various carriers.Although silver base inorganic antibacterial agent antibacterial activity is very high, safety is fine, but the silver ion in this class material is stable not, under ultraviolet ray is irradiated or after being heated to uniform temperature, silver ion is reduced to argent, or be converted into silver oxide and make its color articles, become ash or blackening, thereby affect the commercial value of goods.Simultaneously, because occurring in nature microbe species is various, use separately Nano Silver will reach when multiple-microorganism is had to desirable inhibitory action simultaneously, its expense is large (Zhang Changhui often, Xie Yu, Xu Xuan. the progress [J] of antibacterial agent. chemical industry progress, 2007,26(9): 1237-1242.).Previous research work shows, independent Nano silver solution is better to the inhibition of bacterium, but undesirable to the inhibition of fungi, reach when yeast and mold is had to desirable inhibitory action, its minimal inhibitory concentration (MIC) is up to 40 μ g/ml, and aequum is larger.And silver is a kind of expensive noble metal, the use cost that Nano Silver is higher is also to limit its widely used another main cause.
Nano silver particles and different antibacterial agents are carried out reasonably composite, can produce synergy and doublely control effect, expanding prevention object, and reduce use cost, and increase economic efficiency, can also reduce the generation of Nano Silver agglomeration simultaneously.At present, antibacterial research for nano silver composite antibacterial agent is less, although following method can be prepared nano silver composite antibacterial agent, but still there are some problems: 1) as at CN 101669519A(polyaniline compound antibacterial agent and preparation method thereof) in Nano Silver/polyaniline compound antibacterial agent to saccharomycete, Escherichia coli, staphylococcus aureuses etc. all have excellent bactericidal action, wherein polyaniline and silver components show significant synergetic antibacterial effect, but preparation method's complexity of this nano silver composite antibacterial agent, required time long (>24h), 2) as preparation method and application thereof at a CN 103172775 A(antibacterial complex emulsions that comprises nano silver particles) in Nano Silver/azodiisobutyronitrile complex antimicrobials the antibiotic rate of Escherichia coli and staphylococcus aureus is respectively more than 95.5% and 95.5%, but the antibacterial effect of complex antimicrobials to bacterium only studied in this invention, it is not verified fungi and saccharomycetic antibacterial effect, and its broad-spectrum antibacterial property need to investigate, 3) as at CN 103563983 A(Nano Silver peroxide composite bactericidal liquid and preparation method thereof) in Nano Silver/peroxide composite bactericidal liquid can reach in the short period of time higher sterilizing rate, but preparation method's complexity of this disclosure of the invention, required time long (> 96h), and the antibacterial effect of this complex antimicrobials to staphylococcus aureus, Candida albicans and pseudomonas aeruginosa only studied in this invention, its broad-spectrum antibacterial property need to investigate.
The advantages such as organic antibacterial agent has that sterilization speed is fast, germicidal efficiency is high, colour stable, cheap and easy to get and broad spectrum antibacterial, belong to stripping property Antibacterial Mechanism; And silver base inorganic antibacterial agent belongs to non-stripping property Antibacterial Mechanism, the antibacterial term of validity is long, little to skin irritation, has a broad antifungal spectrum, but antibacterial action onset is more late, and larger to the minimal inhibitory concentration value of fungi, antimycotic efficiency is lower.Be not difficult to expect, both compound will make up the other side's deficiency mutually, brings into play both advantages separately, obtains the stronger antibacterial agent of combination property.
Summary of the invention
The object of the invention is the stable not problem of silver ion in, silver base inorganic antibacterial agent undesirable to fungi restraining effect for Nano silver solution, a kind of preparation method of nano silver composite antibacterial agent has been proposed, this nano silver composite antibacterial agent has wide spectrum, efficient anti-microbial property, and stability is high.
For reaching object of the present invention, the inventor has investigated respectively the inhibition of independent Nano silver solution to Escherichia coli, Huo Shi enterobacteria, staphylococcus aureus, bacillus subtilis, Rhodotorula mucilaginosa, mould, aspergillus niger.Wherein Escherichia coli and Huo Shi enterobacteria represent Gram-negative bacteria, and staphylococcus aureus and bacillus subtilis represent gram-positive bacteria, and Rhodotorula mucilaginosa represents saccharomycete, and mould and aspergillus niger represent mould.Result shows, Nano silver solution is better to the inhibition of bacterium, its minimal inhibitory concentration (MIC) is less than 10 μ g/ml, but undesirable to mould and saccharomycetic inhibition, reach when yeast and mold is had to desirable inhibitory action, its minimal inhibitory concentration (MIC) is up to 40 μ g/ml, and aequum is larger, thereby has increased use cost.
For expanding prevention object, and reduce Nano Silver use cost, increase economic efficiency, increase the stability of Nano Silver simultaneously, the inventor carries out at least one organic antibacterial agent in Nano silver solution and efficient, low toxicity, safety stable butyl hydroxybenzoate, isothiazolinone, triclosan reasonably compound, makes nano silver composite antibacterial agent.By transmission electron microscope and laser particle analyzer, pattern and the dispersity variation to nano silver particles in nano silver composite antibacterial agent analyzed, result shows, Nano silver solution has the characteristic feature of colloidal solution, under excessive electrolyte effect, its stability can be destroyed, and micelle flocculates.Therefore, in the time that the organic antibacterial agent adding in system is too much, excessive organic antibacterial agent will play electrolytical effect, causes the nano silver colloidal sol forming to flocculate, and small nano particle is agglomerated into larger nano particle and separates out from colloidal sol; And low concentration (≤20 μ g/ml) organic antibacterial agent can not make nano silver particles produce reunite, the particle diameter of compound rear nano silver particles and dispersity significantly do not change, this explanation and the compound stability that can not affect Nano Silver of certain density organic antibacterial agent.Uv absorption situation and the particle size situation of change of nano silver composite antibacterial agent nano silver particles under different pH condition have been investigated by ultra-violet and visible spectrophotometer and laser particle analyzer, result shows, in acid range, the increase of mixed system pH value is on nano silver particles absworption peak and not significantly impact of particle size, but in alkaline range, along with the increase of mixed system pH value, nano silver particles absorption peak strength reduces gradually and particle diameter becomes large, and this explanation nano silver composite antibacterial agent is unstable in alkaline range.Therefore, the using and store pH condition and should be advisable in acid range of complex antimicrobials, optimum is pH4.5-5.5.Simultaneously, the inventor has also investigated the inhibition of this nano silver composite antibacterial agent to bacterium, saccharomycete and mould, result shows, antibacterial agent after compound is stable and have wide spectrum, an anti-microbial property efficiently, it is all very good to the inhibition of bacterium, saccharomycete and mould, and the minimal inhibitory concentration (MIC) of Escherichia coli, Huo Shi enterobacteria, staphylococcus aureus, bacillus subtilis, Rhodotorula mucilaginosa, mould, aspergillus niger is only needed to 1-10 μ g/ml.
The preparation method of a kind of nano silver composite antibacterial agent provided by the invention, is characterized in that the method passes through following processing step and implement:
(1) be 1 × 10 by 10-100 part concentration
-4g/ml-4 × 10
-4it is 1.5 × 10 that the dispersion protectant of g/ml dropwise joins 10-100 part concentration
-4the AgNO of g/ml
3in solution, stir, obtain mixed system A.
(2) be 1 × 10 by 50-150 part concentration
-5-2 × 10
-5the reductant of g/ml and 50-150 part concentration are 1 × 10
-4g/ml-4 × 10
-4the dispersion protectant of g/ml is uniformly mixed, and obtains mixed system B.
(3) the mixed system B being prepared by step (2) dropwise joins in mixed system A prepared by step (1), and is controlled in 1.5h and adds.Stir, obtain Nano silver solution.
(4) get Nano silver solution prepared by 10-100 part step (3), adding 1-10 part concentration is the organic antibacterial agent of 1 μ g/ml-20 μ g/ml, after stirring, uses 0.1molL under normal temperature
-1naOH solution or 0.1molL
-1it is 4.5-5.5 that HCl solution regulates pH value, obtains nano silver composite antibacterial agent.
The umber of material used is mass parts above.
In the preparation method of above-mentioned nano silver composite antibacterial agent, the dispersion protectant that step (1) and step (2) are used is same.
The dispersion protectant using in above-mentioned nano silver composite antibacterial agent is any one in benzalkonium bromide, sodium citrate.
The reductant using in above-mentioned nano silver composite antibacterial agent is any one in sodium borohydride, hydrazine hydrate.
The organic antibacterial agent using in above-mentioned nano silver composite antibacterial agent is at least one in butyl hydroxybenzoate, isothiazolinone, triclosan.
The preparation method of above-mentioned a kind of nano silver composite antibacterial agent provided by the invention, has the following advantages:
1. method provided by the invention, is skillfully constructed, and experimental implementation is simple, can utilize tradition to prepare the required instrument and equipment of nano silver antimicrobials, and therefore this method does not need extra operating equipment, workable.
2. represent bacterial classification because the present invention has chosen respectively 1-2 kind in bacterium, saccharomycete and mould, therefore, the broad-spectrum antibacterial property of this nano silver composite antibacterial agent has obtained good checking.
3. can not affect particle diameter and the dispersity of nano silver particles after compound due to Nano silver solution and certain density organic antibacterial agent, and Nano silver solution and organic antibacterial agent have synergy and adduction.Therefore the nano silver composite antibacterial agent after compound not only can not be flocculated, deposited phenomenon, and has more wide spectrum, anti-microbial property efficiently.
Due to Nano Silver and the organic antibacterial agent toxicity that uses very low, thereby this nano silver composite antibacterial agent has safe serviceability.
four, embodiment
Provide embodiment below so that the present invention will be described in more detail; it is important to point out that following examples can not be interpreted as limiting the scope of the invention, some nonessential improvement that the person skilled in the art in this field makes the present invention according to the invention described above content and adjustment still belong to protection scope of the present invention.
Embodiment 1
Be 1 × 10 by 10 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 10 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1 × 10 by 50 parts of concentration
-5the sodium borohydride of g/ml and 50 parts of concentration are 1 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Getting 10 parts of Nano silver solutions, add the butyl hydroxybenzoate of 1 part of 1 μ g/ml, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 4.5 by concentration under normal temperature after stirring, and obtains nano silver composite antibacterial agent.
Embodiment 2
Be 2 × 10 by 50 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 20 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1 × 10 by 50 parts of concentration
-5the hydrazine hydrate of g/ml and 50 parts of concentration are 2 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Getting 10 parts of Nano silver solutions, add the butyl hydroxybenzoate of 1 part of 1 μ g/ml, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 4.5 by concentration under normal temperature after stirring, and obtains nano silver composite antibacterial agent.
Embodiment 3
Be 3 × 10 by 50 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 50 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1 × 10 by 100 parts of concentration
-5the sodium borohydride of g/ml and 50 parts of concentration are 3 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 20 parts of Nano silver solutions, add the isothiazolinone of butyl hydroxybenzoate and the 2 part of 2 μ g/ml of 5 part of 2 μ g/ml, after stirring under normal temperature, be that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 4.5 by concentration, obtain nano silver composite antibacterial agent.
Embodiment 4
Be 2 × 10 by 50 parts of concentration
-4it is 1.5 × 10 that the sodium citrate solution of g/ml dropwise joins 50 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.2 × 10 by 50 parts of concentration
-5the sodium borohydride of g/ml and 50 parts of concentration are 2 × 10
-4the sodium citrate solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 40 parts of Nano silver solutions, adding 5 parts of concentration is the triclosan of 5 μ g/ml, 5 parts of butyl hydroxybenzoate and 1 part of isothiazolinone that concentration is 10 μ g/ml that concentration is 5 μ g/ml, after stirring under normal temperature, be that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.0 by concentration, obtain nano silver composite antibacterial agent.
Embodiment 5
Be 4 × 10 by 100 parts of concentration
-4it is 1.5 × 10 that the sodium citrate solution of g/ml dropwise joins 80 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.2 × 10 by 50 parts of concentration
-5the sodium borohydride of g/ml and 50 parts of concentration are 4 × 10
-4the sodium citrate solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 50 parts of Nano silver solutions, adding 5 parts of concentration is the isothiazolinone of 8 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.0 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
Embodiment 6
Be 4 × 10 by 10 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 80 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.25 × 10 by 80 parts of concentration again
-5the hydrazine hydrate of g/ml and 100 parts of concentration are 4 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 50 parts of Nano silver solutions, adding 10 parts of concentration is the triclosan of 10 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.0 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
Embodiment 7
Be 1 × 10 by 10 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 100 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.85 × 10 by 100 parts of concentration again
-5the sodium borohydride of g/ml and 50 parts of concentration are 1 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 50 parts of Nano silver solutions, adding 1 part of concentration is the butyl hydroxybenzoate of 10 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.0 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
Embodiment 8
Be 4 × 10 by 100 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 100 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.5 × 10 by 150 parts of concentration again
-5the sodium borohydride of g/ml and 150 parts of concentration are 4 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 80 parts of Nano silver solutions, adding 1 part of concentration is the triclosan of 15 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.0 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
Embodiment 9
Be 2 × 10 by 50 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 100 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.85 × 10 by 50 parts of concentration again
-5the hydrazine hydrate of g/ml and 150 parts of concentration are 2 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 100 parts of Nano silver solutions, adding 5 parts of concentration is the isothiazolinone of 20 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.0 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
Embodiment 10
Be 1 × 10 by 100 parts of concentration
-4it is 1.5 × 10 that the sodium citrate solution of g/ml dropwise joins 100 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.85 × 10 by 50 parts of concentration again
-5the sodium borohydride of g/ml and 100 parts of concentration are 1 × 10
-4the sodium citrate solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 100 parts of Nano silver solutions, add butyl hydroxybenzoate and 2 parts of isothiazolinone that concentration is 5 μ g/ml that 5 parts of concentration are 5 μ g/ml, after stirring under normal temperature, be that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.5 by concentration, obtain nano silver composite antibacterial agent.
Embodiment 11
Be 1 × 10 by 80 parts of concentration
-4it is 1.5 × 10 that the sodium citrate solution of g/ml dropwise joins 100 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 1.85 × 10 by 150 parts of concentration again
-5the sodium borohydride of g/ml and 150 parts of concentration are 1 × 10
-4the sodium citrate solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 100 parts of Nano silver solutions, adding 5 parts of concentration is the butyl hydroxybenzoate of 20 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.5 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
Embodiment 12
Be 4 × 10 by 100 parts of concentration
-4it is 1.5 × 10 that the benzalkonium bromide solution of g/ml dropwise joins 100 parts of concentration
-3the AgNO of g/ml
3in solution, stir, obtain mixed system A.Be 2 × 10 by 150 parts of concentration again
-5the sodium borohydride of g/ml and 100 parts of concentration are 4 × 10
-4the benzalkonium bromide solution of g/ml is uniformly mixed, and obtains mixed system B.Mixed system B is dropwise joined in mixed system A, and be controlled in 1.5h and add, stir, obtain Nano silver solution.Get 100 parts of Nano silver solutions, adding 10 parts of concentration is the isothiazolinone of 20 μ g/ml, after stirring, is that 0.1mol/L NaOH solution or concentration are that 0.1mol/L HCl solution adjusting pH value is 5.5 by concentration under normal temperature, obtains nano silver composite antibacterial agent.
In order to investigate the anti-microbial property of nano silver composite antibacterial agent prepared by the embodiment of the present invention, the inventor has made following antibacterial test to it:
The antibacterial agent of getting respectively 10ml variable concentrations gradient adds in plate.The agar medium that again 10ml is cooled to 45 DEG C～50 DEG C adds in plate, and limit edged rocks flat board, and antibacterial agent and medium are fully mixed, for subsequent use after solidifying.Get 1 μ l(bacteria containing amount with sample injector and be about 10
7cfu/ml) bacteria suspension dibbling, in the media surface containing antibacterial agent, is inoculated the rear about 5mm～8mm of bacterium liquid loop diameter forming.Putting into (temperature is that 27 DEG C of humidity are 85%) in climatic chamber carries out after the bacterium and mycotic culture of 2 days again, observe the minimum antibacterial agent concentration that colony growth is suppressed completely, for the minimal inhibitory concentration (MIC) (concrete grammar be shown in disinfection technology standard Part II (minimal inhibitory concentration testing experiment)) of this sample to tested bacterium, the results are shown in Table 1, table 2.
。
Claims (5)
1. a preparation method for anti-microbial property wide spectrum, efficient and stable nano silver composite antibacterial agent, is characterized in that the processing step of the method and condition are as follows:
(1) be 1 × 10 by 10-100 part concentration
-4g/ml-4 × 10
-4it is 1.5 × 10 that the dispersion protectant of g/ml dropwise joins 10-100 part concentration
-4the AgNO of g/ml
3in solution, stir, obtain mixed system A;
(2) be 1 × 10 by 50-150 part concentration
-5-2 × 10
-5the reductant of g/ml and 50-150 part concentration are 1 × 10
-4g/ml-4 × 10
-4the dispersion protectant of g/ml is uniformly mixed, and obtains mixed system B;
(3) the mixed system B being prepared by step (2) dropwise joins in mixed system A prepared by step (1), and is controlled in 1.5h and adds;
Stir, obtain Nano silver solution;
(4) get Nano silver solution prepared by 10-100 part step (3), adding 1-10 part concentration is the organic antibacterial agent of 1 μ g/ml-20 μ g/ml, after stirring under normal temperature, be that 0.1mol/L NaOH solution or concentration are that 0.1mol/LHCl solution adjusting pH value is 4.5-5.5 by concentration, obtain nano silver composite antibacterial agent;
The umber of material used is mass parts above.
2. the preparation method of a kind of nano silver composite antibacterial agent according to claim 1, is characterized in that the dispersion protectant using in step (1) and step (2) is same.
3. according to the preparation method of claim 1 and a kind of nano silver composite antibacterial agent claimed in claim 2, it is characterized in that the dispersion protectant that uses in nano silver composite antibacterial agent is for any one in benzalkonium bromide, sodium citrate.
4. the preparation method of a kind of nano silver composite antibacterial agent according to claim 1, is characterized in that the reductant that uses in nano silver composite antibacterial agent is for any one in sodium borohydride, hydrazine hydrate.
5. the preparation method of a kind of nano silver composite antibacterial agent according to claim 1, is characterized in that the organic antibacterial agent that uses in nano silver composite antibacterial agent is at least one in butyl hydroxybenzoate, isothiazolinone, triclosan.
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