CN104126611B - A kind of preparation method of nano silver composite antibacterial agent - Google Patents

A kind of preparation method of nano silver composite antibacterial agent Download PDF

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CN104126611B
CN104126611B CN201410355274.2A CN201410355274A CN104126611B CN 104126611 B CN104126611 B CN 104126611B CN 201410355274 A CN201410355274 A CN 201410355274A CN 104126611 B CN104126611 B CN 104126611B
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antibacterial agent
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nano silver
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CN104126611A (en
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陈武勇
杨威特
唐秋月
李慧
张金伟
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Sichuan University
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Abstract

The preparation method of a kind of nano silver composite antibacterial agent disclosed by the invention, it is characterized in that this nano silver composite antibacterial agent is to be composited according to a certain percentage with organic antibacterial agent by the nanometer silver solution with synergism and adduction, antibacterial structure after Fu He and stable in properties, and there is more quick, efficient, the anti-microbial property of wide spectrum, it only needs 1 10 μ g/ml to escherichia coli, Huo Shi enterobacteria, staphylococcus aureus, bacillus subtilis, Rhodotorula mucilaginosa, penicillium sp, the minimal inhibitory concentration (MIC) of aspergillus niger.The preparation method of a kind of nano silver composite antibacterial agent disclosed by the invention, it is characterised in that in this nano silver composite antibacterial agent, nanometer silver is monodispersity, soilless sticking phenomenon, its preparation method is skillfully constructed, and experimental implementation is simple, workable, cycle is short, is suitable for large-scale production.

Description

A kind of preparation method of nano silver composite antibacterial agent
Technical field
The invention belongs to nano anti-biotic material technical field, be specifically related to a kind of anti-microbial property wide spectrum, efficient and stable The preparation method of nano silver composite antibacterial agent.
Background technology
Nano anti-biotic material is the class new material grown up on the basis of inorganic antibacterial material and nano material.Its In, it is efficient that nanometer silver has anti-microbial property, heat-resist, is not likely to produce Drug resistance and safety advantages of higher, the most antibacterial material Material area research and the focus of application.In recent years, the existing multiple inorganic antibacterial material containing nanometer silver comes out, and some of them are Commercially use, the antibacterial effect of nanometer silver can match in excellence or beauty even 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-H2O [J]. Materials research innovations 2007,11 (1): 3-11.).
Owing to nano silver particles has great specific surface area, belong to thermodynamic unstable system, and there is substantial amounts of table Planar defect and dangling bonds, this makes easily to reunite between granule, forms larger-size aggregate, loses and receive when causing finally applying The due physical property of rice grain and function, thus affect the exploitation application of its product.In order to reduce the generation of nanometer silver agglomeration, Usually by nano-silver loaded on various carriers.Although silver base inorganic antibacterial agent antibacterial activity is the highest, safety is fine, but this kind of Silver ion in material is not sufficiently stable, and under ultraviolet irradiates or after being heated to uniform temperature, silver ion is reduced to argent, Or be converted into silver oxide and make its color articles, graying or blackening, thus have impact on the commercial value of goods.Simultaneously as from So in boundary, microbe species is various, is used alone nanometer silver and to reach that multiple-microorganism is had preferable inhibitory action simultaneously Time, its expense the biggest (Zhang Changhui, Xie Yu, Xu Xuan. the progress [J] of antibacterial. chemical industry is in progress, 2007,26 (9): 1237-1242.).Previous research work shows, single nanometer silver solution is preferable to the inhibition of antibacterial, but right The inhibition of fungus is undesirable, when will reach that yeast and mold is had preferable inhibitory action, and its minimal inhibitory concentration (MIC) being up to 40 μ g/ml, aequum is bigger.And silver is a kind of expensive noble metal, the higher use cost of nanometer silver is also It is to limit its another main cause widely used.
Nano silver particles is reasonably compounded from different antibacterial, potentiation can be produced and double control effect, expanding anti- Control object, and reduce use cost, increase economic efficiency, the generation of nanometer silver agglomeration can also be reduced simultaneously.At present, for The antibacterial research of nano silver composite antibacterial agent is less, although following method can prepare 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 nanometer silver/poly- Aniline complex antimicrobials all has the bactericidal action of excellence, wherein polyphenyl to yeast, escherichia coli, staphylococcus aureus etc. Amine and silver components show significant synergetic antibacterial effect, but the preparation method of this nano silver composite antibacterial agent is complicated, required Time length (> 24h);2) as comprised the preparation method of the antibacterial complex emulsions of nano silver particles CN 103172775 A(mono-kind And application) in nanometer silver/azodiisobutyronitrile complex antimicrobials the antibiotic rate of escherichia coli and staphylococcus aureus is divided Not being 95.5% and more than 95.5%, but this invention only have studied the complex antimicrobials antibacterial effect to antibacterial, it is to fungus And saccharomycetic antibacterial effect is not verified, its broad-spectrum antibacterial property need to investigate;3) as at CN 103563983 A(mono- Kind of nano-silver peroxide composite antibacterial solution and preparation method thereof) in nanometer silver/peroxide composite bactericidal liquid when shorter In can reach higher sterilizing rate, but the preparation method of this disclosure of the invention is complicated, required time length (> 96h), and this Invention only have studied this complex antimicrobials antibacterial effect to staphylococcus aureus, Candida albicans and Pseudomonas aeruginosa, Its broad-spectrum antibacterial property need to investigate.
Organic antibacterial agent has that sterilization speed is fast, germicidal efficiency is high, colour stable, cheap and easy to get and broad spectrum antibacterial etc. are excellent Point, belongs to stripping property Antibacterial Mechanism;And silver base inorganic antibacterial agent belongs to non-stripping property Antibacterial Mechanism, antibacterial effect duration is long, stings skin Swash property little, has a broad antifungal spectrum, but antibacterial action onset is later, and relatively big to the minimal inhibitory concentration value of fungus, antifungal efficiency Relatively low.It is contemplated that both compound will mutually make up the deficiency of the other side, play both respective advantages, it is thus achieved that combination property Stronger antibacterial.
Summary of the invention
It is an object of the invention to the silver in, silver base inorganic antibacterial agent undesirable to fungi restraining effect for nanometer silver solution The problem that ion is not sufficiently stable, it is proposed that the preparation method of a kind of nano silver composite antibacterial agent, this nano silver composite antibacterial agent has There are wide spectrum, efficient anti-microbial property, and stability is high.
For reaching the purpose of the present invention, the present inventor has investigated single nanometer silver solution respectively to escherichia coli, Huo Shi intestinal Bacillus, staphylococcus aureus, bacillus subtilis, Rhodotorula mucilaginosa, penicillium sp, the inhibition of aspergillus niger.Wherein large intestine Bacillus and Huo Shi enterobacteria represent gram negative bacteria, and staphylococcus aureus and bacillus subtilis represent Gram-positive Bacterium, Rhodotorula mucilaginosa represents yeast, and penicillium sp and aspergillus niger represent mycete.Result shows, antibacterial is pressed down by nanometer silver solution Effect processed is preferable, and its minimal inhibitory concentration (MIC) is less than 10 μ g/ml, but pays no attention to mycete and saccharomycetic inhibition Thinking, when will reach that yeast and mold is had preferable inhibitory action, its minimal inhibitory concentration (MIC) is up to 40 μ g/ml, institute Requirement is relatively big, thus adds use cost.
For expanding prevention object, and reduce the use cost of nanometer silver, increase economic efficiency, increase nanometer silver simultaneously Stability, the present inventor is by nanometer silver solution and efficient, low toxicity, safe and stable butoben, isothiazolone, trichlorine At least one organic antibacterial agent in life is reasonably combined, and prepares nano silver composite antibacterial agent.By transmission electron microscope and Pattern and the dispersion change of nano silver particles in nano silver composite antibacterial agent are analyzed by laser particle analyzer, and result shows Showing, nanometer silver solution has the typical characteristic of colloid solution, and under the electrolyte effect of excess, its stability can be destroyed, glue Grain flocculates.Therefore, when the organic antibacterial agent added in system is too much, the organic antibacterial agent of excess will play electrolyte Effect, the nano silver colloidal sol resulted in flocculates, and small nanoparticle is agglomerated into bigger nano-particle and from molten Glue separates out;And the organic antibacterial agent of low concentration (20 μ g/ml) will not make nano silver particles produce reunion, compound rear nanometer silver Particle diameter and the dispersion of particle do not change significantly, and this explanation is compound with certain density organic antibacterial agent does not interferes with nanometer The stability of silver.Nano silver composite antibacterial agent has been investigated at different pH by ultra-violet and visible spectrophotometer and laser particle analyzer The uv absorption situation of nano silver particles and size situation of change under the conditions of value, result shows, in acid range, mixing Nano silver particles absworption peak and size are the most significantly affected by the increase of system pH, but in alkaline range, along with The increase of mixed system pH value, nano silver particles absorption peak strength is gradually lowered and particle diameter becomes big, and this explanation nanometer silver is compound anti- Microbial inoculum is unstable in alkaline range.Therefore, using and storing pH condition of complex antimicrobials should be advisable in acid range, Excellent for pH4.5-5.5.Meanwhile, the present inventor has also investigated this nano silver composite antibacterial agent to antibacterial, yeast and mycete Inhibition, result shows, the antibacterial after being combined is stable and has wide spectrum, efficient anti-microbial property, and it is to antibacterial, yeast And the inhibition of mycete is the most very good, to escherichia coli, Huo Shi enterobacteria, staphylococcus aureus, bacillus subtilis Bacterium, Rhodotorula mucilaginosa, penicillium sp, the minimal inhibitory concentration (MIC) of aspergillus niger only need 1-10 μ g/ml.
The preparation method of a kind of nano silver composite antibacterial agent that the present invention provides, it is characterised in that the method is by following work Skill step is implemented:
(1) it is 1 × 10 by 10-100 part concentration-4g/ml-4×10-4The dispersion protective agent of g/ml is added dropwise to 10-100 Part concentration is 1.5 × 10-4The AgNO of g/ml3In solution, stir, obtain mixed system A.
(2) it is 1 × 10 by 50-150 part concentration-5-2×10-5Reducing agent and 50-150 part concentration of g/ml are 1 × 10- 4g/ml-4×10-4The dispersion protective agent stirring mixing of g/ml, obtains mixed system B.
(3) mixed system B prepared by step (2) is added dropwise in mixed system A prepared by step (1), and controls System adds in 1.5h.Stir, obtain nanometer silver solution.
(4) taking nanometer silver solution prepared by 10-100 part step (3), adding 1-10 part concentration is 1 μ g/ml-20 μ g/ml Organic antibacterial agent, use 0.1mol L after stirring under room temperature-1NaOH solution or 0.1mol L-1 HCl solution regulation pH value For 4.5-5.5, obtain nano silver composite antibacterial agent.
The number of material used above is mass parts.
In the preparation method of above-mentioned nano silver composite antibacterial agent, the dispersion protective agent that step (1) and step (2) use is same A kind of.
The dispersion protective agent used in above-mentioned nano silver composite antibacterial agent is any one in benzalkonium bromide, sodium citrate Kind.
The reducing agent used in above-mentioned nano silver composite antibacterial agent is any one in sodium borohydride, hydrazine hydrate.
The organic antibacterial agent used in above-mentioned nano silver composite antibacterial agent is butoben, isothiazolone, triclosan In at least one.
The preparation method of above-mentioned a kind of nano silver composite antibacterial agent that the present invention provides, has the advantage that
1. the method that the present invention provides, is skillfully constructed, and experimental implementation is simple, and available tradition prepares nano silver antimicrobials institute The instrument and equipment needed, therefore this method need not extra operation equipment, workable.
2. represent strain owing to the present invention have chosen 1-2 kind in antibacterial, yeast and mycete respectively, therefore, this nanometer The broad-spectrum antibacterial property of silver complex antimicrobials has obtained good checking.
3. do not interfere with the particle diameter of nano silver particles after compound due to nanometer silver solution and certain density organic antibacterial agent With dispersion, and nanometer silver solution and organic antibacterial agent have synergism and adduction.Therefore the nanometer silver after being combined is multiple Conjunction antibacterial not only will not flocculate, deposited phenomenon, and has more wide spectrum, efficient anti-microbial property.
4. the lowest due to nanometer silver and the organic antibacterial agent toxicity used, thus this nano silver composite antibacterial agent has peace Full serviceability.
Four, detailed description of the invention
Embodiment is given below so that the present invention will be described in more detail, it is necessary to be pointed out that following example can not be managed Solving is limiting the scope of the invention, and the present invention is made by the person skilled in the art in this field according to the invention described above content Some nonessential improvement and adjust still belong to protection scope of the present invention.
Embodiment 1
It is 1 × 10 by 10 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 10 parts of concentration-3g/ml AgNO3In solution, stir, obtain mixed system A.It is 1 × 10 by 50 parts of concentration-5The sodium borohydride of g/ml and 50 parts dense Degree is 1 × 10- 4The benzalkonium bromide solution stirring mixing of g/ml, obtains mixed system B.Mixed system B is added dropwise to mixing In system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 10 parts of nanometer silver solution, add 1 part The butoben of 1 μ g/ml, is 0.1mol/L NaOH solution by concentration after stirring or concentration is 0.1mol/L under room temperature HCl solution regulation pH value is 4.5, obtains nano silver composite antibacterial agent.
Embodiment 2
It is 2 × 10 by 50 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 20 parts of concentration-3g/ml AgNO3In solution, stir, obtain mixed system A.It is 1 × 10 by 50 parts of concentration-5The hydrazine hydrate of g/ml and 50 parts of concentration It is 2 × 10- 4The benzalkonium bromide solution stirring mixing of g/ml, obtains mixed system B.Mixed system B is added dropwise to mixture It is in A, and controls to add in 1.5h, stir, obtain nanometer silver solution.Take 10 parts of nanometer silver solution, add 1 part of 1 μ The butoben of g/ml, is 0.1mol/L NaOH solution by concentration after stirring or concentration is 0.1mol/L under room temperature HCl solution regulation pH value is 4.5, obtains nano silver composite antibacterial agent.
Embodiment 3
It is 3 × 10 by 50 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 50 parts of concentration-3g/ml AgNO3In solution, stir, obtain mixed system A.It is 1 × 10 by 100 parts of concentration-5The sodium borohydride of g/ml and 50 parts Concentration is 3 × 10- 4The benzalkonium bromide solution stirring mixing of g/ml, obtains mixed system B.It is added dropwise to mix by mixed system B In zoarium system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 20 parts of nanometer silver solution, add 5 It is 0.1mol/L by concentration after stirring under the butoben of part 2 μ g/ml and the isothiazolone of 2 part of 2 μ g/ml, room temperature NaOH solution or concentration be 0.1mol/L HCl solution regulation pH value be 4.5, obtain nano silver composite antibacterial agent.
Embodiment 4
It is 2 × 10 by 50 parts of concentration-4It is 1.5 × 10 that the sodium citrate solution of g/ml is added dropwise to 50 parts of concentration-3g/ml AgNO3In solution, stir, obtain mixed system A.It is 1.2 × 10 by 50 parts of concentration-5The sodium borohydride of g/ml and 50 parts Concentration is 2 × 10- 4The sodium citrate solution stirring mixing of g/ml, obtains mixed system B.It is added dropwise to mix by mixed system B In zoarium system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 40 parts of nanometer silver solution, add 5 Part concentration be the triclosan of 5 μ g/ml, 5 parts of concentration be the butoben of 5 μ g/ml and isothiazole that 1 part of concentration is 10 μ g/ml Quinoline ketone, by concentration is 0.1mol/L NaOH solution after stirring under room temperature or concentration is that 0.1mol/L HCl solution regulates pH Value is 5.0, obtains nano silver composite antibacterial agent.
Embodiment 5
It is 4 × 10 by 100 parts of concentration-4It is 1.5 × 10 that the sodium citrate solution of g/ml is added dropwise to 80 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 1.2 × 10 by 50 parts of concentration-5The sodium borohydride of g/ml and 50 Part concentration is 4 × 10- 4The sodium citrate solution stirring mixing of g/ml, obtains mixed system B.Mixed system B is added dropwise to In mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 50 parts of nanometer silver solution, add Enter the isothiazolone that 5 parts of concentration is 8 μ g/ml, be 0.1mol/L NaOH solution or concentration by concentration after stirring under room temperature It is 5.0 for 0.1mol/L HCl solution regulation pH value, obtains nano silver composite antibacterial agent.
Embodiment 6
It is 4 × 10 by 10 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 80 parts of concentration-3g/ml AgNO3In solution, stir, obtain mixed system A.It is 1.25 × 10 by 80 parts of concentration again-5The hydrazine hydrate of g/ml and 100 Part concentration is 4 × 10- 4The benzalkonium bromide solution stirring mixing of g/ml, obtains mixed system B.Mixed system B is added dropwise to In mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 50 parts of nanometer silver solution, add Enter the triclosan that 10 parts of concentration is 10 μ g/ml, be 0.1mol/L NaOH solution by concentration after stirring under room temperature or concentration is 0.1mol/L HCl solution regulation pH value is 5.0, obtains nano silver composite antibacterial agent.
Embodiment 7
It is 1 × 10 by 10 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 100 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 1.85 × 10 by 100 parts of concentration again-5The sodium borohydride of g/ml It is 1 × 10 with 50 parts of concentration- 4The benzalkonium bromide solution stirring mixing of g/ml, obtains mixed system B.Mixed system B is dropwise added Enter in mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 50 parts of nanometer silvers molten Liquid, adds the butoben that 1 part of concentration is 10 μ g/ml, is that 0.1mol/L NaOH is molten by concentration under room temperature after stirring Liquid or concentration be 0.1mol/L HCl solution regulation pH value be 5.0, obtain nano silver composite antibacterial agent.
Embodiment 8
It is 4 × 10 by 100 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 100 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 1.5 × 10 by 150 parts of concentration again-5The sodium borohydride of g/ml It is 4 × 10 with 150 parts of concentration- 4The benzalkonium bromide solution stirring mixing of g/ml, obtains mixed system B.By mixed system B dropwise Join in mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 80 parts of nanometer silvers molten Liquid, adds the triclosan that 1 part of concentration is 15 μ g/ml, is 0.1mol/L NaOH solution or dense by concentration under room temperature after stirring Spending for 0.1mol/L HCl solution regulation pH value is 5.0, obtains nano silver composite antibacterial agent.
Embodiment 9
It is 2 × 10 by 50 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 100 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 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 stirring mixing of g/ml, obtains mixed system B.Mixed system B is dropwise added Enter in mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 100 parts of nanometer silvers molten Liquid, adds the isothiazolone that 5 parts of concentration is 20 μ g/ml, is 0.1mol/L NaOH solution by concentration under room temperature after stirring Or concentration be 0.1mol/L HCl solution regulation pH value be 5.0, obtain nano silver composite antibacterial agent.
Embodiment 10
It is 1 × 10 by 100 parts of concentration-4It is 1.5 × 10 that the sodium citrate solution of g/ml is added dropwise to 100 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 1.85 × 10 by 50 parts of concentration again-5The sodium borohydride of g/ml It is 1 × 10 with 100 parts of concentration- 4The sodium citrate solution stirring mixing of g/ml, obtains mixed system B.By mixed system B dropwise Join in mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 100 parts of nanometer silvers Solution, adds butoben that 5 parts of concentration is 5 μ g/ml and isothiazolone that 2 parts of concentration is 5 μ g/ml, stirs under room temperature Be 0.1mol/L NaOH solution by concentration after Jun Yun or concentration be 0.1mol/L HCl solution regulation pH value be 5.5, obtain nanometer Silver complex antimicrobials.
Embodiment 11
It is 1 × 10 by 80 parts of concentration-4It is 1.5 × 10 that the sodium citrate solution of g/ml is added dropwise to 100 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 1.85 × 10 by 150 parts of concentration again-5The sodium borohydride of g/ml It is 1 × 10 with 150 parts of concentration- 4The sodium citrate solution stirring mixing of g/ml, obtains mixed system B.By mixed system B dropwise Join in mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 100 parts of nanometer silvers Solution, adds the butoben that 5 parts of concentration is 20 μ g/ml, is that 0.1mol/L NaOH is molten by concentration under room temperature after stirring Liquid or concentration be 0.1mol/L HCl solution regulation pH value be 5.5, obtain nano silver composite antibacterial agent.
Embodiment 12
It is 4 × 10 by 100 parts of concentration-4It is 1.5 × 10 that the benzalkonium bromide solution of g/ml is added dropwise to 100 parts of concentration-3g/ The AgNO of ml3In solution, stir, obtain mixed system A.It is 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 stirring mixing of g/ml, obtains mixed system B.Mixed system B is added dropwise over In mixed system A, and control to add in 1.5h, stir, obtain nanometer silver solution.Take 100 parts of nanometer silver solution, Add the isothiazolone that 10 parts of concentration is 20 μ g/ml, after stirring under room temperature with concentration be 0.1mol/L NaOH solution or Concentration be 0.1mol/L HCl solution regulation pH value be 5.5, obtain 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, it is made by the present inventor Following antibacterial test:
The antibacterial taking 10ml variable concentrations gradient respectively adds in plate.10ml is cooled to 45 DEG C~50 DEG C again Agar culture medium adds in plate, and limit edged rocks flat board, makes antibacterial and culture medium fully mix, to be solidified rear standby.With Sample injector takes 1 μ l(bacteria containing amount and is about 107Cfu/ml) bacteria suspension dibbling is in the media surface containing antibacterial, is formed after inoculation Bacterium solution loop diameter about 5mm~8mm.Place in climatic chamber the antibacterial that (temperature be 27 DEG C of humidity be 85%) is carried out 2 days After mycotic culture, observe the minimum antimicrobial agent concentration that colony growth is totally constrained, for this sample, the minimum of tested bacterium is pressed down Bacteria concentration (MIC) (concrete grammar is shown in disinfection technology standard Part II (minimal inhibitory concentration testing experiment)), the results are shown in Table 1, Table 2.

Claims (3)

1. an anti-microbial property wide spectrum, the preparation method of efficient and stable nano silver composite antibacterial agent, it is characterised in that the party Processing step and the condition of method are as follows:
(1) it is 1 × 10 by 10-100 part concentration-4g/ml-4×10-4It is dense that the dispersion protective agent of g/ml is added dropwise to 10-100 part Degree is 1.5 × 10-4The AgNO of g/ml3In solution, stir, obtain mixed system A;
(2) it is 1 × 10 by 50-150 part concentration-5-2×10-5Reducing agent and 50-150 part concentration of g/ml are 1 × 10-4g/ml-4 ×10-4The dispersion protective agent stirring mixing of g/ml, obtains mixed system B;
(3) mixed system B prepared by step (2) is added dropwise in mixed system A prepared by step (1), and controls Add in 1.5h;
Stir, obtain nanometer silver solution;
(4) taking nanometer silver solution prepared by 10-100 part step (3), adding 1-10 part concentration is having of 1 μ g/ml-20 μ g/ml Machine antibacterial, by concentration is 0.1mol/L NaOH solution after stirring under room temperature or concentration is the regulation of 0.1mol/LHCl solution PH value is 4.5-5.5, obtains nano silver composite antibacterial agent;
The number of material used above is mass parts;
Described dispersion protective agent is sodium citrate;
Described reducing agent is hydrazine hydrate.
The preparation method of a kind of nano silver composite antibacterial agent the most according to claim 1, it is characterised in that step (1) and step Suddenly the dispersion protective agent used in (2) is same.
The preparation method of a kind of nano silver composite antibacterial agent the most according to claim 1, it is characterised in that nanometer silver is combined The organic antibacterial agent used in antibacterial is at least one in butoben, isothiazolone, triclosan.
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