CN100528427C - Method for preparing nanometer silver composite sol - Google Patents
Method for preparing nanometer silver composite sol Download PDFInfo
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- CN100528427C CN100528427C CNB2007101217985A CN200710121798A CN100528427C CN 100528427 C CN100528427 C CN 100528427C CN B2007101217985 A CNB2007101217985 A CN B2007101217985A CN 200710121798 A CN200710121798 A CN 200710121798A CN 100528427 C CN100528427 C CN 100528427C
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Abstract
The present invention relates to a nano-silver composite collosol and the producing method; the raw materials of the collosol comprise silver nitrate solution, zinc nitrate solution, iron nitrate solution, copper nitrate solution, surface activating agent, hydrazine hydrate and dispersant. In the process of producing the composite collosol, the silver nitrate solution, zinc nitrate solution, iron nitrate solution and copper nitrate solution are mixed and the surface activating agent is added; at last, the hydrazine hydrate is added and mixed slowly; after inert reaction, the mixing solution is cleansed with water and dried under low temperature; and then the nano-composite powder of a plurality of components such as silver, zinc, copper, etc. is obtained; after standing, separation and cleansing, the powder is dispersed into solvent again to get the composite collosol of a grain size of 10 to 100 nm; the collosol has even grain size; the raw material is easy to obtain; the process is simple and the cost is low; the present invention is convenient for industrial production and the present invention can be applied in extremely wide fields.
Description
Technical field
The present invention relates to a kind of preparation method of colloidal sol, be specifically related to a kind of preparation method of Nano Silver complex sol.
Background technology
Argent is a kind of antibacterial material safely and effectively.Its antibacterium or sterilization effects are highly reinforcing when the silver particles size is nano level yardstick.Because himself characteristic widely, high-efficiency environment friendly does not cause any side effect, Nano Silver at home and abroad scientific domain and industrial circle in caused the attention of height.Outside the desilver,, also be effective antibacterial material as metals such as copper and zinc.Compound silver-the zinc of applying nano-copper powder is because the coordination performance of its multiple antibacterial composition is more effective and be applied even more extensively.In addition, the nano combined colloidal sol of argentiferous has very high using value in some special conductive materials.
At present, the raw material ratio of preparation nano silver colloidal sol is more single, adopts liquor argenti nitratis ophthalmicus to prepare more, only contains Nano Silver in the colloidal sol that makes usually, and ratio of component is more single, and the useful effect of Nano Silver is also limited.
In addition, at present, the method that prepare nano silver colloidal sol is also more, mainly be preparation method about the monocomponent nanocomposite silver sol report more, the method for preparing nano silver colloidal sol has multiple, comprises direct-reduction process, chemical deposition, galvanoplastic etc.Wherein will introduce the reunion that protective agent prevents nano silver colloidal sol in direct-reduction process etc., and wherein residual chemical surfactant has chemical toxicity, influenced the performance of nano silver colloidal sol; Require reductant solution freezingly to have relatively high expectations more than 0.5 hour as patent CN200510062319.8, and technology is complicated at 0-8 ℃.
Summary of the invention
At the defective that exists in the prior art; the preparation method who the purpose of this invention is to provide a kind of Nano Silver complex sol; prepare the Nano Silver complex sol good stability that forms by this method; do not need to introduce other protective agent, and epigranular, raw material is easy to get; technology is simple; cost is low, is widely used, and can give full play to the Synergistic antimicrobial performance of nano combined silver-zinc-copper powder.
For reaching above purpose, the technical solution used in the present invention is: a kind of preparation method of Nano Silver complex sol comprises the steps:
(1) prepare following raw material:
A. weight percent concentration is the liquor argenti nitratis ophthalmicus of 0.01-5.0%
B. weight percent concentration is the 0.001-5.0% zinc nitrate solution
C. weight percent concentration is the 0.001-5.0% iron nitrate solution
D. weight percent concentration is the 0.001-5.0% copper nitrate solution
E. weight percent concentration is the 0.01-5.0% surfactant solution
F. weight percent concentration is the 0.001-1.0% hydrazine hydrate
G. dispersion solvent
Wherein, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is 1.0: 0.001-0.31: 0.001-0.48: 0.001-0.43: 0.001-1.0: 0.5-4.5;
In the above-mentioned raw materials, in described B, C, three kinds of materials of D, can select wherein any one, two kinds or three kinds;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, add surfactant then, and then adding distilled water, pure water or deionized water dilute, add hydrazine hydrate and slowly stirring at last again, mixing speed is changeed for per minute 500-3000, when the pH of solution value reaches 6.5-7.5, stop to add hydrazine hydrate, continue then to mix and stirred 10-30 minute, obtain to comprise the nano-complex particle of Nano Silver at last;
(3) place by step (2) products therefrom and promptly comprise nano-complex particle 5-12 hour of Nano Silver, obtain to contain the nano composite powder of Nano Silver then through separation, washing, 50-60 ℃ dry back, wherein, the content of Nano Silver is 50-99.6%, and granularity is 10-100nm;
(4) will be dispersed in the dispersion solvent by the nano composite powder that step (3) obtain, supersonic oscillations 10-30 minute then, promptly obtain the Nano Silver complex sol.
Further, obtain better invention effect for making the present invention, the raw material described in the step (1) is preferably as follows:
A. weight percent concentration is the liquor argenti nitratis ophthalmicus of 0.01-3.0%
B. weight percent concentration is the zinc nitrate solution of 0.01-5.0%
C. weight percent concentration is the iron nitrate solution of 0.001-3.0%
D. weight percent concentration is the copper nitrate solution of 0.001-4.0%
E. weight percent concentration is the surfactant solution of 0.01-2.0%
F. weight percent concentration is the hydrazine hydrate of 0.001-0.9%
G. dispersion solvent
Wherein, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1.0: 0.01-0.31: 0.001-0.29: 0.001-0.35: 0.001-0.4: 0.5-4.5;
Further, obtain better invention effect for making the present invention, the raw material described in the step (1) is more preferably as follows:
A. weight percent concentration is the liquor argenti nitratis ophthalmicus of 0.01-2.0%
B. weight percent concentration is the zinc nitrate solution of 0.1-5.0%
C. weight percent concentration is the iron nitrate solution of 0.01-3.0%
D. weight percent concentration is the copper nitrate solution of 0.001-2.0%
E. weight percent concentration is the surfactant solution of 0.1-2.0%
F. weight percent concentration is the hydrazine hydrate of 0.001-0.6%
G. dispersion solvent
Wherein, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1.0: 0.1-0.30: 0.01-0.29: 0.001-0.18: 0.01-0.4: 0.5-2.7.
Further, obtain better invention effect for making the present invention, the surfactant described in the step (1) is one or more compositions in lauryl sodium sulfate, sodium lauryl sulfate, polyvinylpyrrolidone or the polyphosphate sodium;
Further, obtain better invention effect for making the present invention, the dispersion solvent described in the step (1) can be a polar solvent, and described polar solvent is isopropyl alcohol, absolute ethyl alcohol, acetone or deionized water.
Further, obtain better invention effect for making the present invention, the mixing speed in the step (2) is changeed for per minute 1000-2000; The pH value of solution stops to add hydrazine hydrate when reaching 7.0-7.5; After stopping to add hydrazine hydrate, continuing to mix the time of stirring is 20-30 minute;
Further, obtain better invention effect for making the present invention, the time of placing the nano-complex particle that comprises Nano Silver in the step (3) is 8-12 hour; Baking temperature is 55-60 ℃;
Further, obtain better invention effect for making the present invention, the supersonic oscillations time is 15-25 minute in the step (4).
Effect of the present invention is: adopt method of the present invention preparation and the Nano Silver complex sol, granularity is 10-50nm, and epigranular, raw material is easy to get, and technology is simple, cost is low, realize easily suitability for industrialized production, and not only contain Nano Silver in this kind Nano Silver complex sol and also contain compositions such as nanometer copper and nanometer zinc, Synergistic antimicrobial better effects if, therefore application is more extensive, and effect is also better.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment:
Embodiment 1
(1) raw material in the present embodiment is as follows, in weight percent concentration:
A.0.2% 50 milliliters of liquor argenti nitratis ophthalmicuses
E.0.1% 70 milliliters of polyvinylpyrrolidones
F.0.01% 200 milliliters of hydrazine hydrates
G. isopropyl alcohol is 10 milliliters
In the present embodiment, silver nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.266: 0.7;
(2) be ready to the raw material A described in the step (1), add E again at normal temperature then, add pure water then, make liquor capacity reach 200 milliliters, add F at last, slowly adding hydrazine hydrate solution under the stirring, mixing speed is: per minute 500 changes; When reaching 6.5, the pH of solution value stops to add hydrazine hydrate solution.Then mixed solution is continued stirring and stop after 30 minutes, obtain nano silver particles;
(3) be that nano silver particles was placed after 10 hours with the product in the top step (2), then through the nano powder that separates, washs, 50 ℃ of dry backs obtain argentiferous;
(4) will be dispersed in the isopropyl alcohol 4 minutes through the nano powder of the drying that obtains after the step (3), supersonic oscillations 30 minutes promptly get nano silver colloidal sol.
Embodiment 2
(1) raw material in the present embodiment is as follows, in weight percent concentration:
A.0.2% 50 milliliters of liquor argenti nitratis ophthalmicuses
B.0.01% 10 milliliters of zinc nitrate solutions
E.0.1% 70 milliliters of sodium dodecyl sulfate solutions
F.0.01% 200 milliliters of hydrazine hydrates
G. absolute ethyl alcohol is 10 milliliters
In the present embodiment, silver nitrate, zinc nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.009: 0.266: 0.7;
(2) raw material A, the B described in the step (1) mixed at normal temperatures, and then add E, add pure water then, make liquor capacity reach 200 milliliters, add F at last, slowly adding hydrazine hydrate solution under the stirring, mixing speed is: per minute 500 changes; When the pH of solution value reaches 7.0, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 20 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly comprised Nano Silver was placed after 10 hours, then through the nano composite powder that separates, washs, 50 ℃ of dry backs obtain argentiferous, wherein, contain 90.2% silver, 9.8% zinc in the present embodiment, the average grain diameter of powder is 10nm;
(4) will be dispersed in the absolute ethyl alcohol 5 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 20 minutes promptly get the complex sol of Nano Silver.
Embodiment 3
(1) raw material in the present embodiment is as follows, in weight percent concentration:
A.0.2% 50 milliliters of liquor argenti nitratis ophthalmicuses
B.0.01% 10 milliliters of zinc nitrate solutions
C.0.001% 10 milliliters of iron nitrate solutions
E.0.1% 50 milliliters of polyvinylpyrrolidones, 20 milliliters of 0.1% sodium dodecyl sulfate solutions
F.0.01% 200 milliliters of hydrazine hydrates
G. isopropyl alcohol is 10 milliliters
In the present embodiment, silver nitrate, zinc nitrate, ferric nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.009: 0.007: 0.266: 0.7;
(2) raw material A, B, the C described in the step (1) mixed at normal temperatures, and then add E, add pure water then, make liquor capacity reach 200 milliliters, add F at last, slowly adding hydrazine hydrate solution under the stirring, mixing speed is: per minute 2000 changes; When the pH of solution value reaches 6.5, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 20 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly comprised Nano Silver was placed after 10 hours, then through the nano composite powder that separates, washs, 60 ℃ of dry backs obtain argentiferous, wherein, contain 90.1% silver, 9.8% zinc, 0.1% iron powder in the present embodiment, the average grain diameter of powder is 10nm;
(4) will be dispersed in the isopropyl alcohol 4 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 30 minutes promptly get the complex sol of Nano Silver.
Embodiment 4:
(1) raw material in the present embodiment is as follows, in weight percent concentration:
A.0.2% 50 milliliters of liquor argenti nitratis ophthalmicuses
B.0.01% 10 milliliters of zinc nitrate solutions
C.0.001% 10 milliliters of iron nitrate solutions
D.0.001% 10 milliliters of copper nitrate solutions
E.0.1% 50 milliliters of polyvinylpyrrolidones, 20 milliliters of 0.1% sodium dodecyl sulfate solutions
F.0.01% 200 milliliters of hydrazine hydrates
G. absolute ethyl alcohol is 10 milliliters
In the present embodiment, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.009: 0.007: 0.001: 0.266: 0.7;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, and then add E, add pure water then, make liquor capacity reach 200 milliliters, add F at last, slowly adding hydrazine hydrate solution under the stirring, mixing speed is: per minute 500 changes; When the pH of solution value reaches 6.5, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 30 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly comprised Nano Silver was placed after 10 hours, then through the nano composite powder that separates, washs, 50 ℃ of dry backs obtain argentiferous, wherein, contain the iron powder of 90% silver, 9.8% zinc, 0.1% bronze medal and 0.1% in the present embodiment, the average grain diameter of powder is 10nm;
(4) will be dispersed in the absolute ethyl alcohol 5 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 25 minutes promptly get the complex sol of Nano Silver.
Embodiment 5
(1) raw material in the present embodiment is as follows, in weight percent concentration:
A.0.8% 30 milliliters of liquor argenti nitratis ophthalmicuses
B.0.5% 15 milliliters of zinc nitrate solutions
C.0.5% 10 milliliters of iron nitrate solutions
D.0.001% 10 milliliters of copper nitrate solutions
E.0.5% 25 milliliters of polyvinylpyrrolidones, 20 milliliters of 0.5% sodium dodecyl sulfate solutions
F.0.04% 200 milliliters of hydrazine hydrates
G. absolute ethyl alcohol is 15 milliliters
In the present embodiment, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.28: 0.15: 0.004: 0.259: 1.15;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, and then add E, add deionized water then, make liquor capacity reach 200 milliliters, add F at last, add hydrazine hydrate solution under stirring, mixing speed is: per minute 3000 changes; When the pH of solution value reaches 7.0, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 10 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly contained Nano Silver was placed after 12 hours, then through the nano composite powder that separates, washs, 60 ℃ of dry backs obtain argentiferous, wherein, contain 80.2% silver in the present embodiment, 13.6% zinc, 6.1% iron and 0.1% bronze medal, the average grain diameter of powder is 16nm;
(4) will be dispersed in the absolute ethyl alcohol 5 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 25 minutes promptly get the complex sol of Nano Silver.
Embodiment 6
(1) raw material in the present embodiment is as follows, in weight percent concentration:
A.0.01% 20 milliliters of liquor argenti nitratis ophthalmicuses
B.0.005% 10 milliliters of zinc nitrate solutions
C.0.002% 10 milliliters of iron nitrate solutions
D.0.001% 10 milliliters of copper nitrate solutions
E.0.01% 20 milliliters of polyvinylpyrrolidones, 25 milliliters of 0.01% sodium dodecyl sulfate solutions
F.0.001% 200 milliliters of hydrazine hydrates
G. isopropyl alcohol is 0.15 milliliter
In the present embodiment, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.228: 0.07: 0.045: 0.664: 3.4;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, and then add E, add distilled water then, make liquor capacity reach 200 milliliters, add F at last, add hydrazine hydrate solution under stirring, mixing speed is: per minute 1000 changes; When the pH of solution value reaches 7.5, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 15 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly contained Nano Silver was placed after 6 hours, then through the nano composite powder that separates, washs, 60 ℃ of dry backs obtain argentiferous, wherein, contain 40.2% silver in the present embodiment, 30.6% zinc, 15.2% iron and 14% bronze medal, the average grain diameter of powder is 40nm;
(4) will be dispersed in the isopropyl alcohol 3 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 20 minutes promptly get the complex sol of Nano Silver.
Embodiment 7
(1) raw material that uses in the present embodiment is as follows, in weight percent concentration:
A.5% 50 milliliters of liquor argenti nitratis ophthalmicuses
B.0.1% 15 milliliters of zinc nitrate solutions
C.1.0% 15 milliliters of iron nitrate solutions
D.4% 10 milliliters of copper nitrate solutions
E.5% 20 milliliters of polyvinylpyrrolidones, 25 milliliters of 5% sodium dodecyl sulfate solutions
F.1.0% 200 milliliters of hydrazine hydrates
G. isopropyl alcohol is 160 milliliters
In the present embodiment, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.005: 0.042: 0.144: 0.267: 2.726;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, and then add E, add deionized water then, make liquor capacity reach 200 milliliters, add F at last, add hydrazine hydrate solution under stirring, mixing speed is: per minute 2000 changes; When the pH of solution value reaches 7.0, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 20 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly contained Nano Silver was placed after 8 hours, then through the nano composite powder that separates, washs, 55 ℃ of dry backs obtain argentiferous, wherein, contain 79.2% silver in the present embodiment, 10.6% zinc, 0.2% iron and 10.0% bronze medal, the average grain diameter of powder is 20nm;
(4) will be dispersed in the isopropyl alcohol 3 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 30 minutes promptly get the complex sol of Nano Silver.
Embodiment 8
(1) raw material that uses in the present embodiment is as follows, in weight percent concentration:
A.0.8% 30 milliliters of liquor argenti nitratis ophthalmicuses
B.0.5% 10 milliliters of zinc nitrate solutions
C.0.5% 15 milliliters of iron nitrate solutions
D.0.001% 10 milliliters of copper nitrate solutions
E.0.2% 10 milliliters of polyvinylpyrrolidones, 35 milliliters of 0.2% sodium dodecyl sulfate solutions
F.0.1% 200 milliliters of hydrazine hydrates
G. acetone is 20 milliliters
In the present embodiment, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1: 0.187: 0.225: 0.0038: 0.176: 2.825;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, and then add E, add pure water then, make liquor capacity reach 200 milliliters, add F at last, add hydrazine hydrate solution under stirring, mixing speed is: per minute 800 changes; When the pH of solution value reaches 6.8, stop to add hydrazine hydrate solution, then mixed solution is continued stirring and stop after 20 minutes, obtain comprising the nano-complex particle of Nano Silver;
(3) nano-complex particle that the product in the top step (2) is promptly contained Nano Silver was placed after 10 hours, then through the nano composite powder that separates, washs, 55 ℃ of dry backs obtain argentiferous, wherein, contain 78.2% silver in the present embodiment, 9.6% zinc, 9.1% iron and 3.1% bronze medal, the average grain diameter of powder is 28nm;
(4) will be dispersed in the acetone 5 minutes through the nano composite powder of the drying that obtains after the step (3), supersonic oscillations 30 minutes promptly get the complex sol of Nano Silver.
The present invention is illustrated with the illustrational embodiment of this paper, and the present invention also can implement with other ad hoc fashion or other particular form, and does not depart from main idea of the present invention or substantive characteristics.Therefore, the embodiment of description all should be considered as illustrative from any aspect but not be determinate.Scope of the present invention should be by additional claim explanation, and the intention of any and claim and the variation of scope equivalence also should be within the scope of the present invention.
Claims (10)
1, a kind of preparation method of Nano Silver complex sol comprises the steps:
(1) prepare following raw material:
A. weight percent concentration is the liquor argenti nitratis ophthalmicus of 0.01-5.0%
B. weight percent concentration is the 0.001-5.0% zinc nitrate solution
C. weight percent concentration is the 0.001-5.0% iron nitrate solution
D. weight percent concentration is the 0.001-5.0% copper nitrate solution
E. weight percent concentration is the 0.01-5.0% surfactant solution
F. weight percent concentration is the 0.001-1.0% hydrazine hydrate
G. dispersion solvent
Wherein, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is 1.0: 0.001-0.31: 0.001-0.48: 0.001-0.43: 0.001-1.0: 0.5-4.5;
(2) raw material A, B, C, the D described in the step (1) mixed at normal temperatures, add surfactant then, and then adding distilled water, pure water or deionized water dilute, add hydrazine hydrate and slowly stirring at last again, mixing speed is changeed for per minute 500-3000, when the pH of solution value reaches 6.5-7.5, stop to add hydrazine hydrate, continue then to mix and stirred 10-30 minute, obtain to comprise the nano-complex particle of Nano Silver at last;
(3) product of placing step (2) gained promptly comprises nano-complex particle 5-12 hour of Nano Silver, obtain to contain the nano composite powder of Nano Silver then through separation, washing, 50-60 ℃ dry back, wherein, the content of Nano Silver is 50-99.6%, and granularity is 10-100nm;
(4) will be dispersed in the dispersion solvent by the nano composite powder that step (3) obtain, supersonic oscillations 10-30 minute then, promptly obtain the Nano Silver complex sol.
2, the preparation method of a kind of Nano Silver complex sol as claimed in claim 1 is characterized in that: the surfactant described in the step (1) is one or more compositions in lauryl sodium sulfate, sodium lauryl sulfate, polyvinylpyrrolidone or the polyphosphate sodium.
3, the preparation method of a kind of Nano Silver complex sol as claimed in claim 1 or 2 is characterized in that: the dispersion solvent described in the step (1) is a polar solvent, and described polar solvent is isopropyl alcohol, absolute ethyl alcohol, acetone or deionized water.
4, the preparation method of a kind of Nano Silver complex sol as claimed in claim 3 is characterized in that: the raw material described in the step (1) is as follows:
A. weight percent concentration is the liquor argenti nitratis ophthalmicus of 0.01-3.0%
B. weight percent concentration is the zinc nitrate solution of 0.01-5.0%
C. weight percent concentration is the iron nitrate solution of 0.001-3.0%
D. weight percent concentration is the copper nitrate solution of 0.001-4.0%
E. weight percent concentration is the surfactant solution of 0.01-2.0%
F. weight percent concentration is the hydrazine hydrate of 0.001-0.9%
G. dispersion solvent
Wherein, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is: 1.0: 0.01-0.31: 0.001-0.29: 0.001-0.35: 0.001-0.4: 0.5-4.5.
5, the preparation method of a kind of Nano Silver complex sol as claimed in claim 4 is characterized in that: the raw material described in the step (1) is as follows:
A. weight percent concentration is the liquor argenti nitratis ophthalmicus of 0.01-2.0%
B. weight percent concentration is the zinc nitrate solution of 0.1-5.0%
C. weight percent concentration is the iron nitrate solution of 0.01-3.0%
D. weight percent concentration is the copper nitrate solution of 0.001-2.0%
E. weight percent concentration is the surfactant solution of 0.1-2.0%
F. weight percent concentration is the hydrazine hydrate of 0.001-0.6%
G. dispersion solvent
Wherein, silver nitrate, zinc nitrate, ferric nitrate, copper nitrate, surfactant, the mol ratio of hydrazine hydrate is 1.0: 0.1-0.30: 0.01-0.29: 0.001-0.18: 0.01-0.4: 0.5-2.7.
6, the preparation method of a kind of Nano Silver complex sol as claimed in claim 3 is characterized in that: the mixing speed in the step (2) is changeed for per minute 1000-2000.
7, the preparation method of a kind of Nano Silver complex sol as claimed in claim 3 is characterized in that: stop to add hydrazine hydrate when the pH value of solution reaches 7.0-7.5 in the step (2).
8, the preparation method of a kind of Nano Silver complex sol as claimed in claim 3 is characterized in that: in the step (2), after stopping to add hydrazine hydrate, continuing to mix the time of stirring is 20-30 minute.
9, the preparation method of a kind of Nano Silver complex sol as claimed in claim 3 is characterized in that: the time of placing the nano-complex particle that comprises Nano Silver in the step (3) is 8-12 hour; Baking temperature is 55-60 ℃.
10, the preparation method of a kind of Nano Silver complex sol as claimed in claim 3 is characterized in that: the supersonic oscillations time is 15-25 minute in the step (4).
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| CN107552069A (en) * | 2017-09-07 | 2018-01-09 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method of Research of Silver Copper Oxide Composite |
| CN108871659B (en) * | 2018-07-06 | 2020-11-24 | 山东大学 | Preparation method of colorimetric stress sensor based on Ag nano particle assembly |
| CN109819979A (en) * | 2019-03-15 | 2019-05-31 | 尚蒙科技无锡有限公司 | Nano silver copper bimetallic colloid/liquid of high anti-microbial property and preparation method thereof |
| CN112273396A (en) * | 2019-07-24 | 2021-01-29 | 陈信行 | Nano silver solvent |
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| CN1197708A (en) * | 1998-03-03 | 1998-11-04 | 浙江大学 | Preparation of nanometer silver-copper alloy powder |
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| CN1803351A (en) * | 2005-12-29 | 2006-07-19 | 黄德欢 | Preparation method of inorganic carried nanometer silver sol |
| CN1803350A (en) * | 2005-12-23 | 2006-07-19 | 西安交通大学 | Preparation method of colloidal silver nanometer granule |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197708A (en) * | 1998-03-03 | 1998-11-04 | 浙江大学 | Preparation of nanometer silver-copper alloy powder |
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN1709618A (en) * | 2005-07-08 | 2005-12-21 | 昆明理工大学 | Method for preparing nano or submicron silver powder |
| CN1803350A (en) * | 2005-12-23 | 2006-07-19 | 西安交通大学 | Preparation method of colloidal silver nanometer granule |
| CN1803351A (en) * | 2005-12-29 | 2006-07-19 | 黄德欢 | Preparation method of inorganic carried nanometer silver sol |
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