CN107127353B - Nano silver sol and preparation method thereof - Google Patents
Nano silver sol and preparation method thereof Download PDFInfo
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- CN107127353B CN107127353B CN201710359697.5A CN201710359697A CN107127353B CN 107127353 B CN107127353 B CN 107127353B CN 201710359697 A CN201710359697 A CN 201710359697A CN 107127353 B CN107127353 B CN 107127353B
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Abstract
The invention provides a preparation method of nano-silver sol, which comprises the steps of mixing a protective agent aqueous solution and a reducing agent aqueous solution, and then mixing the protective agent aqueous solution and a silver nitrate aqueous solution to obtain a primary mixed material; carrying out a first reduction reaction on the primary mixed material at 35-45 ℃ for 30-35 min to obtain a nano silver sol precursor; mixing the nano-silver sol precursor with a polyol aqueous solution to obtain a mixed material; and carrying out a second reduction reaction on the mixed material at 35-45 ℃ for 10-30 s to obtain the nano-silver sol. The preparation method provided by the invention has the advantages of simple steps, safety, environmental protection and low production cost; the prepared nano silver sol has small and uniform (10-20 nm) particle size distribution of nano silver particles and high stability, and is stored in a brown bottle at room temperature in a dark place for 6 months without flocculation and precipitation.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to nano silver sol and a preparation method thereof.
Background
Compared with corresponding macroscopic silver metal, the nano silver often shows remarkable and unique performances in the aspects of physics, chemistry and biology, such as surface enhanced Raman scattering, catalysis, data storage, biological and medical sensors, strong broad-spectrum antibacterial activity, no toxicity to human cells and the like. The nano silver has wide application prospect in the fields of antibacterial materials, high-efficiency catalysts, lubricants, light absorption materials, coatings, sensors, conductive slurry, high-performance electrode materials and the like, and becomes a research hotspot in the field of novel functional materials.
The performance of the nano silver strongly depends on physical characteristics of the nano silver particles such as appearance, size, stability and the like. The preparation method of nano silver reported in the literature at present mainly comprises two major types, namely a chemical method and a physical method, wherein the chemical method mainly comprises a chemical reduction method, an electrochemical reduction method and a photochemical reduction method. However, these methods all have certain disadvantages to different degrees, such as slow preparation speed by electrochemical reduction method, high concentration of protective agent, and deposition of more silver particles with large particle size on the cathode during the preparation process, which greatly increases the cost for preparing nano silver, and the prepared nano silver particles have wide particle size distribution and poor stability, which severely restricts the popularization and use; the photochemical reduction method has the advantages of slow reaction rate, small product amount prepared each time and unsuitability for industrial production; the reducing agents used in the chemical reduction method, such as sodium borohydride, hydrazine hydrate, formaldehyde and the like, have high toxicity, and the nano silver particles prepared by the reducing agents have large particle size and are unevenly distributed, so that the performance of the nano silver is greatly limited.
Disclosure of Invention
The invention aims to provide a nano silver sol and a preparation method thereof, and the preparation method provided by the invention has the advantages of simple steps, safety, environmental protection and low production cost; the prepared nano silver sol has small and uniform (10-20 nm) particle size distribution of nano silver particles and high stability, and is stored in a brown bottle at room temperature in a dark place for 6 months without flocculation and precipitation.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of nano silver sol, which comprises the following steps:
(1) mixing a protective agent aqueous solution and a reducing agent aqueous solution, and then mixing the protective agent aqueous solution and a silver nitrate aqueous solution to obtain a primary mixed material;
(2) carrying out a first reduction reaction on the primary mixed material in the step (1) at the temperature of 35-45 ℃ for 30-35 min to obtain a nano silver sol precursor;
(3) mixing the nano-silver sol precursor in the step (2) with a polyol aqueous solution to obtain a mixed material;
(4) and (4) carrying out a second reduction reaction on the mixed material in the step (3) at 35-45 ℃ for 10-30 s to obtain the nano silver sol.
Preferably, the mass concentration of silver nitrate in the primary mixed material in the step (1) is 0.08-0.12 mg/mL.
Preferably, the mass ratio of the silver nitrate, the protective agent and the reducing agent in the primary mixed material in the step (1) is 1: (4.5-5.5): (0.45-0.55).
Preferably, the protective agent comprises polyvinylpyrrolidone or polyethylene glycol.
Preferably, the polyvinylpyrrolidone has a number average molecular weight of 25000 to 35000.
Preferably, the number average molecular weight of the polyethylene glycol is 5500-7500.
Preferably, the reducing agent comprises N, N-dimethylethanolamine, triethanolamine or methyldiethanolamine.
Preferably, the mass concentration of the polyol in the mixed material in the step (3) is 0.013-0.017 mg/mL.
Preferably, the polyol comprises mannitol, glycerol or pentaerythritol.
The invention provides the nano-silver sol prepared by the preparation method in the technical scheme, wherein the particle size of nano-silver particles in the nano-silver sol is 10-20 nm.
The invention provides a preparation method of nano-silver sol, which comprises the steps of mixing a protective agent aqueous solution and a reducing agent aqueous solution, and then mixing the protective agent aqueous solution and a silver nitrate aqueous solution to obtain a primary mixed material; carrying out a first reduction reaction on the primary mixed material at 35-45 ℃ for 30-35 min to obtain a nano silver sol precursor; mixing the nano-silver sol precursor with a polyol aqueous solution to obtain a mixed material; and carrying out a second reduction reaction on the mixed material at 35-45 ℃ for 10-30 s to obtain the nano-silver sol. The preparation method provided by the invention has the advantages of simple steps, safety, environmental protection and low production cost, and can prepare the nano-silver sol at a lower temperature; the polyol is adopted for carrying out the second reduction reaction, so that the reaction rate can be higher at a lower temperature, and the reaction time can be effectively shortened; the prepared nano silver sol has small and uniform (10-20 nm) particle size distribution of nano silver particles and high stability, and is stored in a brown bottle at room temperature in a dark place for 6 months without flocculation and precipitation.
Drawings
FIG. 1 is a UV-Vis spectrum of nano-silver sol prepared in example 1 and comparative example 1 of the present invention; wherein, (1) is the ultraviolet-visible spectrum curve of the nano silver sol prepared in the embodiment 1 of the invention, and (2) is the ultraviolet-visible spectrum curve of the nano silver sol prepared in the comparative example 1 of the invention;
FIG. 2 is a transmission electron microscope image of the nano-silver sol prepared in example 1 of the present invention;
fig. 3 is a transmission electron microscope image of the nano silver sol prepared in comparative example 1 of the present invention.
Detailed Description
The invention provides a preparation method of nano silver sol, which comprises the following steps:
(1) mixing a protective agent aqueous solution and a reducing agent aqueous solution, and then mixing the protective agent aqueous solution and a silver nitrate aqueous solution to obtain a primary mixed material;
(2) carrying out a first reduction reaction on the primary mixed material in the step (1) at the temperature of 35-45 ℃ for 30-35 min to obtain a nano silver sol precursor;
(3) mixing the nano-silver sol precursor in the step (2) with a polyol aqueous solution to obtain a mixed material;
(4) and (4) carrying out a second reduction reaction on the mixed material in the step (3) at 35-45 ℃ for 10-30 s to obtain the nano silver sol.
The invention mixes the aqueous solution of the protective agent and the aqueous solution of the reducing agent, and then mixes the aqueous solution of the protective agent and the aqueous solution of the silver nitrate to obtain the primary mixed material. In the invention, the protective agent, the reducing agent and the silver nitrate are used in the form of aqueous solution, which is beneficial to preparing the nano-silver sol with good stability. In the present invention, the water in the aqueous protective agent solution, the aqueous reducing agent solution and the aqueous silver nitrate solution is preferably deionized water.
In the present invention, the mixing of the aqueous protecting agent solution and the aqueous reducing agent solution, and the mixing of the resulting mixture with the aqueous silver nitrate solution are preferably performed under stirring conditions. In the present invention, the stirring is preferably magnetic stirring; the speed of the magnetic stirring is independently preferably 300-400 rpm, more preferably 330-370 rpm, and most preferably 350 rpm.
In the invention, the mass concentration of silver nitrate in the initial mixed material is preferably 0.08-0.12 mg/mL, more preferably 0.09-0.11 mg/mL, and most preferably 0.10 mg/mL. In the invention, the mass ratio of the silver nitrate, the protective agent and the reducing agent in the initial mixed material is preferably 1: (4.5-5.5): (0.45 to 0.55), more preferably 1: (4.8-5.2): (0.48 to 0.52), most preferably 1: 5: 0.5.
in the present invention, the protective agent preferably includes polyvinylpyrrolidone or polyethylene glycol, more preferably polyvinylpyrrolidone. In the present invention, the polyvinylpyrrolidone has a number average molecular weight of preferably 25000 to 35000, more preferably 27000 to 33000, and most preferably 29000 to 31000. In the present invention, the number average molecular weight of the polyethylene glycol is preferably 5500 to 7500, and more preferably 6000 to 7000. In the invention, the protective agent can reduce the surface energy of the generated nano silver particles and prevent the nano silver particles from agglomerating and precipitating.
In the present invention, the reducing agent preferably includes N, N-dimethylethanolamine, triethanolamine or methyldiethanolamine, and more preferably N, N-dimethylethanolamine. In the present invention, the reducing agent is capable of reducing silver ions to atomic silver; on the other hand, the reducing agent can be coated on the surface of the nano silver particles to prevent the nano silver particles from agglomerating and precipitating, the better the symmetry of the reducing agent molecular structure is, and the tighter the coating is, so that the resistance of agglomeration of the nano silver particles can be increased.
In the present invention, the initial mixture is preferably obtained by the following steps:
under the condition of stirring, mixing an original reducing agent aqueous solution, an original protective agent aqueous solution and water, and then mixing with an original silver nitrate aqueous solution to obtain a primary mixed material.
In the invention, the mass concentration of the original reducing agent aqueous solution is preferably 1.8-2.2 mg/mL, more preferably 1.9-2.1 mg/mL, and most preferably 2.0 mg/mL. In the invention, the mass concentration of the original protective agent aqueous solution is preferably 18.0-22.0 mg/mL, more preferably 19.0-21.0 mg/mL, and most preferably 20.0 mg/mL. In the invention, the mass concentration of the original silver nitrate aqueous solution is preferably 1.8-2.2 mg/mL, more preferably 1.9-2.1 mg/mL, and most preferably 2.0 mg/mL.
In the embodiment of the invention, the appropriate amount of water is selected according to the mass concentrations of the original reducing agent aqueous solution, the original protective agent aqueous solution and the original silver nitrate aqueous solution and the mass concentrations of the reducing agent, the protective agent and the silver nitrate in the primary mixed material.
In the embodiment of the present invention, the water in the original reducing agent aqueous solution, the original protective agent aqueous solution and the original silver nitrate aqueous solution is preferably deionized water; the water is preferably deionized water.
After the primary mixed material is obtained, carrying out a first reduction reaction on the primary mixed material at the temperature of 35-45 ℃ for 30-35 min to obtain a nano silver sol precursor. In the present invention, the first reduction reaction is preferably carried out under stirring; the stirring is preferably magnetic stirring; the speed of the magnetic stirring is preferably 300-400 rpm, more preferably 330-370 rpm, and most preferably 350 rpm. In the invention, the temperature of the first reduction reaction is 35-45 ℃, preferably 38-43 ℃, and more preferably 40-42 ℃. In the invention, the time of the first reduction reaction is 30-35 min, preferably 31-34 min, and more preferably 32-33 min.
After the first reduction reaction is finished, the obtained nano silver sol precursor is mixed with a polyalcohol aqueous solution to obtain a mixed material. In the present invention, the mixing is preferably performed under stirring conditions, and the stirring is preferably magnetic stirring; the speed of the magnetic stirring is preferably 300-400 rpm, more preferably 330-370 rpm, and most preferably 350 rpm. In the invention, the mass concentration of the polyhydric alcohol in the mixed material is preferably 0.013-0.017 mg/mL, more preferably 0.014-0.016 mg/mL, and most preferably 0.015 mg/mL. In the invention, the mass concentration of the polyhydric alcohol aqueous solution is preferably 1.8-2.2 mg/mL, more preferably 1.9-2.1 mg/mL, and most preferably 2.0 mg/mL. In the embodiment of the invention, the adding amount of the polyol aqueous solution is selected according to the mass concentration of the polyol aqueous solution, the volume of the nano silver sol precursor and the mass concentration of the polyol in the mixed material. In the embodiment of the present invention, the water in the polyol aqueous solution is preferably deionized water.
In the present invention, the polyol preferably includes mannitol, glycerol or pentaerythritol, and more preferably mannitol.
After the mixed material is obtained, carrying out a second reduction reaction on the mixed material at 35-45 ℃ for 10-30 s to obtain the nano silver sol. In the present invention, the second reduction reaction is preferably carried out under stirring; the stirring is preferably magnetic stirring; the speed of the magnetic stirring is preferably 300-400 rpm, more preferably 330-370 rpm, and most preferably 350 rpm. In the invention, the temperature of the second reduction reaction is 35-45 ℃, preferably 38-43 ℃, and more preferably 40-42 ℃. In the invention, the time of the second reduction reaction is 10-30 s, preferably 15-25 s, and more preferably 18-22 s.
In the invention, the polyol contains a plurality of hydroxyl groups, has reducibility, can form a synergistic effect with a reducing agent, accelerates the reduction reaction rate, is also favorable for enabling the particle size of the formed nano silver particles to be more uniform, and improves the content of the nano silver particles in the nano silver sol and the stability of the nano silver sol.
The invention provides the nano-silver sol prepared by the preparation method in the technical scheme, wherein the particle size of nano-silver particles in the nano-silver sol is 10-20 nm. In the invention, the nano silver sol is golden yellow transparent sol. In the present invention, the nano silver sol is preferably sealed in a brown reagent bottle and stored in a dark place.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Under the condition that the magnetic stirring speed is 350rpm, mixing 36mL of deionized water, 1mL of a 1mLN, N-dimethylethanolamine aqueous solution (the mass concentration is 2mg/mL) and 1mL of a polyvinylpyrrolidone aqueous solution (the mass concentration is 20mg/mL), and then mixing with 2mL of a silver nitrate aqueous solution (the mass concentration is 2mg/mL) to obtain a primary mixed material;
(2) under the condition that the magnetic stirring speed is 350rpm, carrying out a first reduction reaction on the primary mixed material in the step (1) at 35 ℃ for 30min to obtain a nano silver sol precursor;
(3) under the condition that the magnetic stirring speed is 350rpm, mixing the nano-silver sol precursor in the step (2) with 300 mu L of mannitol aqueous solution (the mass concentration is 2mg/mL) to obtain a mixed material;
(4) and (3) carrying out a second reduction reaction on the mixture obtained in the step (3) at 35 ℃ for 30s under the condition that the magnetic stirring speed is 350rpm to obtain nano silver sol, and sealing in a brown reagent bottle for light-shielding storage.
Comparative example 1
The nano silver sol was prepared according to the raw material ratio and method of example 1 without adding mannitol aqueous solution.
The nano silver sols prepared in example 1 and comparative example 1 were subjected to uv-vis spectroscopy, and the results are shown in fig. 1; in fig. 1, (1) is a uv-vis spectrum curve of the nano silver sol prepared in example 1, and (2) is a uv-vis spectrum curve of the nano silver sol prepared in comparative example 1. Generally, the content of the nano silver particles in the nano silver sol can be judged according to the absorbance and the maximum absorption wavelength of the ultraviolet-visible spectrum, and the smaller the maximum absorption wavelength is, the larger the absorbance is, the higher the content of the nano silver particles in the nano silver sol is. As can be seen from fig. 1, the maximum absorption wavelengths of the curve (1) and the curve (2) are substantially the same, but the absorbance of the curve (1) is much greater than that of the curve (2), which indicates that the content of the nano silver particles in the nano silver sol can be increased by adding mannitol. Meanwhile, the curve (1) has better peak shape symmetry and narrower half-peak width, which shows that the particle size distribution of the nano silver particles in the nano silver sol obtained by adding mannitol is more uniform.
The nano silver sols prepared in example 1 and comparative example 1 were subjected to transmission electron microscopy analysis, and the results are shown in fig. 2 and 3; fig. 2 is a transmission electron microscope image of the nano silver sol prepared in example 1, and fig. 3 is a transmission electron microscope image of the nano silver sol prepared in comparative example 1. As can be seen from fig. 2 and 3, the shape and the size of the nano silver particles in fig. 2 are more uniformly distributed, and the particle size of the nano silver particles is 10-20 nm, which indicates that the particle size distribution of the nano silver particles in the nano silver sol is more uniform after the mannitol is added, and thus the application range of the nano silver sol is greatly widened.
Example 2
(1) Under the condition that the magnetic stirring speed is 300rpm, mixing 36mL of deionized water, 1mL of a 1mLN, N-dimethylethanolamine aqueous solution (the mass concentration is 2mg/mL) and 1mL of a polyvinylpyrrolidone aqueous solution (the mass concentration is 20mg/mL), and then mixing with 2mL of a silver nitrate aqueous solution (the mass concentration is 2mg/mL) to obtain a primary mixed material;
(2) under the condition that the magnetic stirring speed is 300rpm, carrying out a first reduction reaction on the primary mixed material in the step (1) at 40 ℃ for 35min to obtain a nano silver sol precursor;
(3) under the condition that the magnetic stirring speed is 300rpm, mixing the nano-silver sol precursor in the step (2) with 300 mu L of mannitol aqueous solution (the mass concentration is 2mg/mL) to obtain a mixed material;
(4) and (3) carrying out a second reduction reaction on the mixture obtained in the step (3) at 40 ℃ for 20s under the condition that the magnetic stirring speed is 300rpm to obtain nano silver sol, and sealing in a brown reagent bottle for light-shielding storage.
Example 3
(1) Under the condition that the magnetic stirring speed is 400rpm, mixing 36mL of deionized water, 1mL of a 1mLN, N-dimethylethanolamine aqueous solution (the mass concentration is 2mg/mL) and 1mL of a polyvinylpyrrolidone aqueous solution (the mass concentration is 20mg/mL), and then mixing with 2mL of a silver nitrate aqueous solution (the mass concentration is 2mg/mL) to obtain a primary mixed material;
(2) under the condition that the magnetic stirring speed is 400rpm, carrying out a first reduction reaction on the primary mixed material in the step (1) at 45 ℃ for 30min to obtain a nano silver sol precursor;
(3) under the condition that the magnetic stirring speed is 400rpm, mixing the nano-silver sol precursor in the step (2) with 300 mu L of mannitol aqueous solution (the mass concentration is 2mg/mL) to obtain a mixed material;
(4) and (3) carrying out a second reduction reaction on the mixture obtained in the step (3) at 45 ℃ for 10s under the condition that the magnetic stirring speed is 400rpm to obtain nano silver sol, and sealing in a brown reagent bottle for light-shielding storage.
According to the embodiment, the preparation method provided by the invention has the advantages of simple steps, safety, environmental protection and low production cost; the prepared nano silver sol has small and uniform (10-20 nm) particle size distribution of nano silver particles and high stability, and is stored in a brown bottle at room temperature in a dark place for 6 months without flocculation and precipitation.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A preparation method of nano silver sol comprises the following steps:
(1) mixing a protective agent aqueous solution and a reducing agent aqueous solution, and then mixing the protective agent aqueous solution and a silver nitrate aqueous solution to obtain a primary mixed material; the mass concentration of silver nitrate in the primary mixed material is 0.08-0.12 mg/mL, and the mass ratio of the silver nitrate, the protective agent and the reducing agent in the primary mixed material is 1: (4.5-5.5): (0.45-0.55); the reducing agent comprises N, N-dimethylethanolamine, triethanolamine or methyldiethanolamine;
(2) carrying out a first reduction reaction on the primary mixed material in the step (1) at the temperature of 35-45 ℃ for 30-35 min to obtain a nano silver sol precursor;
(3) mixing the nano-silver sol precursor in the step (2) with a polyol aqueous solution to obtain a mixed material; the mass concentration of the polyhydric alcohol in the mixed material is 0.013-0.017 mg/mL; the polyhydric alcohol comprises mannitol, glycerol or pentaerythritol;
(4) and (4) carrying out a second reduction reaction on the mixed material in the step (3) at 35-45 ℃ for 10-30 s to obtain the nano silver sol.
2. The method of claim 1, wherein the protective agent comprises polyvinylpyrrolidone or polyethylene glycol.
3. The method according to claim 2, wherein the polyvinylpyrrolidone has a number average molecular weight of 25000 to 35000.
4. The method according to claim 2, wherein the polyethylene glycol has a number average molecular weight of 5500 to 7500.
5. The nano silver sol prepared by the preparation method of any one of claims 1 to 4, wherein the particle size of nano silver particles in the nano silver sol is 10 to 20 nm.
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