CN114367674B - Silver powder preparation method - Google Patents
Silver powder preparation method Download PDFInfo
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- CN114367674B CN114367674B CN202210282806.9A CN202210282806A CN114367674B CN 114367674 B CN114367674 B CN 114367674B CN 202210282806 A CN202210282806 A CN 202210282806A CN 114367674 B CN114367674 B CN 114367674B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention discloses a preparation method of silver powder, wherein a liquid phase reduction method is adopted in the scheme, silver nitrate and a reducing agent are adopted according to the main principle, and a certain amount of aqueous dispersant or oily dispersant is added, so that the silver powder with certain dispersibility is obtained; the method can be applied to any method for preparing the silver powder by using the water-based dispersing agent, can realize the complete sedimentation of the silver powder, and has higher practicability because the organic residue on the surface of the obtained silver powder is more than 0.3 percent lower than that of the silver powder without the method.
Description
Technical Field
The invention relates to the technical field of silver powder preparation, in particular to a preparation method of silver powder.
Background
The existing silver powder preparation method generally adopts a liquid phase reduction method, in order to improve the dispersibility of the silver powder, a certain amount of water-based or oil-based dispersing agent is generally added into the silver powder, and the actual preparation process mainly adopts the water-based dispersing agent as a main material because the water-based dispersing agent can obtain the silver powder with high dispersibility and uniform particle size compared with the oil-based dispersing agent.
When an aqueous dispersant is used, the amount of the dispersant is often large in order to obtain a silver powder having high dispersibility, but when the amount of the dispersant is increased, the reaction solution using water as a solvent takes a gel state, which causes the silver powder to float in a large amount in water and not settle after the reduction is completed. Even if a certain variety of flocculating agents are used for settling, the organic residue ratio on the surface of the silver powder is high, and the use performance of the silver powder in the slurry at the later stage is influenced.
In view of the above situation, the present application discloses a method for preparing silver powder, so as to solve the technical problem.
Disclosure of Invention
The present invention is directed to a method for preparing silver powder to solve the above problems of the background art.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for preparing silver powder comprises the following steps:
(1) taking deionized water and silver nitrate, uniformly stirring, adding a dispersing agent, and stirring to a dissolved state at 25-35 ℃ to obtain a solution A;
taking deionized water and a reducing agent, uniformly mixing, adding a dispersing agent, and stirring at 30-35 ℃ to a dissolved state to obtain a solution B;
(2) adding the solution B into the solution A, and reacting completely at 50-60 ℃ to obtain a suspension C;
(3) and adding alkali liquor into the suspension C to adjust the pH to 8-14, heating to 65-90 ℃, keeping the temperature and stirring for 0.5-2h, collecting silver powder after stirring, washing, performing suction filtration and drying to obtain a finished product.
In a more optimized scheme, in the step (1), the dispersing agent is any one or more of gelatin, Arabic gum and polyvinylpyrrolidone; the reducing agent is any one or more of ascorbic acid, formaldehyde, hydrazine hydrate and hydrogen peroxide.
In the optimized scheme, in the step (3), the alkali liquor is any one or more of sodium hydroxide, potassium hydroxide and a salt solution containing hydroxide radical; the alkali liquor which is commonly used in the actual processing is sodium hydroxide solution with the concentration of 50 percent; in the step (2), the solution B is added to the solution A at a rate of 2-3L/min.
In an optimized scheme, the concentration of the silver nitrate is 0.5mol/L, and the mass ratio of the reducing agent to the silver nitrate is (1-4): 1. the preferable scheme is that the mass ratio of the reducing agent to the silver nitrate is 1: 1.
according to an optimized scheme, in the step (1), the dispersing agent is a mixture of N-alkyl benzotriazole and benzotriazole, and the mass ratio of the N-alkyl benzotriazole to the benzotriazole is (3-4): 1.
according to an optimized scheme, the preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 20-30min, adding sodium hydroxide, stirring at 50-60 deg.C until completely dissolved, adding bromohexadecane, stirring for reaction for 20-24h, distilling under reduced pressure to remove solvent, washing with deionized water at 70-75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
In an optimized scheme, the magnetic field intensity is 20-30mT when the magnetic field is applied in the steps (1) and (2).
According to an optimized scheme, the specific steps in the step (3) are as follows: adding alkali liquor into the suspension C, adjusting the pH to 9, adding cleaning solution, performing ultrasonic dispersion for 20-30min, stirring for 30-40min, continuously adding alkali liquor to adjust the pH to 14, heating to 70-75 ℃, keeping the temperature, stirring for 1-2h, collecting silver powder after stirring, washing, performing suction filtration, and drying to obtain a finished product.
In an optimized scheme, the cleaning solution is a polyhydroxy polyamine chelating agent.
In the optimized scheme, in the step (3), after the silver powder is collected after stirring, the silver powder is mixed with an ethanol solution, ultrasonic dispersion is carried out for 5-10min, the mixture is under UV illumination in the ultrasonic dispersion process, and the illumination intensity is 200-2Then washing with deionized water, filtering, and drying to obtain the final product.
Compared with the prior art, the invention has the following beneficial effects:
the application discloses a preparation method of silver powder, wherein a liquid phase reduction method is adopted in the scheme, silver nitrate and a reducing agent are adopted according to the main principle, and a certain amount of a water-based dispersing agent or an oil-based dispersing agent is added, so that the silver powder with certain dispersibility is obtained, the water-based dispersing agent is generally gelatin, Arabic gum, polyvinylpyrrolidone and the like, the oil-based dispersing agent is generally saturated fatty acid, unsaturated fatty acid and the like, in order to ensure that the silver powder with high dispersibility and uniform particle size can be obtained, the water-based dispersing agent is adopted in the application, meanwhile, the reducing agent is any one or more of ascorbic acid, formaldehyde, hydrazine hydrate and hydrogen peroxide, and after the reduction reaction is finished, alkali liquor is continuously added, so that the pH value of a suspension C is adjusted to 8-14. The system contains a large amount of hydroxide ions and has strong basicity, and the structure of the dispersing agent can be damaged by exerting a synergistic effect through heating treatment, so that the dissociation effect is achieved, the reaction liquid is prevented from being in a gel state, and the silver powder can be completely settled as soon as possible; the process treatment can effectively reduce the organic residues on the surface of the silver powder and greatly improve the service performance of the silver powder.
On the basis of the scheme, the dispersing agent is further improved, the scheme adopts the mixture of N-alkyl benzotriazole and benzotriazole as the dispersing agent, and the extra-nuclear electron arrangement of silver shows that silver atoms have empty tracks and can coordinate with lone-pair electrons of the N-alkyl benzotriazole and the benzotriazole to form coordinate bonds, so that the agglomeration of silver particles is hindered through the steric hindrance effect, and the dispersion of the silver powder is realized; compared with the conventional dispersing agent, the dispersing agent is prepared by mixing N-alkyl benzotriazole and benzotriazole, and the long-chain alkyl in the N-alkyl benzotriazole is introduced, so that the dispersing performance of the silver powder can be effectively improved, the particle size and uniformity of the silver powder are improved, and the service performance of the subsequent silver powder is improved. Meanwhile, the benzotriazole and the N-alkyl benzotriazole have excellent solubility in the concentrated alkali, so that the concentrated alkali can be conveniently added in the subsequent steps for dissociation, and the floating condition of the silver powder is avoided.
Meanwhile, in actual operation, the fact that the silver powder has excellent dispersing effect when the N-alkyl benzotriazole and the benzotriazole are mixed to be used as the dispersing agent is found, but organic residues on the surface of the silver powder are high after the subsequent concentrated alkali dissociation is used for assisting the degradation of the silver powder, so that the subsequent silver powder is influenced; in order to solve the technical problem, the cleaning solution is purposefully introduced in the dissociation step and is a polyhydroxy polyamine chelating agent, ethylenediaminetetraacetic acid tetra (tetrahydroxyethyl ethylenediamine) is used as the cleaning solution, the pH value is adjusted to 9, the stability of the dispersing agent matched with the surface of the silver powder begins to decline in an alkaline environment, the cleaning solution is competitively adsorbed by the dispersing agent by utilizing the strong chelating capacity of the cleaning solution, the pH value is adjusted to 14 by alkali liquor, the cleaning solution is matched with the dissociation action of concentrated alkali, the sedimentation of the silver powder is realized, the organic residue on the surface of the silver powder is greatly reduced, and the subsequent use effect of the silver powder is ensured.
Meanwhile, after the silver powder is collected after stirring, the silver powder is mixed with an ethanol solution, and the mixture is subjected to ultrasonic dispersion for 5-10min, wherein the mixture is under UV illumination in the ultrasonic dispersion process, and the illumination intensity is 200-2Washing with deionized water, filtering, and drying to obtain the final product; the purpose of this step is to further remove organic residues from the surfaceRemoving to ensure the conductive effect of the silver powder and avoid influencing the subsequent use of the silver powder; meanwhile, in order to ensure the dispersion performance, the step has higher requirements on process parameters, and is limited to ultrasonic dispersion for 5-10min, wherein the irradiation intensity is 200-300 muW/cm under UV irradiation in the ultrasonic dispersion process2"; ensuring the comprehensive effect of the silver powder.
In the silver powder preparation process, an external magnetic field is introduced, under the action of the external magnetic field, the coordination effect between the dispersing agent and the silver powder is more obvious, and the dispersibility of the silver powder is improved more obviously.
The invention discloses a preparation method of silver powder, which has simple process steps and appropriate process parameters, can be applied to any preparation method of silver powder using a water-based dispersant, can realize the complete sedimentation of the silver powder, and has higher practicability because the organic residue on the surface of the obtained silver powder is lower than that of the silver powder not using the method by more than 0.3 percent.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a scanning electron micrograph of the silver powder prepared in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 25 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 30 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 65 ℃, keeping the temperature and stirring for 0.5h, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
Example 2:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 32 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 34 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 72 ℃, keeping the temperature and stirring for 1.5h, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
Example 3:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 35 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 35 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 3L/min, and completely reacting at 60 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 75 ℃, keeping the temperature and stirring for 2 hours, after the supernatant is clarified, extracting the supernatant, collecting silver powder, washing, filtering, and drying to obtain a finished product.
Comparative example 1:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of gelatin after uniformly stirring, and stirring to a dissolved state at 32 ℃ to obtain a solution A;
taking 60L of deionized water and 4Kg of ascorbic acid, uniformly mixing, adding 360g of gelatin, and stirring at 34 ℃ until the gelatin is dissolved to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 72 ℃, keeping the temperature and stirring for 1.5h, after the supernatant is clarified, extracting the supernatant, collecting silver powder, washing, filtering, and drying to obtain a finished product.
Comparative example 2:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, uniformly stirring, adding a mixture of 250g of Arabic gum and gelatin, and stirring at 32 ℃ to a dissolved state to obtain a solution A;
taking 60L of deionized water and hydrazine hydrate, preparing 60% hydrazine hydrate aqueous solution, adding 360g of a mixture of Arabic gum and gelatin, and stirring at 34 ℃ to a dissolved state to obtain solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 72 ℃, keeping the temperature and stirring for 1.5h, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
Comparative example 3:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 32 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 34 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C; and extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
Comparative example 4:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 32 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 34 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C;
(3) and taking the suspension C, heating to 72 ℃, keeping the temperature and stirring for 1.5h, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
Comparative example 5:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 32 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 34 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, stirring for 1.5h, after the supernatant is clarified, extracting the supernatant, collecting silver powder, washing, carrying out suction filtration and drying to obtain a finished product.
Comparative example 6:
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 32 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 34 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2.5L/min, and completely reacting at 55 ℃ to obtain a suspension C;
(3) and adding stearic acid into the suspension C, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
The performance parameters of the silver powder tested are shown in the following table:
example 4: example 4 an externally applied magnetic field was introduced on the basis of example 1.
A method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of Arabic gum after uniformly stirring, and stirring to a dissolved state at 25 ℃ to obtain a solution A;
uniformly mixing 60L of deionized water and 4Kg of ascorbic acid, adding 360g of Arabic gum, and stirring at 30 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 65 ℃, keeping the temperature and stirring for 0.5h, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
The magnetic field intensity is 20mT when the magnetic material is prepared in the steps (1) and (2) in an external magnetic field.
The performance parameters of the silver powder are detected as follows: d10=0.46, D50=1.07, D90=2.90, D100=5.64, tap density 6.18, specific surface area 0.79, organic residue 0.58%; the dispersibility is high.
Example 5: embodiment 5, the dispersant is changed on the basis of embodiment 1, in embodiment 5, the dispersant is a mixture of N-alkyl benzotriazole and benzotriazole, and the mass ratio of the N-alkyl benzotriazole to the benzotriazole is 3: 1.
a method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of dispersant after uniformly stirring, and stirring to a dissolved state at 25 ℃ to obtain a solution A;
taking 60L of deionized water and 4Kg of ascorbic acid, uniformly mixing, adding 360g of dispersing agent, and stirring at 30 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C to adjust the pH value to 14, heating to 65 ℃, keeping the temperature and stirring for 0.5h, after the supernatant is clarified, extracting the supernatant, collecting the silver powder, washing, filtering, and drying to obtain a finished product.
The preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 30min, adding sodium hydroxide, stirring at 60 deg.C until completely dissolved, adding bromohexadecane, stirring for 24h, distilling under reduced pressure to remove solvent, washing with deionized water at 75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
The performance parameters of the silver powder are detected as follows: d10=0.51, D50=1.10, D90=2.87, D100=5.70, tap density 6.19, specific surface area 0.77, organic residue 0.57%; the dispersibility was high, and the dispersing effect was excellent as compared with example 1.
Example 6: example 6 a cleaning solution was introduced on the basis of example 5.
A method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of dispersant after uniformly stirring, and stirring to a dissolved state at 25 ℃ to obtain a solution A;
taking 60L of deionized water and 4Kg of ascorbic acid, uniformly mixing, adding 360g of dispersing agent, and stirring at 30 ℃ to a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C, adjusting the pH value to 9, adding a cleaning solution, performing ultrasonic dispersion for 20min, stirring for 30min, continuously adding a 50% sodium hydroxide solution to adjust the pH value to 14, heating to 70 ℃, keeping the temperature, stirring for 2h, collecting silver powder after stirring, washing, performing suction filtration, and drying to obtain a finished product. The cleaning solution is polyhydroxy polyamine chelating agent (Tianjin crystal mountain microelectronic material Co., Ltd.).
The preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 30min, adding sodium hydroxide, stirring at 60 deg.C until completely dissolved, adding bromohexadecane, stirring for 24h, distilling under reduced pressure to remove solvent, washing with deionized water at 75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
The performance parameters of the silver powder are detected as follows: d10=0.54, D50=1.11, D90=2.93, D100=5.72, tap density 6.20, specific surface area 0.76, organic residue 0.51%; the dispersibility was high, and the dispersing effect was excellent as compared with example 5.
Example 7: example 7 cleaning solution was introduced on the basis of example 5, and parameters were adjusted
The preparation method of the silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of dispersing agent after uniformly stirring, and stirring at 25 ℃ to a dissolved state to obtain a solution A;
taking 60L of deionized water and 4Kg of ascorbic acid, uniformly mixing, adding 360g of dispersing agent, and stirring at 30 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; and adding a 50% sodium hydroxide solution into the suspension C, adjusting the pH value to 9, adding a cleaning solution, performing ultrasonic dispersion for 30min, stirring for 40min, continuously adding a 50% sodium hydroxide solution to adjust the pH value to 14, heating to 75 ℃, keeping the temperature, stirring for 1h, collecting silver powder after stirring, washing, performing suction filtration, and drying to obtain a finished product. The cleaning solution is polyhydroxy polyamine chelating agent (Tianjin crystal mountain microelectronic material Co., Ltd.).
The preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 30min, adding sodium hydroxide, stirring at 60 deg.C until completely dissolved, adding bromohexadecane, stirring for 24h, distilling under reduced pressure to remove solvent, washing with deionized water at 75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
The silver powder prepared in example 7 had a surface organic residue of 0.48%; the dispersibility was high, and the dispersing effect was excellent as compared with example 5.
Example 8: example 8 introduction of UV light illumination on the basis of example 6
A method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of dispersant after uniformly stirring, and stirring to a dissolved state at 25 ℃ to obtain a solution A;
taking 60L of deionized water and 4Kg of ascorbic acid, uniformly mixing, adding 360g of dispersing agent, and stirring at 30 ℃ to be in a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; adding 50% sodium hydroxide solution into the suspension C, adjusting pH to 9, adding cleaning solution, ultrasonically dispersing for 20min, stirring for 30min, continuously adding 50% sodium hydroxide solution to adjust pH to 14, heating to 70 deg.C, stirring for 2h, collecting silver powder after stirring, mixing the silver powder with ethanol solution, ultrasonically dispersing for 5min under UV light with illumination intensity of 300 μ W/cm during ultrasonic dispersion2Then washing with deionized water, filtering, and drying to obtain the final product. The cleaning solution is polyhydroxy polyamine chelating agent (Tianjin crystal mountain microelectronic material Co., Ltd.).
The preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 30min, adding sodium hydroxide, stirring at 60 deg.C until completely dissolved, adding bromohexadecane, stirring for 24h, distilling under reduced pressure to remove solvent, washing with deionized water at 75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
The silver powder prepared in example 8 had a surface organic residue of 0.46%; the dispersibility is high.
Example 9: example 9 UV illumination was performed on the basis of example 6 and UV illumination parameters were adjusted.
A method for preparing silver powder comprises the following steps:
(1) taking 60L of deionized water and 4Kg of silver nitrate, wherein the concentration of the silver nitrate is 0.5mol/L, adding 250g of dispersant after uniformly stirring, and stirring to a dissolved state at 25 ℃ to obtain a solution A;
taking 60L of deionized water and 4Kg of ascorbic acid, uniformly mixing, adding 360g of dispersing agent, and stirring at 30 ℃ to a dissolved state to obtain a solution B;
(2) taking the solution B, adding the solution B into the solution A at the speed of 2L/min, and completely reacting at 50 ℃ to obtain a suspension C;
(3) taking 24kg of sodium hydroxide, and preparing into 50% sodium hydroxide solution; adding 50% sodium hydroxide solution into the suspension C, adjusting the pH value to 9, adding cleaning solution, performing ultrasonic dispersion for 20min, stirring for 30min, continuously adding 50% sodium hydroxide solution to adjust the pH value to 14, heating to 70 ℃, keeping the temperature and stirring for 2h, collecting silver powder after stirring, mixing the silver powder with ethanol solution after stirring, performing ultrasonic dispersion for 10min, and performing UV illumination under the illumination intensity of 200 mu W/cm in the ultrasonic dispersion process2Then washing with deionized water, filtering, and drying to obtain the final product. The cleaning solution is polyhydroxy polyamine chelating agent (Tianjin crystal mountain microelectronic material Co., Ltd.).
The preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 30min, adding sodium hydroxide, stirring at 60 deg.C until completely dissolved, adding bromohexadecane, stirring for 24h, distilling under reduced pressure to remove solvent, washing with deionized water at 75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
The silver powder prepared in example 9 had a surface organic residue of 0.43%; the dispersibility is high.
And (4) conclusion: the invention discloses a preparation method of silver powder, which has simple process steps and appropriate process parameters, can be applied to any preparation method of silver powder using a water-based dispersant, can realize the complete sedimentation of the silver powder, and has higher practicability because the organic residue on the surface of the obtained silver powder is lower than that of the silver powder not using the method by more than 0.3 percent.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for preparing silver powder is characterized in that: the method comprises the following steps:
(1) taking deionized water and silver nitrate, adding a dispersing agent, and stirring to a dissolved state to obtain a solution A;
taking deionized water and a reducing agent, adding a dispersing agent, and stirring to a dissolved state to obtain a solution B; the dispersing agent is any one of gelatin, Arabic gum and polyvinylpyrrolidone; or the dispersant is a mixture of N-alkyl benzotriazole and benzotriazole;
(2) adding the solution B into the solution A, and obtaining a suspension C after the reaction is completed;
(3) adding alkali liquor into the suspension C, adjusting the pH to 9, adding cleaning solution, performing ultrasonic dispersion for 20-30min, stirring for 30-40min, continuously adding alkali liquor to adjust the pH to 14, heating to 70-75 ℃, keeping the temperature, stirring for 1-2h, collecting silver powder after stirring, washing, performing suction filtration, and drying to obtain a finished product;
the cleaning solution is polyhydroxy polyamine chelating agent.
2. The method for producing silver powder according to claim 1, characterized in that: in the step (1), the reducing agent is any one or more of ascorbic acid, formaldehyde, hydrazine hydrate and hydrogen peroxide.
3. The method for producing a silver powder according to claim 1, characterized in that: in the step (3), the alkali liquor is any one or more of sodium hydroxide, potassium hydroxide and a salt solution containing hydroxide radical, and in the step (2), the solution B is added into the solution A at the speed of 2-3L/min.
4. The method for producing silver powder according to claim 1, characterized in that: the concentration of the silver nitrate is 0.5mol/L, and the mass ratio of the reducing agent to the silver nitrate is (1-4): 1.
5. the method for producing silver powder according to claim 1, characterized in that: in the step (3), the heat preservation and stirring time is 0.5-2 h.
6. The method for producing silver powder according to claim 1, characterized in that: in the step (1), the mass ratio of the N-alkyl benzotriazole to the benzotriazole is (3-4): 1;
the preparation method of the N-alkyl benzotriazole comprises the following steps: mixing benzotriazole and absolute ethyl alcohol, stirring for 20-30min, adding sodium hydroxide, stirring at 50-60 deg.C until completely dissolved, adding bromohexadecane, stirring for reaction for 20-24h, distilling under reduced pressure to remove solvent, washing with deionized water at 70-75 deg.C, standing for layering, removing water layer, and drying oil layer to obtain the final product.
7. The method for producing silver powder according to claim 1, characterized in that: the magnetic field intensity is 20-30mT when the magnetic material is prepared in the step (1) and the step (2) in an external magnetic field.
8. The method for producing silver powder according to claim 1, characterized in thatThe method comprises the following steps: in the step (3), after the silver powder is collected after stirring, mixing the silver powder with an ethanol solution, and ultrasonically dispersing for 5-10min under UV illumination with the illumination intensity of 200-2Then washing with deionized water, filtering, and drying to obtain the final product.
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