CN112355318B - Large-particle-size porous spherical nickel powder and preparation method thereof - Google Patents
Large-particle-size porous spherical nickel powder and preparation method thereof Download PDFInfo
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- CN112355318B CN112355318B CN202011133632.7A CN202011133632A CN112355318B CN 112355318 B CN112355318 B CN 112355318B CN 202011133632 A CN202011133632 A CN 202011133632A CN 112355318 B CN112355318 B CN 112355318B
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
Abstract
The invention relates to a large-particle-size porous spherical nickel powder and a preparation method thereof, wherein the preparation method comprises the following steps: respectively preparing a tannic polyphenol solution with the concentration of 1-2wt%, a liquid alkali solution with the concentration of 30-32wt%, an ammonia water solution with the concentration of 16-18wt% and a formaldehyde solution with the concentration of 5-20 wt%; preparing 80-130g/L nickel salt solution, and adjusting the pH of the nickel salt solution to 4.0-5.5 by using acid to obtain solution A; mixing tannin polyphenol solution with solution A according to the volume ratio of (1-5): 100 to obtain solution B; and (3) respectively pumping the solution B, the aqueous alkali solution and the aqueous ammonia solution into a reaction kettle for precipitation reaction, and finally reducing the nickel hydroxide powder obtained by filtering to obtain nickel powder. In the invention, tannin and aldehyde are condensed to generate tannin resin, and the existence of the tannin resin promotes the nickel ions added subsequently to continue to grow on the basis of original nickel hydroxide particles, thereby obtaining spherical nickel hydroxide with large particle size.
Description
Technical Field
The invention relates to the technical field of materials, in particular to large-particle-size porous spherical nickel powder and a preparation method thereof.
Background
The nickel powder is widely applied in industry, in the prior art, the nickel powder is mainly prepared by adopting an electrolytic method, a carbonylation method, a hydrogen reduction method and the like, in the electrolytic method, enriched sulfide ore is roasted into oxide firstly, then the oxide of nickel is reduced into crude nickel by carbon, and finally the crude nickel is electrolyzed to obtain pure metallic nickel; in the carbonylation method, nickel sulfide ore reacts with carbon monoxide to generate nickel tetracarbonyl, and then the nickel tetracarbonyl is heated and decomposed to obtain metal nickel with high purity; the hydrogen reduction method mainly uses hydrogen to reduce nickel oxide and nickel carbonate, and then the metallic nickel can be obtained. Among the above-mentioned several preparation methods, the highest purity of the product is the carbonylation method, then the reduction method and finally the electrolysis method, but the carbonylation method has very strong toxicity, because nickel tetracarbonyl is easy to volatilize and easy to dissolve in adipose tissue, and the binding force of the nickel tetracarbonyl with protein and nucleic acid is also very strong while the nickel tetracarbonyl is easy to enter the cell membrane. Nickel tetracarbonyl has irritation to respiratory tract and systemic toxic action, and can result in lung, liver and brain damage, and the incidence rate of respiratory tract cancer is higher than that of general population in nickel operation workers, and the incidence rate of lung cancer is higher than that of lung cancer by 2 times, 6 times and even 16 times, and the incidence rate of nasal cavity cancer is higher than that of nasal cavity cancer by 37-196 times in nickel operation workers.
In the field of porous materials, nickel powder having a particle diameter of 30 μm or more and spherical or spheroidic morphology is required. Because carbonyl nickel powder is toxic, the particle size and morphology of the carbonyl nickel powder and electrolytic nickel powder cannot meet the requirements, a hydrogen reduction method is generally adopted at present, namely, the nickel oxide and the nickel carbonate are granulated and then subjected to high-temperature reduction sintering to form balls, but the high-temperature sintering energy consumption is high, and the prepared nickel powder has the defects of less pores, low activity and poor performance.
Disclosure of Invention
In order to solve the problems, a nickel powder having a large particle diameter, a large number of voids and a spherical shape and a method for producing the same are provided.
The specific technical scheme is as follows:
the first aspect of the present invention is to provide a method for producing a large-particle-diameter porous spherical nickel powder, having such a feature that it comprises the steps of:
1) Respectively preparing a tannin polyphenol solution with the concentration of 1-2wt%, a liquid alkali solution with the concentration of 30-32wt%, an ammonia water solution with the concentration of 16-18wt% and a formaldehyde solution with the concentration of 5-20 wt%;
2) Preparing nickel salt solution with the concentration of 80-130g/L, and then adjusting the pH value of the nickel salt solution to 4.0-5.5 by using acid to obtain solution A;
3) Uniformly mixing the tannin polyphenol solution with the solution A according to the volume ratio of (1-5): 100 to obtain a solution B;
4) Pumping the solution B, the liquid alkali solution, the ammonia water solution and the formaldehyde solution into a reaction kettle respectively by metering pumps for precipitation reaction, wherein the reaction temperature is controlled to be 40-70 ℃, the pH value of the mother solution is 9.1-10.5, the concentration of free ammonia in the mother solution is 3-12g/L, and the reaction time is 50-180h;
5) Stopping the reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder with hydrogen at high temperature, and screening to obtain the large-particle-size porous spherical nickel powder.
The above preparation method further has the feature that the nickel hydroxide powder reduction method in step 5) is: nickel hydroxide powder is reduced with hydrogen at 350-500 deg.c.
The above preparation method further has the feature that the acid in step 2) is one of hydrochloric acid, nitric acid or sulfuric acid.
The above preparation method is also characterized in that the nickel salt in the nickel salt solution is one of nickel sulfate, nickel chloride or nickel nitrate.
In the invention, tannin polyphenol and Ni are utilized 2+ Stable complex is formed at pH value above 6.4, and then the complex reaction and the hydrolysis polymerization reaction with metal ion take place simultaneously with the rise of pH value, so that tannin polyphenol also shows strong reducibility while complexing to prevent Ni 2+ Is a metal oxide semiconductor device.
In the invention, nickel salt solution, liquid alkali and ammonia water are subjected to complexation and precipitation reaction to generate nickel hydroxide particles; meanwhile, the tannin and aldehyde are condensed under alkaline condition to generate tannin resin with adhesive property, and the existence of the tannin resin promotes the nickel ions added subsequently to continue to grow on the basis of the original nickel hydroxide particles, so as to obtain spherical nickel hydroxide with large particle size.
The second aspect of the present invention is to provide a large-particle-diameter porous spherical nickel powder prepared according to the above-described preparation method.
The D50 particle size of the nickel powder provided by the invention is 30-50um.
The nickel powder provided by the invention has the advantages of large particle size, many gaps and spherical shape.
Drawings
FIG. 1 is an SEM image of nickel powder provided in example 1 of the invention;
FIG. 2 is a graph showing the specific surface area of nickel powder provided in example 1 of the present invention;
FIG. 3 is an SEM image of nickel powder provided in example 2 of the invention;
FIG. 4 is a graph showing the specific surface area of nickel powder provided in example 2 of the present invention;
fig. 5 is an SEM image of the nickel powder provided in the comparative example of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention is further described below with reference to the drawings and specific examples, which are not intended to be limiting.
Example 1
The preparation of the large-particle-size porous spherical nickel powder comprises the following steps:
1) Respectively preparing a tannin polyphenol solution with the concentration of 1 weight percent, a liquid alkali solution with the concentration of 30 weight percent, an ammonia water solution with the concentration of 16 weight percent and a formaldehyde solution with the concentration of 5 weight percent;
2) Preparing nickel chloride solution with the concentration of 80g/L, and then adjusting the pH value of the nickel chloride solution to 4.0 by using acid to obtain solution A;
3) Uniformly mixing the tannin polyphenol solution and the solution A according to the volume ratio of 1:100 to obtain a solution B;
4) Pumping the solution B, the liquid alkali solution, the ammonia water solution and the formaldehyde solution into a reaction kettle respectively by metering pumps for precipitation reaction, controlling the reaction temperature to be 40+/-3 ℃, controlling the pH value of the mother solution to be 9.1-10.5, controlling the concentration of free ammonia in the mother solution to be 3-12g/L, and controlling the stirring rotation speed to be 150r/min for 180 hours;
5) Stopping the reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder with hydrogen at 350-500 ℃, and screening to obtain the large-particle-size porous spherical nickel powder.
As shown in fig. 1, the nickel powder provided in this embodiment is spherical.
As shown in FIG. 2, the nickel powder D50 provided in this example had a particle size of 31.98um and a BET specific surface area of 3.5cm 2 /g。
Example 2
The preparation of the large-particle-size porous spherical nickel powder comprises the following steps:
1) Respectively preparing a tannin polyphenol solution with the concentration of 1.5 weight percent, a liquid alkali solution with the concentration of 31 weight percent, an ammonia water solution with the concentration of 17 weight percent and a formaldehyde solution with the concentration of 10 weight percent;
2) Preparing nickel nitrate solution with the concentration of 110g/L, and then adjusting the pH value of the nickel nitrate solution to 4.7 by using acid to obtain solution A;
3) Uniformly mixing the tannin polyphenol solution and the solution A according to the volume ratio of 3:100 to obtain a solution B;
4) Pumping the solution B, the liquid alkali solution, the ammonia water solution and the formaldehyde solution into a reaction kettle respectively by metering pumps for precipitation reaction, controlling the reaction temperature to be 55+/-3 ℃, controlling the pH value of the mother solution to be 9.1-10.5, controlling the concentration of free ammonia in the mother solution to be 3-12g/L, and controlling the stirring rotation speed to be 200r/min for reaction for 90 hours;
5) Stopping the reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder with hydrogen at 350-500 ℃ and screening to obtain the large-particle-size porous spherical nickel powder.
As shown in fig. 3, the nickel powder provided in this embodiment is spherical.
As shown in FIG. 4, the nickel powder D50 provided in this example had a particle size of 56.049um and a BET specific surface area of 2.8cm 2 /g。
Example 3
The preparation of the large-particle-size porous spherical nickel powder comprises the following steps:
1) Respectively preparing a tannin polyphenol solution with the concentration of 2 weight percent, a liquid alkali solution with the concentration of 32 weight percent, an ammonia water solution with the concentration of 18 weight percent and a formaldehyde solution with the concentration of 20 weight percent;
2) Preparing a nickel salt solution with the concentration of 130g/L, and then adjusting the pH value of the nickel salt solution to 5.5 by using acid to obtain a solution A;
3) Uniformly mixing the tannin polyphenol solution and the solution A according to the volume ratio of 5:100 to obtain a solution B;
4) Pumping the solution B, the liquid alkali solution, the ammonia water solution and the formaldehyde solution into a reaction kettle respectively by metering pumps for precipitation reaction, wherein the reaction temperature is controlled to be 70+/-3 ℃, the pH value of the mother solution is 9.1-10.5, the concentration of free ammonia in the mother solution is 3-12g/L, the stirring rotation speed is 300r/min, and the reaction time is 50h;
5) Stopping the reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder with hydrogen at 350-500 ℃ and screening to obtain the large-particle-size porous spherical nickel powder.
Comparative example
In this comparative example, there is provided a nickel powder, the preparation of which comprises the steps of:
1) Preparing 32wt% of aqueous alkali solution and 18wt% of aqueous ammonia solution;
2) Preparing a nickel salt solution with the concentration of 130g/L, and then adjusting the pH value of the nickel salt solution to 4.7 by using acid;
3) Pumping the nickel salt solution, the liquid alkali solution and the ammonia water solution into a reaction kettle respectively by metering pumps to carry out precipitation reaction, controlling the reaction temperature to be 65+/-3 ℃, controlling the pH value of the mother solution to be 9.5+/-0.1, controlling the concentration of free ammonia in the mother solution to be 10-12 g/L, and controlling the stirring rotation speed to be 200r/min for 180h of reaction;
5) Stopping the reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder with hydrogen at 350-500 ℃ and screening to obtain the nickel powder.
As shown in fig. 5, the nickel powder is relatively dense and has small voids. The specific surface area test shows that the particle size of the nickel powder D50 is 14.049um, and the BET specific surface area is 0.76m 2 /g。
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, and it will be appreciated by those skilled in the art that equivalent substitutions and obvious variations may be made using the description and illustrations of the present invention, and are intended to be included within the scope of the present invention.
Claims (5)
1. The preparation method of the large-particle-size porous spherical nickel powder is characterized by comprising the following steps of:
1) Respectively preparing a tannin polyphenol solution with the concentration of 1-2wt%, a liquid alkali solution with the concentration of 30-32wt%, an ammonia water solution with the concentration of 16-18wt% and a formaldehyde solution with the concentration of 5-20 wt%;
2) Preparing nickel salt solution with the concentration of 80-130g/L, and then adjusting the pH value of the nickel salt solution to 4.0-5.5 by using acid to obtain solution A;
3) Uniformly mixing the tannin polyphenol solution with the solution A according to the volume ratio of (1-5): 100 to obtain a solution B;
4) Pumping the solution B, the aqueous ammonia solution of the aqueous alkali solution and the formaldehyde solution into a reaction kettle respectively by metering pumps for precipitation reaction, wherein the reaction temperature is controlled to be 40-70 ℃, the pH value of the mother solution is 9.1-10.5, the concentration of free ammonia in the mother solution is 3-12g/L, and the reaction time is 50-180h;
5) Stopping the reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder with hydrogen at high temperature, and screening to obtain the large-particle-size porous spherical nickel powder.
2. The method according to claim 1, wherein the nickel hydroxide powder reduction method in step 5) is: nickel hydroxide powder is reduced with hydrogen at 350-500 deg.c.
3. The method according to claim 1 or 2, wherein the acid in step 2) is one of hydrochloric acid, nitric acid or sulfuric acid.
4. The method according to claim 1 or 2, wherein the nickel salt in the nickel salt solution in step 2) is one of nickel sulfate, nickel chloride or nickel nitrate.
5. A large-particle-diameter porous spherical nickel powder, characterized by being prepared by the preparation method according to any one of claims 1 to 4.
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| CN113523271B (en) * | 2021-07-16 | 2023-04-18 | 安徽大学 | Method for preparing high-corrosion-resistance aluminum powder by complexing natural polyphenol and metal ions |
| CN116618642B (en) * | 2023-07-13 | 2023-10-10 | 长沙立优金属材料有限公司 | Nickel powder with large particles and low apparent density and preparation method and application thereof |
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