CN112355318A - 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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- B22F9/00—Making metallic powder or suspensions thereof
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- 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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Abstract
The invention relates to large-particle size porous spherical nickel powder and a preparation method thereof, wherein the preparation method comprises the following steps: respectively preparing 1-2 wt% tannin polyphenol solution, 30-32 wt% liquid alkali solution, 16-18 wt% ammonia water solution and 5-20 wt% formaldehyde solution; preparing to obtain 80-130g/L nickel salt solution, and adjusting the pH value of the nickel salt solution to 4.0-5.5 by using acid to obtain solution A; mixing the tannin polyphenol solution with the solution A according to the volume ratio of (1-5) to 100 to obtain a solution B; and respectively pumping the solution B, the liquid alkali solution and the ammonia water solution into a reaction kettle for precipitation reaction, and finally reducing the filtered nickel hydroxide powder to obtain the 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 growing on the basis of the original nickel hydroxide particles, thereby obtaining the 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, and in the prior art, the nickel powder is mainly prepared by an electrolytic method, a carbonylation method, a hydrogen reduction method and the like, wherein in the electrolytic method, enriched sulfide ore is roasted into oxide, then carbon is used for reducing the nickel oxide into crude nickel, and finally the crude nickel is electrolyzed to obtain pure metal nickel; in the carbonylation method, firstly, sulfide ore of nickel 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 is mainly to reduce nickel oxide and nickel carbonate by using hydrogen to obtain metallic nickel. The preparation method has the highest product purity of the carbonylation method, the reduction method and the electrolysis method, but the carbonylation method has very strong toxicity because the nickel tetracarbonyl is easy to volatilize and dissolve in adipose tissues, and the nickel tetracarbonyl can easily enter cell membranes and has strong binding force with proteins and nucleic acids. Nickel tetracarbonyl has stimulation effect on respiratory tract and systemic toxicity effect, and can cause damage to lung, liver and brain, respiratory tract cancer incidence rate in nickel workers is higher than that of general people, according to statistics, lung cancer incidence rate in nickel workers is 2, 6 or even 16 times higher, and nasal cavity cancer is 37-196 times higher.
In the field of porous materials, nickel powder with a particle size of more than 30um and a spherical or spheroidal morphology is required. Because the carbonyl nickel powder is toxic, and the particle size and the morphology of the carbonyl nickel powder and the electrolytic nickel powder can not meet the requirements, the prior hydrogen reduction method is generally adopted, 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 nickel powder prepared by the method has the defects of less pores, low activity and poor performance.
Disclosure of Invention
In view of the above problems, there are provided a nickel powder having a large particle diameter, a large number of voids and a spherical shape, and a method for producing the same.
The specific technical scheme is as follows:
the first aspect of the present invention is to provide a method for preparing large-particle size porous spherical nickel powder, having such characteristics that it comprises the steps of:
1) respectively preparing 1-2 wt% tannin polyphenol solution, 30-32 wt% liquid alkali solution, 16-18 wt% ammonia water solution and 5-20 wt% formaldehyde solution;
2) preparing a 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 a solution A;
3) uniformly mixing the tannin polyphenol solution with the solution A according to the volume ratio of (1-5) to 100 to obtain a solution B;
4) pumping the solution B, the liquid alkali solution and the ammonia water solution into a reaction kettle by a metering pump respectively for precipitation reaction, wherein the reaction temperature is controlled to be 40-70 ℃, the pH value of mother liquor is 9.1-10.5, the concentration of free ammonia in the mother liquor is 3-12g/L, and the reaction time is 50-180 h;
5) stopping reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder by hydrogen at high temperature, and screening to obtain the large-particle-size porous spherical nickel powder.
The above-mentioned production method is also characterized in that the nickel hydroxide powder reduction method in step 5) is: the nickel hydroxide powder is reduced by hydrogen gas under the conditions of 350-500 ℃.
The above-mentioned production method is also characterized in that the acid in the step 2) is one of hydrochloric acid, nitric acid and sulfuric acid.
The above-mentioned preparation method is also characterized in that the nickel salt in the nickel salt solution is one of nickel sulfate, nickel chloride and nickel nitrate.
The invention utilizes tannin polyphenol and Ni2+Stable complex formation is started at pH above 6.4, and then the above-mentioned complexation reaction and its hydrolytic complexation reaction with metal ion occur simultaneously with the increase of pH, so that tannin polyphenol can exhibit strong reducibility at the same time of complexation to prevent Ni2+Oxidation of (2).
In the invention, nickel salt solution, liquid alkali and ammonia water are subjected to complexation and precipitation reaction to generate nickel hydroxide particles; meanwhile, tannin and aldehyde are condensed under the alkaline condition to generate tannin resin with the characteristic of an adhesive, and the existence of the tannin resin promotes the nickel ions added subsequently to continue growing on the basis of the original nickel hydroxide particles, so that the spherical nickel hydroxide with large particle size is obtained.
The second aspect of the present invention is to provide a large-particle size porous spherical nickel powder prepared according to the above preparation method.
The particle size of the D50 of the nickel powder provided by the invention is 30-50 um.
The nickel powder provided by the invention has the advantages of large particle size, more gaps and spherical shape.
Drawings
FIG. 1 is an SEM image of nickel powder provided in example 1 of the present invention;
FIG. 2 is a test chart of 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 present invention;
FIG. 4 is a test chart of specific surface area of nickel powder provided in example 2 of the present invention;
FIG. 5 is an SEM image of nickel powders provided in comparative examples of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
Example 1
The preparation method 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 wt%, a liquid alkali solution with the concentration of 30 wt%, an ammonia water solution with the concentration of 16 wt% and a formaldehyde solution with the concentration of 5 wt%;
2) preparing a 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 a solution A;
3) uniformly mixing the tannin polyphenol solution with 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 and the ammonia water solution into a reaction kettle by a metering pump respectively for precipitation reaction, controlling the reaction temperature to be 40 +/-3 ℃, the pH value of the mother liquor to be 9.1-10.5, the concentration of free ammonia in the mother liquor to be 3-12g/L, the stirring speed to be 150r/min, and reacting for 180 hours;
5) stopping reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder by hydrogen at the temperature of 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 example is spheroidal.
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 3.5cm2/g。
Example 2
The preparation method 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 wt%, a liquid alkali solution with the concentration of 31 wt%, an ammonia water solution with the concentration of 17 wt% and a formaldehyde solution with the concentration of 10 wt%;
2) preparing a 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 a solution A;
3) uniformly mixing the tannin polyphenol solution with 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 and the ammonia water solution into a reaction kettle by a metering pump respectively for precipitation reaction, controlling the reaction temperature to be 55 +/-3 ℃, the pH value of the mother liquor to be 9.1-10.5, the concentration of free ammonia in the mother liquor to be 3-12g/L, the stirring speed to be 200r/min, and reacting for 90 hours;
5) stopping reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder by hydrogen at the temperature of 350-500 ℃, and then screening to obtain the large-particle-size porous spherical nickel powder.
As shown in FIG. 3, the nickel powder provided in this example is spheroidal.
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 2.8cm2/g。
Example 3
The preparation method 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 wt%, a liquid alkali solution with the concentration of 32 wt%, an ammonia water solution with the concentration of 18 wt% and a formaldehyde solution with the concentration of 20 wt%;
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 with 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 and the ammonia water solution into a reaction kettle by a metering pump respectively for precipitation reaction, controlling the reaction temperature to be 70 +/-3 ℃, the pH value of the mother liquor to be 9.1-10.5, the concentration of free ammonia in the mother liquor to be 3-12g/L, the stirring speed to be 300r/min and the reaction time to be 50 h;
5) stopping reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder by hydrogen at the temperature of 350-500 ℃, and then screening to obtain the large-particle-size porous spherical nickel powder.
Comparative example
In this comparative example, there is provided a nickel powder prepared by the steps of:
1) preparing 32 wt% of liquid caustic soda solution and 18 wt% of ammonia water 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 by a metering pump respectively for precipitation reaction, controlling the reaction temperature to be 65 +/-3 ℃, the pH value of the mother liquor to be 9.5 +/-0.1, the concentration of free ammonia in the mother liquor to be 10-12 g/L, the stirring speed to be 200r/min, and reacting for 180 hours;
5) stopping reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder by hydrogen at the temperature of 350-500 ℃, and then 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 0.76m2/g。
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of large-particle-size porous spherical nickel powder is characterized by comprising the following steps:
1) respectively preparing 1-2 wt% tannin polyphenol solution, 30-32 wt% liquid alkali solution, 16-18 wt% ammonia water solution and 5-20 wt% formaldehyde solution;
2) preparing a 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 a solution A;
3) uniformly mixing the tannin polyphenol solution with the solution A according to the volume ratio of (1-5) to 100 to obtain a solution B;
4) pumping the solution B, the liquid alkali solution and the ammonia water solution into a reaction kettle by a metering pump respectively for precipitation reaction, wherein the reaction temperature is controlled to be 40-70 ℃, the pH value of mother liquor is 9.1-10.5, the concentration of free ammonia in the mother liquor is 3-12g/L, and the reaction time is 50-180 h;
5) stopping reaction, filtering, washing and drying filter residues to obtain nickel hydroxide powder, reducing the nickel hydroxide powder by hydrogen at high temperature, and screening to obtain the large-particle-size porous spherical nickel powder.
2. The production method according to claim 1, wherein the nickel hydroxide powder reduction method in step 5) is: the nickel hydroxide powder is reduced by hydrogen gas under the conditions of 350-500 ℃.
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. Large-particle-size porous spherical nickel powder produced by the production method according to any one of claims 1 to 4.
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Cited By (2)
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| CN113523271A (en) * | 2021-07-16 | 2021-10-22 | 安徽大学 | Method for preparing high-corrosion-resistance aluminum powder by complexing natural polyphenol and metal ions |
| CN116618642A (en) * | 2023-07-13 | 2023-08-22 | 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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| CN113523271A (en) * | 2021-07-16 | 2021-10-22 | 安徽大学 | Method for preparing high-corrosion-resistance aluminum powder by complexing natural polyphenol and metal ions |
| CN116618642A (en) * | 2023-07-13 | 2023-08-22 | 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 |
| 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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