CN113087026A - Continuous crystallization production process of nickel chloride solution - Google Patents
Continuous crystallization production process of nickel chloride solution Download PDFInfo
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- CN113087026A CN113087026A CN202110475484.5A CN202110475484A CN113087026A CN 113087026 A CN113087026 A CN 113087026A CN 202110475484 A CN202110475484 A CN 202110475484A CN 113087026 A CN113087026 A CN 113087026A
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- nickel chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/08—Halides
- C01G53/09—Chlorides
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a continuous crystallization production process of a nickel chloride solution, which comprises the following steps: feeding liquid, adding seed crystals, siphoning crystal slurry and filtering and separating, wherein the nickel chloride hexahydrate crystal obtained by the method of continuously feeding liquid and filtering and separating has good glossiness and is not easy to agglomerate, and the chemical quality is superior to the requirement of the existing nickel chloride industry standard for electroplating (HG/T2771-one 2009). The method has the advantages of simple and stable process and strong operability, not only has high crystallization rate, but also can not introduce other impurities, and is a new method for producing electroplated nickel chloride by continuous crystallization of the nickel chloride solution.
Description
Technical Field
The invention belongs to the technical field of nickel chloride production, and particularly relates to a continuous crystallization production process of a nickel chloride solution.
Background
Industrial nickel chloride is mainly used in the electroplating industry, is the main nickel salt raw material for electroplating and chemical plating, and can dissociate nickel ions and chloride ions during electroplating. The nickel plating solution is mainly applied to the domestic high-end nickel plating market, and comprises high-end automobile parts, computer hard disks in the electronic industry, microelectronic chips, printed circuit boards, high-end bathrooms, decorative electroplating of hardware and the like.
The crystallization mode commonly adopted in industrial production is intermittent crystallization, and specifically comprises the following steps: the nickel chloride hexahydrate product is produced by the methods of evaporation concentration and cooling crystallization. This method has the following disadvantages: 1) the supersaturation degree is not easy to control in the evaporation process of the solution, so that the chemical quality and the physical appearance of the final product are not stable enough; 2) the cooling crystallization process needs to consume a large amount of low-temperature water, and the crystallization period is long.
Disclosure of Invention
The invention provides a continuous crystallization production process of a nickel chloride solution, and aims to solve the problems of unstable quality and long crystallization period of a nickel chloride crystallization product at present.
Therefore, the invention adopts the following technical scheme:
a continuous crystallization production process of a nickel chloride solution comprises the following steps:
1) liquid feeding: inserting a liquid inlet pipe into the crystallization kettle, wherein the lower end of the liquid inlet pipe is positioned in the middle or lower part of the crystallization kettle; inputting supersaturated nickel chloride solution into the crystallization kettle through a liquid inlet pipe, starting stirring after the liquid level is over a stirrer, and stopping liquid inlet when the liquid level is increased to 75-85%;
2) seed crystal addition: cooling the crystallization kettle by using a coil pipe, controlling the temperature of circulating water in the coil pipe to be 18-23 ℃, adding seed crystals when the temperature of a solution in the crystallization kettle is reduced to 32-34 ℃, and then preserving the temperature for 20-30 min;
3) crystal slurry siphoning: inserting a siphon pipe into the bottom of the crystallization kettle, starting the siphon, and simultaneously starting a liquid inlet pipe to continuously feed liquid; controlling the temperature of the solution in the crystallization kettle to be 31-32 ℃, and controlling the liquid discharge speed of a siphon to be equal to the liquid inlet speed of a liquid inlet pipe;
4) filtering and separating: and (3) sending the crystal slurry discharged by the siphon in the step 3) into a filtering device for filtering and separating, drying the obtained crystals to obtain a final product, and sending the crystallization mother liquor to a recovery system for reuse.
Further, the concentration of the nickel chloride solution in the step 1) is 5-5.5 mol/L.
Further, the rotating speed of the stirrer in the step 1) is 133 +/-5 r/min.
Further, the volume ratio of the seed crystal added in the step 2) to the volume of the solution in the crystallization kettle is 1: 20-30.
Further, the solid-to-liquid ratio in the crystallization kettle needs to exceed 30% when the siphon is opened in the step 3).
The nickel chloride hexahydrate crystal obtained by the method of continuously feeding liquid, controlling the temperature of a crystallization kettle, separating out crystals, siphoning crystal mush and filtering and separating has the advantages of regular crystal form, good glossiness, difficult agglomeration and chemical quality superior to the requirement of the existing industrial nickel chloride standard (HG/T2824-2009); the method has the advantages of simple and reliable process, strong operability and strong continuity, effectively reduces energy consumption, and does not introduce other impurities; the invention can obviously reduce the crystallization energy consumption, has better economic value and is a new method for continuously crystallizing the nickel chloride solution.
Detailed Description
The invention will be further illustrated with reference to specific examples:
the nickel chloride aqueous solution used in the invention has the following component concentration: 314.34g/L Ni; 0.001g/L of Co; 0.001g/L of Cu; 0.002g/L of Fe; pb is 0.001 g/L; 0.001g/L of Zn; 0.011g/L of Ca; 0.005g/L of Mg; na is 0.007 g/L; size of crystallization kettle: phi 1500 x 4500, the bottom is conical.
Example 1
Inputting the solution of the components into a crystallization kettle, starting stirring after the liquid level of the solution is over a stirrer, introducing cooling water with the temperature of 21.5 ℃ into a coil pipe, controlling the temperature of the crystallization kettle at 32 ℃, stopping liquid inlet when the liquid level is raised to 80%, adding nickel chloride crystal seeds for 1t, keeping the temperature for 30min after adding the crystal seeds, and enabling crystals to grow and be separated out; measuring the solid-liquid ratio of the crystallization kettle to be 40%, starting siphoning, simultaneously starting continuous liquid feeding, and controlling the temperature of the crystallization kettle to be 32 ℃; and filtering and separating the crystal slurry discharged from the siphon by using a belt filter, and drying to obtain 8t of nickel chloride hexahydrate crystals. The chemical composition is Ni: 24.20 percent; co: 0.0002 percent; cu: 0.0001 percent; 0.0004 percent of Fe; 0.0001 percent of Pb; zn: 0.0001 percent; ca: 0.001 percent; mg: 0.0005%; na: 0.0017%; water-insoluble matter: 0.0015 percent; pH: 4.76.
example 2
Inputting the solution of the components into a crystallization kettle, starting stirring after the liquid level of the solution is over a stirrer, introducing cooling water with the temperature of 21.5 ℃ into a coil pipe, controlling the temperature of the crystallization kettle at 33 ℃, stopping liquid inlet when the liquid level rises to 80%, adding nickel chloride crystal seeds for 1t, keeping the temperature for 30min after adding the crystal seeds, and enabling crystals to grow and be separated out; measuring the solid-liquid ratio of the crystallization kettle to be 45%, starting siphoning, simultaneously starting continuous liquid feeding, and controlling the temperature of the crystallization kettle to be 31 ℃; and filtering and separating the crystal slurry discharged from the siphon by using a belt filter, and drying to obtain 6t nickel chloride hexahydrate crystals. The chemical composition is Ni: 24.22 percent; co: 0.0002 percent; cu: 0.0001 percent; 0.0003 percent of Fe; 0.0001 percent of Pb; zn: 0.0001 percent; ca: 0.001 percent; mg: 0.0007 percent; na: 0.0012%; water-insoluble matter: 0.0015 percent; pH: 5.11.
example 3
Inputting the solution of the components into a crystallization kettle, starting stirring after the liquid level of the solution is over a stirrer, introducing cooling water with the temperature of 22.5 ℃ into a coil pipe, controlling the temperature of the crystallization kettle at 32 ℃, stopping liquid inlet when the liquid level is raised to 80%, adding nickel chloride crystal seeds for 0.9t, keeping the temperature for 30min after adding the crystal seeds, and enabling crystals to grow and be separated out; measuring the solid-liquid ratio of the crystallization kettle to be 35%, starting siphoning, simultaneously starting continuous liquid feeding, and controlling the temperature of the crystallization kettle to be 32 ℃; and filtering and separating the crystal slurry discharged from the siphon by using a belt filter, and drying to obtain 5.5t of nickel chloride hexahydrate crystals. The chemical composition is Ni: 24.16 percent; co: 0.0003 percent; cu: 0.0001 percent; 0.0004 percent of Fe; 0.0001 percent of Pb; zn: 0.0001 percent; ca: 0.001 percent; mg: 0.0004 percent; na: 0.0011%; water-insoluble matter: 0.0015 percent; pH: 4.43.
example 4
Inputting the solution of the components into a crystallization kettle, starting stirring after the liquid level of the solution is over a stirrer, introducing cooling water with the temperature of 21.5 ℃ into a coil pipe, controlling the temperature of the crystallization kettle at 34 ℃, stopping liquid inlet when the liquid level is raised to 80%, adding nickel chloride crystal seeds for 0.9t, keeping the temperature for 30min after adding the crystal seeds, and enabling crystals to grow and be separated out; measuring the solid-liquid ratio of the crystallization kettle to be 40%, starting siphoning, simultaneously starting continuous liquid feeding, and controlling the temperature of the crystallization kettle to be 32 ℃; and filtering and separating the crystal slurry discharged from the siphon by using a belt filter, and drying to obtain 4t of nickel chloride hexahydrate crystals. The chemical composition is Ni: 24.12 percent; co: 0.0002 percent; cu: 0.0001 percent; 0.0003 percent of Fe; 0.0001 percent of Pb; zn: 0.0001 percent; ca: 0.001 percent; mg: 0.0004 percent; na: 0.0014%; water-insoluble matter: 0.0015 percent; pH: 4.52.
example 5
Inputting the solution of the components into a crystallization kettle, starting stirring after the liquid level of the solution is over a stirrer, introducing cooling water with the temperature of 21.5 ℃ into a coil pipe, controlling the temperature of the crystallization kettle at 32 ℃, stopping liquid inlet when the liquid level is raised to 80%, adding nickel chloride crystal seeds for 1t, keeping the temperature for 30min after adding the crystal seeds, and enabling crystals to grow and be separated out; measuring the solid-liquid ratio of the crystallization kettle to be 40%, starting siphoning, simultaneously starting continuous liquid feeding, and controlling the temperature of the crystallization kettle to be 32 ℃; and filtering and separating the crystal slurry discharged from the siphon by using a belt filter, and drying to obtain 6t nickel chloride hexahydrate crystals. The chemical composition is Ni: 24.20 percent; co: 0.0003 percent; cu: 0.0001 percent; 0.0004 percent of Fe; 0.0001 percent of Pb; zn: 0.0001 percent; ca: 0.001 percent; mg: 0.0008 percent; na: 0.0014%; water-insoluble matter: 0.0015 percent; pH: 5.04.
it should be noted that the above are only some embodiments of the present invention, and it should be noted that, for those skilled in the art, many modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (5)
1. A continuous crystallization production process of a nickel chloride solution is characterized by comprising the following steps:
1) liquid feeding: inserting a liquid inlet pipe into the crystallization kettle, wherein the lower end of the liquid inlet pipe is positioned in the middle or lower part of the crystallization kettle; inputting supersaturated nickel chloride solution into the crystallization kettle through a liquid inlet pipe, starting stirring after the liquid level is over a stirrer, and stopping liquid inlet when the liquid level is increased to 75-85%;
2) seed crystal addition: cooling the crystallization kettle by using a coil pipe, controlling the temperature of circulating water in the coil pipe to be 18-23 ℃, adding seed crystals when the temperature of a solution in the crystallization kettle is reduced to 32-34 ℃, and then preserving the temperature for 20-30 min;
3) crystal slurry siphoning: inserting a siphon pipe into the bottom of the crystallization kettle, starting the siphon, and simultaneously starting a liquid inlet pipe to continuously feed liquid; controlling the temperature of the solution in the crystallization kettle to be 31-32 ℃, and controlling the liquid discharge speed of a siphon to be equal to the liquid inlet speed of a liquid inlet pipe;
4) filtering and separating: and (3) sending the crystal slurry discharged by the siphon in the step 3) into a filtering device for filtering and separating, drying the obtained crystals to obtain a final product, and sending the crystallization mother liquor to a recovery system for reuse.
2. The continuous crystallization production process of the nickel chloride solution according to claim 1, wherein the concentration of the nickel chloride solution in the step 1) is 5-5.5 mol/L.
3. The continuous crystallization production process of a nickel chloride solution according to claim 1, wherein the rotation speed of the stirrer in the step 1) is 133 ± 5 r/min.
4. The continuous crystallization production process of the nickel chloride solution according to claim 1, wherein the volume ratio of the seed crystal added in the step 2) to the solution in the crystallization kettle is 1: 20-30.
5. The continuous crystallization production process of nickel chloride solution according to claim 1, wherein the solid-to-liquid ratio in the crystallization kettle in step 3) is more than 30% when the siphon is opened.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114225465A (en) * | 2021-12-31 | 2022-03-25 | 金川集团镍盐有限公司 | Method for producing electroplated nickel sulfate by continuous crystallization of nickel sulfate solution |
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2021
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| JP2000336408A (en) * | 1999-05-26 | 2000-12-05 | Sumitomo Metal Mining Co Ltd | Production of nickel powder for multilayer ceramic capacitor electrode and device for producing it |
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| CN114225465A (en) * | 2021-12-31 | 2022-03-25 | 金川集团镍盐有限公司 | Method for producing electroplated nickel sulfate by continuous crystallization of nickel sulfate solution |
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