CN116835675A - Method for obtaining battery grade nickel sulfate solution by one-step half extraction of nickel cobalt sulfate leaching solution - Google Patents
Method for obtaining battery grade nickel sulfate solution by one-step half extraction of nickel cobalt sulfate leaching solution Download PDFInfo
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- CN116835675A CN116835675A CN202310685893.7A CN202310685893A CN116835675A CN 116835675 A CN116835675 A CN 116835675A CN 202310685893 A CN202310685893 A CN 202310685893A CN 116835675 A CN116835675 A CN 116835675A
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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
- C01G53/10—Sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention relates to a method for obtaining a battery grade nickel sulfate solution by one-step semi-extraction of a nickel cobalt sulfate leaching solution, which comprises the following steps: (1) Adding sulfonated kerosene into P204, then adding NaOH solution, and phase-separating to obtain P204 sodium soap organic phase; (2) The P204 sodium soap organic phase reacts with the nickel-cobalt sulfate leaching solution, and then extraction and phase separation are carried out, so that a P204 load organic phase and a nickel sulfate solution containing high cobalt and magnesium are obtained; (3) Washing the P204 loaded organic phase with dilute hydrochloric acid at normal temperature to obtain a P204 loaded organic phase after nickel washing and nickel washing liquid; (4) And (3) carrying out back extraction on the P204 loaded organic phase after nickel washing by hydrochloric acid to obtain chloride back extraction liquid for removing nickel, cobalt and magnesium. According to the invention, the battery grade nickel sulfate solution is obtained by only adopting the one-step semi-extraction procedure by utilizing phosphoric acid and the P204 extractant, so that the use of extraction materials and procedure steps in the prior art are greatly reduced, the extraction rate of the whole finished product nickel sulfate and the washing cobalt mixed solution is obviously improved, and excellent cost reduction and synergy are realized.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal smelting, and particularly relates to a method for obtaining a battery grade nickel sulfate solution by one-step semi-extraction of a nickel sulfate cobalt leaching solution.
Background
Nickel sulfate is widely used in the industries of electroplating, storage battery materials, catalysts, pigments and the like. In recent years, with the development of aluminum profile surface treatment technology and the updating of battery products, the application field of nickel sulfate is continuously widened. Nickel sulfate is one of the main raw materials of the ternary battery, and the market demand is rising year by year.
Cobalt nickel hydroxide, one of the laterite nickel ore intermediates, has now become one of the primary nickel raw materials for the electrolysis of nickel and nickel salts. In a sulfuric acid system, crude cobalt nickel hydroxide prepared from nickel sulfide concentrate is used as a raw material, and nickel sulfate is produced through processes such as acid dissolution, extraction, impurity removal, cooling crystallization and the like, and the process is relatively more mature and reliable. The existing nickel-cobalt sulfate leaching solution generally needs to be subjected to multiple extraction processes of multiple extraction agents in a multi-cycle mode, for example, P204 extraction is used for separating copper, manganese and zinc in the solution, P507 extraction is used for separating nickel and cobalt, and finally C272 extraction is used for removing magnesium, so that the whole process is complex, the material consumption is huge, and the extraction rate of the whole nickel sulfate finished product is low.
The inventor of the invention provides a method for obtaining a battery grade nickel sulfate solution by one-step and half-extraction of a nickel cobalt sulfate leaching solution through continuous exploration, and on the basis of the nickel cobalt sulfate leaching solution prepared by a method for intermittently adding acid to leach the nickel cobalt sulfate leaching solution corresponding to a nickel cobalt oxide raw material, only one P204 extractant is adopted to carry out one-step and half-extraction process to obtain the battery grade nickel sulfate solution, so that the use of extraction materials and process steps in the prior art are greatly reduced, the extraction rate of a whole finished product nickel sulfate and a washing cobalt mixed solution is obviously improved, and excellent cost reduction and synergy are realized.
Disclosure of Invention
The invention aims to provide a method for obtaining a battery grade nickel sulfate solution by one-step semi-extraction of a nickel cobalt sulfate leaching solution, which is used for obtaining a finished product nickel sulfate solution and a washing cobalt mixed solution by one-step semi-extraction of the nickel cobalt sulfate leaching solution. Under the conditions of greatly reducing the use of extraction materials and working procedure steps in the prior art, the invention obviously improves the extraction rate of the whole finished product nickel sulfate and washing cobalt mixed solution and realizes good cost reduction and synergy.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for obtaining a battery grade nickel sulfate solution by one-step semi-extraction of a nickel cobalt sulfate leaching solution comprises the following steps:
(1) Adding sulfonated kerosene into P204, then adding NaOH solution, adjusting the hydrogen ion concentration in the P204 after adding the sulfonated kerosene from 0.5mol/L to 0.6mol/L to 0.2mol/L to 0.3mol/L, and separating phases to obtain a P204 sodium soap organic phase;
(2) The P204 sodium soap organic phase reacts with the nickel-cobalt sulfate leaching solution, and then extraction and phase separation are carried out, so that a P204 load organic phase and a nickel sulfate solution containing high cobalt and magnesium are obtained;
(3) Washing the P204 loaded organic phase with dilute hydrochloric acid at normal temperature to obtain a P204 loaded organic phase after nickel washing and nickel washing liquid;
(4) And (3) carrying out back extraction on the P204 loaded organic phase after nickel washing by hydrochloric acid to obtain chloride back extraction liquid for removing nickel, cobalt and magnesium.
Further, the elements of the nickel cobalt sulfate leaching solution are set as (unit g/l) Ni=130-140, co=8-9, na=0.1-0.15, mg=3.5-4, ca=0.15-0.22, cu=0.012-0.021, fe=0.0009-0.0012, mu=12.5-13.0, pb=0.001, zn=1.5-1.75, cd=0.001-0.0012, cr=0.0037-0.0041, al=0.004-0.0055, C l =0.0055-0.0065, wherein PH=4.
Further, the washing cobalt mixed solution comprises the following components (unit g/l): co=80-100, mn=2-5, mg=15, ni=0.001, cu=0.01, zn=0.001, ca=0.05.
Further, the anti-impurity mixed solution comprises the following components (unit g/l): mn=100-130, cu=20-30, zn=30, co=0.2, mg=2.
In the step (2), the P204 sodium soap organic phase reacts with the nickel cobalt sulfate leaching solution, and then 9-10-level countercurrent extraction is carried out at the temperature of 30-40 ℃ and phase separation is carried out; the ratio of the P204 sodium soap organic phase to the nickel cobalt sulfate leaching solution is 2:1.
Further, in the step (3), the organic phase loaded with P204 is subjected to 8-10-stage countercurrent washing at normal temperature by dilute hydrochloric acid with the concentration of 1.0mol/L to 2.0mol/L, and the ratio of the organic phase loaded with P204 after washing to the hydrochloric acid solution with the concentration of 2mol/L to 4mol/L is 10:1.
in the step (4), the organic phase loaded by the P204 after nickel washing is back extracted by hydrochloric acid with the concentration of 2 to 4mol/L, and the ratio of the organic phase loaded by the P204 after nickel washing to the hydrochloric acid solution with the concentration of 2 to 4mol/L is 8:1.
Further, the mass percentage concentration of the NaOH solution in the step (1) is 25% -30%, and the P204 and the sulfonated kerosene are mixed according to the volume ratio of 1:3.
Further, the method for obtaining the nickel cobalt sulfate leaching solution comprises the following steps: step one, mixing raw ore containing cobalt nickel hydroxide with water for size mixing to obtain a solid-liquid ratio of 1: 2-3 raw material ore pulp;
starting a stirrer, feeding the raw material ore pulp obtained in the step one, intermittently adding concentrated sulfuric acid into the stirrer after feeding, and carrying out raw material leaching reaction for 60-90 min after adding acid, wherein the end point PH is controlled to be less than or equal to 2.5;
step three, standing for 20-30 min after the reaction in the step two, and after the obtained leaching slurry is subjected to dense separation, overflowing the supernatant to a transfer tank to be used as a pre-iron-aluminum liquid and underflow slag for later use;
step four, a solid-liquid ratio is configured to be 1: 2-3, adding the raw material ore pulp serving as a precipitator into the iron and aluminum removing precursor solution obtained in the step three to perform iron and aluminum removing reaction, wherein the reaction time is more than or equal to 1h;
and fifthly, carrying out solid-liquid separation on the slurry obtained in the step four to obtain a purified nickel cobalt sulfate solution, and conveying the purified nickel cobalt sulfate solution to the downstream as an extraction raw solution to obtain iron-aluminum waste residues for later use. .
Further, the mass percentage concentration of the concentrated sulfuric acid is 93% -98%.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, only one P204 extractant combination sulfonated kerosene is adopted for the nickel cobalt sulfate leaching solution, only one round of extraction, washing and back extraction processes are carried out, and the whole extraction process is greatly improved compared with the prior art while the nickel sulfate solution and the washing cobalt mixed solution with high yield are obtained, so that the extraction process flow of other extractants is reduced, the cost of materials and extraction equipment is greatly reduced, the produced waste is reduced, and excellent cost reduction and synergy are realized.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
The invention provides a method for obtaining a battery grade nickel sulfate solution by one-step half extraction of nickel cobalt sulfate leaching solution, wherein the selected nickel cobalt sulfate leaching solution comprises the following elements (unit g/l) of Ni=130-140, co=8-9, na=0.1-0.15, mg=3.5-4, ca=0.15-0.22, cu=0.012-0.021, fe=0.0009-0.0012, mu=12.5-13.0, pb=0.001, zn=1.5-1.75, cd=0.001-0.0012, cr=0.0037-0.0041, al=0.004-0.0055, C l =0.0055-0.0065 and PH=4, and the specific method comprises the following steps:
(1) Adding sulfonated kerosene into P204, and then adding NaOH solution, so that the concentration of hydrogen ions in the P204 after adding the sulfonated kerosene is adjusted from 0.5mol/L to 0.6mol/L to 0.2mol/L
0.3mol/L, and separating phases to obtain a P204 sodium soap organic phase; wherein the mass percentage concentration of the NaOH solution is 25% -30%, and P204 and sulfonated kerosene are mixed according to the volume ratio of 1:3;
(2) The P204 sodium soap organic phase reacts with the nickel-cobalt sulfate leaching solution, and then extraction and phase separation are carried out, so that a P204 load organic phase and a nickel sulfate solution containing high cobalt and magnesium are obtained; wherein, the P204 sodium soap organic phase reacts with the nickel cobalt sulfate leaching solution, and is subjected to 9-10-level countercurrent extraction at 30-40 ℃ and then phase separation; the ratio of the P204 sodium soap organic phase to the nickel cobalt sulfate leaching solution is 2:1;
(3) Washing the P204 loaded organic phase with dilute hydrochloric acid at normal temperature to obtain a P204 loaded organic phase after nickel washing and nickel washing liquid; wherein the P204 loaded organic phase is subjected to 8-10-level countercurrent washing at normal temperature by dilute hydrochloric acid with the concentration of 1.0mol/L to 2.0mol/L, and the ratio of the washed P204 loaded organic phase to the hydrochloric acid solution with the concentration of 2mol/L to 4mol/L is 10:1, a step of;
(4) Carrying out back extraction on the P204 loaded organic phase after nickel washing by hydrochloric acid to obtain chloride back extraction liquid for removing nickel, cobalt and magnesium; wherein the P204 loaded organic phase after nickel washing is back extracted by hydrochloric acid with the concentration of 2 to 4mol/L, and the ratio of the P204 loaded organic phase after nickel washing to the hydrochloric acid solution with the concentration of 2 to 4mol/L is 8:1.
Further, the washing cobalt mixed solution comprises the following components (unit g/l): co=80-100, mn=2-5, mg=15, ni=0.001, cu=0.01, zn=0.001, ca=0.05.
Further, the anti-impurity mixed solution comprises the following components (unit g/l): mn=100-130, cu=20-30, zn=30, co=0.2, mg=2.
The method for obtaining the nickel cobalt sulfate leaching solution comprises the following steps: step one, mixing raw ore containing cobalt nickel hydroxide with water for size mixing to obtain a solid-liquid ratio of 1: 2-3 raw material ore pulp;
starting a stirrer, feeding the raw material ore pulp obtained in the step one, intermittently adding concentrated sulfuric acid into the stirrer after feeding, and carrying out raw material leaching reaction for 60-90 min after adding acid, wherein the end point PH is controlled to be less than or equal to 2.5;
step three, standing for 20-30 min after the reaction in the step two, and after the obtained leaching slurry is subjected to dense separation, overflowing the supernatant to a transfer tank to be used as a pre-iron-aluminum liquid and underflow slag for later use;
step four, a solid-liquid ratio is configured to be 1: 2-3, adding the raw material ore pulp serving as a precipitator into the iron and aluminum removing precursor solution obtained in the step three to perform iron and aluminum removing reaction, wherein the reaction time is more than or equal to 1h;
and fifthly, carrying out solid-liquid separation on the slurry obtained in the step four to obtain a purified nickel cobalt sulfate solution, and conveying the purified nickel cobalt sulfate solution to the downstream as an extraction raw solution to obtain iron-aluminum waste residues for later use. .
Further, the mass percentage concentration of the concentrated sulfuric acid is 93% -98%.
Wherein the cobalt nickel hydroxide raw material intermediate used in the examples of the present invention is outsourced, typical components are set in two proportions as follows.
The cobalt nickel hydroxide intermediate comprises the following components in percentage by mass: 48.27% of Ni and Ni, 2.92% of Co and Co, 0.059% of Cu and Cu, 7.19% of Mn and Mn, 1.93% of Mg and Mg, 0.00085% of Cd and Cd, 0.037% of Na, 0.0094% of Ca and Zn, 0.15% of Zn and Zn, 0.0019% of Pb and Pb, 0.1% of Fe, 0.023% of Al and Al, 0.051% of Cr and Si, 0.044% of water and 51.45%.
The element components of the nickel-cobalt sulfate leaching solution obtained by the method for obtaining the nickel-cobalt sulfate leaching solution in practical application are (unit g/l):
ni= 134.21, co=8.67, na=0.124, mg=3.71, ca=0.202, cu=0.017, fe=0.001, mu=12.76, pb=0.001, zn=1.63, cd=0.0011, cr=0.0039, al=0.005, C l =0.006, where ph=4.
Examples
Based on the nickel-cobalt sulfate leaching solution, the method is implemented according to the method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel-cobalt sulfate leaching solution, and the obtained washing cobalt mixed solution comprises the following components (unit g/l): co=92.5, mn=3.2, mg=15, N i =0.001, cu=0.01, zn=0.001, ca=0.05.
The corresponding back-extracted back-mixed solution comprises the following components (unit g/l): mn=125.4, cu=20-30, zn=30, co=0.2, mg=2. Obtaining a finished solution for sale to downstream manufacturers.
In the integral extraction process, the nickel sulfate solution containing high cobalt and magnesium obtained in the step (2) accounts for 94% of the nickel content in the nickel cobalt sulfate leaching solution, and the extraction rate of the finished product nickel sulfate and the washing cobalt mixed solution is further improved to 99% in the step (3), so that the method has an excellent economic effect.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The method for obtaining the battery grade nickel sulfate solution by one-step semi-extraction of the nickel cobalt sulfate leaching solution is characterized by comprising the following steps of: (1) Adding sulfonated kerosene into P204, then adding NaOH solution, adjusting the concentration of hydrogen ions in the P204 after adding the sulfonated kerosene from 0.5mol/L to 0.6mol/L to 0.2mol/L to 0.3mol/L, and separating phases to obtain a P204 sodium soap organic phase;
(2) The P204 sodium soap organic phase reacts with the nickel-cobalt sulfate leaching solution, and then extraction and phase separation are carried out, so that a P204 load organic phase and a nickel sulfate solution containing high cobalt and magnesium are obtained;
(3) Washing the P204 loaded organic phase with dilute hydrochloric acid at normal temperature to obtain a P204 loaded organic phase after nickel washing and nickel washing liquid;
(4) And (3) carrying out back extraction on the P204 loaded organic phase after nickel washing by hydrochloric acid to obtain chloride back extraction liquid for removing nickel, cobalt and magnesium.
2. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to claim 1, which is characterized in that: the elements of the leaching solution of nickel and cobalt sulfate are set as (unit g/l) Ni=130-140, co=8-9, na=0.1-0.15, mg=3.5-4, ca=0.15-0.22, cu=0.012-0.021, fe=0.0009-0.0012, mu=12.5-13.0, pb=0.001, zn=1.5-1.75, cd=0.001-0.0012, cr=0.0037-0.0041, al=0.004-0.0055 and Cl=0.0055-0.0065, wherein PH=4.
3. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to claim 2, which is characterized in that: the cobalt washing mixed solution comprises the following components (unit g/l): co=80-100, mn=2-5, mg=15, ni=0.001, cu=0.01, zn=0.001, ca=0.05.
4. A method for obtaining a battery grade nickel sulfate solution by one-step half extraction of a nickel cobalt sulfate leaching solution according to claim 3, which is characterized in that: the anti-impurity mixed solution comprises the following components (unit g/l): mn=100-130, cu=20-30, zn=30, co=0.2, mg=2.
5. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to any one of claims 1 to 4, which is characterized in that: in the step (2), the P204 sodium soap organic phase reacts with the nickel cobalt sulfate leaching solution, and then 9-10-level countercurrent extraction is carried out at the temperature of 30-40 ℃ and then phase separation is carried out; the ratio of the P204 sodium soap organic phase to the nickel cobalt sulfate leaching solution is 2:1.
6. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to any one of claims 1 to 4, which is characterized in that: in the step (3), the P204 loaded organic phase is subjected to 8-10-level countercurrent washing at normal temperature by dilute hydrochloric acid with the concentration of 1.0 mol/L-2.0 mol/L, and the ratio of the washed P204 loaded organic phase to the hydrochloric acid solution with the concentration of 2mol/L-4mol/L is 10:1.
7. the method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to any one of claims 1 to 4, which is characterized in that: in the step (4), hydrochloric acid with the concentration of 2mol/L-4mol/L is used for carrying out back extraction on the P204 loaded organic phase after nickel washing, and the ratio of the P204 loaded organic phase after nickel washing to the hydrochloric acid solution with the concentration of 2mol/L-4mol/L is 8:1.
8. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to any one of claims 1 to 4, which is characterized in that: the concentration of NaOH solution in the step (1) is 25-30% by mass, and P204 and sulfonated kerosene are mixed according to the volume ratio of 1:3.
9. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to any one of claims 1 to 4, which is characterized in that: the method for obtaining the nickel cobalt sulfate leaching solution comprises the following steps:
step one, mixing raw ore containing cobalt nickel hydroxide with water for size mixing to obtain a solid-liquid ratio of 1: 2-3 raw material ore pulp;
step two, starting a stirrer, feeding the raw material ore pulp obtained in the step one, intermittently adding concentrated sulfuric acid into the stirrer after feeding, carrying out raw material leaching reaction for 60-90 min after adding acid, and controlling the end point PH to be less than or equal to 2.5;
step three, standing for 20-30 min after the reaction in the step two, and after the obtained leaching slurry is subjected to dense separation, overflowing the supernatant to a transfer tank to serve as a pre-iron-aluminum liquid and underflow slag for later use;
step four, a solid-liquid ratio is configured to be 1: 2-3, adding the raw material ore pulp serving as a precipitator into the iron and aluminum removing precursor solution obtained in the step three to perform iron and aluminum removing reaction, wherein the reaction time is more than or equal to 1h;
and fifthly, carrying out solid-liquid separation on the slurry obtained in the step four to obtain a purified nickel cobalt sulfate solution, and conveying the purified nickel cobalt sulfate solution to the downstream as an extraction raw solution to obtain iron-aluminum waste residues for later use.
10. The method for obtaining the battery grade nickel sulfate solution by one-step half extraction of the nickel cobalt sulfate leaching solution according to the claim/9, which is characterized in that: wherein the mass percentage concentration of the concentrated sulfuric acid is 93% -98%.
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| CN118880055A (en) * | 2024-07-11 | 2024-11-01 | 宜昌邦普宜化新材料有限公司 | A method for removing impurities from nickel sulfate stock solution and its application |
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| CN112708779A (en) * | 2020-12-08 | 2021-04-27 | 金川集团镍盐有限公司 | Preparation method of cobalt sulfate solution |
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| CN112708779A (en) * | 2020-12-08 | 2021-04-27 | 金川集团镍盐有限公司 | Preparation method of cobalt sulfate solution |
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| CN118880055A (en) * | 2024-07-11 | 2024-11-01 | 宜昌邦普宜化新材料有限公司 | A method for removing impurities from nickel sulfate stock solution and its application |
| CN118880055B (en) * | 2024-07-11 | 2026-01-02 | 宜昌邦普宜化新材料有限公司 | A method for removing impurities from nickel sulfate stock solution and its application |
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Application publication date: 20231003 |