CN114657394A - Method for removing impurities and purifying cobalt salt solution - Google Patents
Method for removing impurities and purifying cobalt salt solution Download PDFInfo
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- CN114657394A CN114657394A CN202210151889.8A CN202210151889A CN114657394A CN 114657394 A CN114657394 A CN 114657394A CN 202210151889 A CN202210151889 A CN 202210151889A CN 114657394 A CN114657394 A CN 114657394A
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- extraction
- cobalt
- salt solution
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
Abstract
The invention discloses a method for removing impurities and purifying a cobalt salt solution, which comprises the following steps: (1) first-stage extraction: extracting the cobalt salt solution to be subjected to impurity removal by using a P204 extracting agent at the temperature of 50-60 ℃ to remove impurities such as iron, manganese, zinc, copper and calcium; (2) second-stage extraction: under the condition of 20-26 ℃, separating cobalt, magnesium and nickel from P204 raffinate by using P507 extraction liquid, and then back-extracting cobalt by using sulfuric acid to obtain cobalt sulfate; (3) three-stage extraction: under the condition of 30-40 ℃, the P204 extracting agent, the N235 extracting agent and the solvent oil are mixed according to the part ratio of 0.5-1.5: 8, and then the mixture is added into the cobalt sulfate solution obtained by the extraction of the P507 extraction liquid for extraction, so as to further remove cadmium and lead in the cobalt sulfate solution and realize the impurity removal and purification of the cobalt salt solution.
Description
Technical Field
The invention relates to the technical field of cobalt salt extraction treatment, in particular to a method for removing impurities and purifying a cobalt salt solution.
Background
The cobalt salt is a substance composed of a cobalt ion and an acid group, and may contain other ions in a certain proportion. Cobalt salts are used to improve the adhesion of rubber to metal, are widely accepted and are widely used in products such as radial tires and steel hose.
In the existing metallurgical production, because other metal elements exist in the minerals, when the metallurgical production is carried out, a link of removing other impurities in a cobalt salt solution to improve the purity of the cobalt salt is particularly important, an extraction method is a traditional cobalt salt purification scheme, then, in most of the existing extraction methods, a rough process link is mostly adopted, and relatively no more fine research is carried out on the aspects of extraction temperature, composition of an extracting agent or pH adjustment of a system and the like.
Disclosure of Invention
Aiming at the situation of the prior art, the invention aims to provide the method for removing and purifying the cobalt salt solution, which is stable and reliable to implement, convenient to operate, good in purification effect and low in cost.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a method for removing impurities and purifying a cobalt salt solution is used for removing impurities of copper, manganese, iron, calcium and magnesium from the cobalt salt solution by adopting a three-stage extraction method, and comprises the following steps:
(1) first-stage extraction: extracting a cobalt salt solution to be subjected to impurity removal by using a P204 extracting agent at 50-60 ℃ to remove impurities such as iron, manganese, zinc, copper and calcium to obtain a P204 raffinate, wherein before the impurities such as iron, manganese, zinc, copper and calcium are removed, the temperature of an extraction mixed system is reduced to 15-20 ℃ at a cooling rate of 3-5 ℃/min;
(2) second-stage extraction: under the condition of 20-26 ℃, separating cobalt, magnesium and nickel from P204 raffinate by using P507 extraction liquid, and then back-extracting cobalt by using sulfuric acid to obtain cobalt sulfate, wherein when the practical sulfuric acid is used for back-extracting cobalt, the temperature of a back-extraction mixed system is adjusted to 10-15 ℃;
(3) three-stage extraction: under the condition of 30-40 ℃, mixing a P204 extracting agent, an N235 extracting agent and solvent oil according to the part ratio of 0.5-1.5: 8, and adding the mixture into a cobalt sulfate solution obtained by extracting P507 extraction liquid for extraction so as to further remove cadmium and lead in the cobalt sulfate solution, thereby realizing the impurity removal and purification of the cobalt salt solution.
As a possible implementation mode, in the step (1), the P204 extracting agent and sodium hydroxide are saponified according to the mixing ratio of 3: 1, the saponification rate of the saponified P204 extracting agent is 63% -65%, and impurities such as iron, manganese, zinc, copper and calcium are extracted after 2-stage saponification, 16-stage extraction, 4-stage washing, 5-stage back extraction, 3-stage purification and 1-stage water washing.
As a preferred embodiment, it is preferred that in the first stage extraction, in the 16 stages of extraction, a cobalt washing solution is also generated by washing with sulfuric acid, and the cobalt washing solution is sent to the cobalt salt solution to continue the first stage extraction.
As a possible embodiment, the P507 extract in step (2) is further saponified with sodium hydroxide at a mixing ratio of 3: 1, the saponification rate of the saponified P507 extractant is 53% to 55%, and cobalt, magnesium and nickel are separated from the P204 raffinate after 2-stage saponification, 7-stage extraction, 8-stage washing, 5-stage back extraction, 3-stage regeneration and 1-stage water washing.
As a possible embodiment, further, the first-stage extraction is: and (3) extracting the cobalt salt solution to be subjected to impurity removal by using a P204 extracting agent at the temperature of 54-56 ℃.
As a possible embodiment, further, the second-stage extraction is: and (3) separating cobalt, magnesium and nickel from the P204 raffinate by using a P507 extraction liquid at the temperature of 24-26 ℃.
As a possible embodiment, further, the one-stage extraction is carried out at pH 4.0. + -. 0.5.
As a possible embodiment, further, the two-stage extraction is performed at pH 5.0. + -. 0.5.
As a possible embodiment, further: the three-stage extraction is carried out under the condition of pH4.0 +/-0.5.
Based on the method, the invention also provides a production method of the cobalt salt solution, which comprises the method for removing impurities and purifying the cobalt salt solution.
By adopting the technical scheme, compared with the prior art, the invention has the beneficial effects that: the invention further optimizes and improves the impurity removal effect by skillfully adjusting the temperature of the three-stage extraction, particularly changing the solubility and chemical activity of the components by adopting a temperature difference method in the first-stage extraction process and the second-stage extraction process, so that cobalt salt with considerable purity can be obtained after the cobalt salt solution is extracted.
Detailed Description
Example 1
The embodiment of the invention provides a method for impurity removal and purification of a cobalt salt solution, which is used for removing impurities of copper, manganese, iron, calcium and magnesium from the cobalt salt solution by a three-stage extraction method and comprises the following steps:
(1) first-stage extraction: under the conditions of 50-53 ℃ and pH4.0 +/-0.5, saponifying the P204 extracting agent and sodium hydroxide according to the mixing ratio of 3: 1, wherein the saponification rate of the saponified P204 extracting agent is 63-65%, the saponified P204 extracting agent and a cobalt salt solution to be purified are subjected to 2-stage saponification, 16-stage extraction, 4-stage washing, 5-stage back extraction, 3-stage purification and 1-stage water washing to extract iron, manganese, zinc, copper and calcium impurities to obtain P204 raffinate, wherein before the iron, manganese, zinc, copper and calcium impurities are removed, the temperature of an extraction mixed system is reduced to 15-20 ℃ at the cooling rate of 3-5 ℃/min, a cobalt washing solution is generated in a 16-stage extraction section through sulfuric acid washing and is conveyed to the cobalt salt solution to continuously participate in the first-stage extraction;
(2) second-stage extraction: saponifying P507 extract liquid and sodium hydroxide according to the mixing ratio of 3: 1 under the conditions of 20-23 ℃ and pH5.0 +/-0.5, wherein the saponification rate of the saponified P507 extractant is 53-55%, the P507 extractant liquid and P204 raffinate liquid are subjected to 2-level saponification, 7-level extraction, 8-level washing, 5-level back extraction, 3-level regeneration and 1-level water washing to separate cobalt, magnesium and nickel from the P507 extractant liquid, and then back extraction of the cobalt is performed by using sulfuric acid to obtain cobalt sulfate, wherein when practical sulfuric acid is used for back extraction of the cobalt, the temperature of a back extraction mixed system is adjusted to 10-15 ℃;
(3) three-stage extraction: under the conditions of 30-33 ℃ and pH4.0 +/-0.5, mixing a P204 extracting agent, an N235 extracting agent and solvent oil according to the part ratio of 1.0: 8, and adding the mixture into a cobalt sulfate solution obtained by extracting a P507 extraction liquid for extraction so as to further remove cadmium and lead in the cobalt sulfate solution, thereby realizing the impurity removal and purification of the cobalt salt solution.
And (3) carrying out component determination on the obtained cobalt salt solution to obtain the percentage contents of iron, manganese, zinc, copper, calcium, nickel, cadmium and lead, wherein the obtained result is as follows: 0.4mg/L of iron, 0.3mg/L of manganese, 0.6mg/L of zinc, 0.3mg/L of copper, 0.8mg/L of calcium, 0.5mg/L of magnesium, 0.6mg/L of nickel, 0.7mg/L of cadmium and 0.4mg/L of lead.
Example 2
The embodiment of the invention provides a method for impurity removal and purification of a cobalt salt solution, which is used for removing impurities of copper, manganese, iron, calcium and magnesium from the cobalt salt solution by a three-stage extraction method and comprises the following steps:
(1) first-stage extraction: under the conditions of 54-56 ℃ and pH4.0 +/-0.5, saponifying the P204 extracting agent and sodium hydroxide according to the mixing ratio of 3: 1, wherein the saponification rate of the saponified P204 extracting agent is 63% -65%, the saponified P204 extracting agent and a cobalt salt solution to be purified are subjected to 2-stage saponification, 16-stage extraction, 4-stage washing, 5-stage back extraction, 3-stage purification and 1-stage water washing to extract iron, manganese, zinc, copper and calcium impurities to obtain P204 raffinate, wherein before the iron, manganese, zinc, copper and calcium impurities are removed, the temperature of an extraction mixed system is reduced to 15-20 ℃ at the cooling rate of 3-5 ℃/min, a cobalt washing solution is generated in a 16-stage extraction section through sulfuric acid washing and is conveyed to the cobalt salt solution to continuously participate in the first-stage extraction;
(2) second-stage extraction: saponifying P507 extract liquid and sodium hydroxide according to the mixing ratio of 3: 1 under the conditions of 20-23 ℃ and pH5.0 +/-0.5, wherein the saponification rate of the saponified P507 extractant is 53-55%, the P507 extractant liquid and P204 raffinate liquid are subjected to 2-level saponification, 7-level extraction, 8-level washing, 5-level back extraction, 3-level regeneration and 1-level water washing to separate cobalt, magnesium and nickel from the P507 extractant liquid, and then back extraction of the cobalt is performed by using sulfuric acid to obtain cobalt sulfate, wherein when practical sulfuric acid is used for back extraction of the cobalt, the temperature of a back extraction mixed system is adjusted to 10-15 ℃;
(3) three-stage extraction: under the conditions of 34-36 ℃ and pH4.0 +/-0.5, mixing a P204 extracting agent, an N235 extracting agent and solvent oil according to the part ratio of 0.5: 1.5: 8, and adding the mixture into a cobalt sulfate solution obtained by extracting P507 extract for extraction so as to further remove cadmium and lead in the cobalt sulfate solution and realize impurity removal and purification of the cobalt salt solution.
And (3) carrying out component determination on the obtained cobalt salt solution to obtain the percentage contents of iron, manganese, zinc, copper, calcium, nickel, cadmium and lead, wherein the obtained result is as follows: 0.3mg/L of iron, 0.4mg/L of manganese, 0.5mg/L of zinc, 0.4mg/L of copper, 0.7mg/L of calcium, 0.6mg/L of magnesium, 0.5mg/L of nickel, 0.6mg/L of cadmium and 0.5mg/L of lead.
Example 3
The embodiment of the invention provides a method for impurity removal and purification of a cobalt salt solution, which is used for removing impurities of copper, manganese, iron, calcium and magnesium from the cobalt salt solution by a three-stage extraction method and comprises the following steps:
(1) first-stage extraction: under the conditions of 57-60 ℃ and pH4.0 +/-0.5, saponifying the P204 extracting agent and sodium hydroxide according to the mixing ratio of 3: 1, wherein the saponification rate of the saponified P204 extracting agent is 63-65%, the saponified P204 extracting agent and a cobalt salt solution to be purified are subjected to 2-stage saponification, 16-stage extraction, 4-stage washing, 5-stage back extraction, 3-stage purification and 1-stage water washing to extract iron, manganese, zinc, copper and calcium impurities to obtain P204 raffinate, wherein before the iron, manganese, zinc, copper and calcium impurities are removed, the temperature of an extraction mixed system is reduced to 15-20 ℃ at the cooling rate of 3-5 ℃/min, a cobalt washing solution is generated in a 16-stage extraction section through sulfuric acid washing and is conveyed to the cobalt salt solution to continuously participate in the first-stage extraction;
(2) second-stage extraction: saponifying P507 extract liquid and sodium hydroxide according to the mixing ratio of 3: 1 under the conditions of 23-26 ℃ and pH5.0 +/-0.5, wherein the saponification rate of the saponified P507 extractant is 53-55%, the P507 extractant liquid and P204 raffinate liquid are subjected to 2-level saponification, 7-level extraction, 8-level washing, 5-level back extraction, 3-level regeneration and 1-level water washing to separate cobalt, magnesium and nickel from the P507 extractant liquid, and then back extraction of the cobalt is performed by using sulfuric acid to obtain cobalt sulfate, wherein when practical sulfuric acid is used for back extraction of the cobalt, the temperature of a back extraction mixed system is adjusted to 10-15 ℃;
(3) three-stage extraction: under the conditions of 37-40 ℃ and pH4.0 +/-0.5, mixing a P204 extracting agent, an N235 extracting agent and solvent oil according to the part ratio of 1.5: 0.5: 8, and adding the mixture into a cobalt sulfate solution obtained by extracting a P507 extraction liquid for extraction so as to further remove cadmium and lead in the cobalt sulfate solution, thereby realizing the impurity removal and purification of the cobalt salt solution.
And (3) carrying out component determination on the obtained cobalt salt solution to obtain the percentage contents of iron, manganese, zinc, copper, calcium, nickel, cadmium and lead, wherein the obtained result is as follows: 0.5mg/L of iron, 0.4mg/L of manganese, 0.5mg/L of zinc, 0.4mg/L of copper, 0.5mg/L of calcium, 0.4mg/L of magnesium, 0.5mg/L of nickel, 0.6mg/L of cadmium and 0.5mg/L of lead.
The foregoing is directed to embodiments of the present invention, and equivalents, modifications, substitutions and variations such as will occur to those skilled in the art, which fall within the scope and spirit of the appended claims.
Claims (10)
1. A method for removing impurities and purifying cobalt salt solution is used for removing impurities of copper, manganese, iron, calcium and magnesium from the cobalt salt solution by adopting a three-stage extraction method, and is characterized in that: which comprises the following steps:
(1) first-stage extraction: extracting a cobalt salt solution to be subjected to impurity removal by using a P204 extracting agent at 50-60 ℃ to remove impurities such as iron, manganese, zinc, copper and calcium to obtain a P204 raffinate, wherein before the impurities such as iron, manganese, zinc, copper and calcium are removed, the temperature of an extraction mixed system is reduced to 15-20 ℃ at a cooling rate of 3-5 ℃/min;
(2) second-stage extraction: under the condition of 20-26 ℃, separating cobalt, magnesium and nickel from P204 raffinate by using P507 extraction liquid, and then back-extracting cobalt by using sulfuric acid to obtain cobalt sulfate, wherein when the practical sulfuric acid is used for back-extracting cobalt, the temperature of a back-extraction mixed system is adjusted to 10-15 ℃;
(3) three-stage extraction: under the condition of 30-40 ℃, mixing a P204 extracting agent, an N235 extracting agent and solvent oil according to the part ratio of 0.5-1.5: 8, and adding the mixture into a cobalt sulfate solution obtained by extracting P507 extraction liquid for extraction so as to further remove cadmium and lead in the cobalt sulfate solution, thereby realizing the impurity removal and purification of the cobalt salt solution.
2. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the P204 extractant and sodium hydroxide are saponified according to the mixing ratio of 3: 1, the saponification rate of the saponified P204 extractant is 63% -65%, and impurities such as iron, manganese, zinc, copper and calcium are extracted through 2-level saponification, 16-level extraction, 4-level washing, 5-level back extraction, 3-level purification and 1-level water washing.
3. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 2, wherein the method comprises the following steps: in the first-stage extraction, cobalt washing liquid is generated in a 16-stage extraction stage through sulfuric acid washing, and the cobalt washing liquid is conveyed into a cobalt salt solution to continuously participate in the first-stage extraction.
4. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein the method comprises the following steps: and (3) saponifying the P507 extract liquid and sodium hydroxide according to the mixing ratio of 3: 1 in the step (2), wherein the saponification rate of the saponified P507 extract agent is 53-55%, and cobalt, magnesium and nickel are separated from the P204 raffinate after 2-stage saponification, 7-stage extraction, 8-stage washing, 5-stage back extraction, 3-stage regeneration and 1-stage water washing.
5. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein: the first-stage extraction comprises the following steps: and (3) extracting the cobalt salt solution to be subjected to impurity removal by using a P204 extracting agent at the temperature of 54-56 ℃.
6. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein the method comprises the following steps: the second-stage extraction comprises the following steps: and (3) separating cobalt, magnesium and nickel from the P204 raffinate by using a P507 extraction liquid at the temperature of 24-26 ℃.
7. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein the method comprises the following steps: the one-stage extraction is carried out under the condition of pH4.0 + -0.5.
8. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein the method comprises the following steps: the second-stage extraction is carried out under the condition of pH5.0 +/-0.5.
9. The method for impurity removal and purification of the cobalt salt solution as claimed in claim 1, wherein the method comprises the following steps: the three-stage extraction is carried out under the condition of pH4.0 +/-0.5.
10. A production method of a cobalt salt solution is characterized by comprising the following steps: which comprises a method for impurity removal and purification of a cobalt salt solution as claimed in one of claims 1 to 9.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101974687A (en) * | 2010-11-02 | 2011-02-16 | 安化金源新材料有限责任公司 | Extraction process for preparing electronic-grade cobalt sulfate from cobalt-containing waste material |
| CN102061390A (en) * | 2010-12-03 | 2011-05-18 | 安化金源新材料有限责任公司 | Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste |
| CN106222411A (en) * | 2016-08-26 | 2016-12-14 | 德清县立荣金属粉末有限公司 | Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution |
| US20190152797A1 (en) * | 2016-10-31 | 2019-05-23 | Hunan Jinyuan New Materials Co., Ltd. | Method for preparing nickel/manganese/lithium/cobalt sulfate and tricobalt tetraoxide from battery wastes |
| AU2020102537A4 (en) * | 2020-06-09 | 2020-11-19 | Bgrimm Technology Group | Method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide |
-
2022
- 2022-02-18 CN CN202210151889.8A patent/CN114657394A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974687A (en) * | 2010-11-02 | 2011-02-16 | 安化金源新材料有限责任公司 | Extraction process for preparing electronic-grade cobalt sulfate from cobalt-containing waste material |
| CN102061390A (en) * | 2010-12-03 | 2011-05-18 | 安化金源新材料有限责任公司 | Method for directly producing high-purity electronic level cobaltous sulfate by using cobalt-containing waste |
| CN106222411A (en) * | 2016-08-26 | 2016-12-14 | 德清县立荣金属粉末有限公司 | Three sections of extraction copper removals, manganese, ferrum, calcium, methods of magnesium are used from cobalt salt solution |
| US20190152797A1 (en) * | 2016-10-31 | 2019-05-23 | Hunan Jinyuan New Materials Co., Ltd. | Method for preparing nickel/manganese/lithium/cobalt sulfate and tricobalt tetraoxide from battery wastes |
| AU2020102537A4 (en) * | 2020-06-09 | 2020-11-19 | Bgrimm Technology Group | Method for preparing battery-grade nickel sulfate and cobalt sulfate from mixed nickel-cobalt hydroxide |
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