CN110747342A - Method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag - Google Patents
Method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- 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
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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Abstract
The invention discloses a method for producing a pure cobalt manganese sulfate solution by using zinc smelting cobalt slag. Firstly, acid washing and filter pressing are carried out on zinc smelting cobalt slag to obtain acid washing slag; washing and filter-pressing the obtained pickling slag to obtain washing slag; carrying out reduction leaching and filter pressing on the washing slag to obtain a leaching solution; carrying out vulcanization, cadmium removal and filter pressing on the leaching solution to obtain a vulcanized solution; adding oxidant into the vulcanized liquid to make Fe in the liquid2+Is oxidized into Fe3+Then adding neutralizing agent to regulate pH value of solution to make Fe3+Hydrolyzing to form precipitate, and performing filter pressing to obtain iron-removed liquid; adding a fluorinating agent into the liquid after iron removal for reaction and filter pressing to obtain a liquid after fluorination; and finally, extracting and phase splitting by adopting organic phase-to-phase fluorinated liquid to obtain raffinate, namely the pure cobalt manganese sulfate solution. Through the technical scheme of the invention, the problem can be solvedThe cobalt slag is difficult to sell, and valuable metals are not fully utilized.
Description
The technical field is as follows:
the invention belongs to the technical field of nonferrous smelting, and particularly relates to a method for producing a pure cobalt manganese sulfate solution from cobalt slag produced in zinc smelting.
Secondly, background art:
with the continuous development of the industry in China, the zinc smelting technology is also continuously improved. The traditional zinc smelting mode is zinc hydrometallurgy, and part of solid hazardous waste rich in valuable metals can be generated in the operation process, and if the solid hazardous waste is discharged to the external environment, the solid hazardous waste not only can pollute the environment, but also can cause waste to the valuable metals in waste residues.
Due to the existence of valuable metal cobalt in the zinc smelting raw material, part of purified cobalt slag can be produced in a wet process purification workshop, and after cadmium is recovered from the purified cobalt slag through a cadmium recovery process, zinc is further recovered through cobalt recovery to enrich cobalt, so that the zinc smelting cobalt slag is obtained. The cobalt content in the zinc smelting cobalt slag is about 20 percent, and the recovery value is high; however, the cobalt slag for zinc smelting has complex components, contains a large amount of manganese and zinc, and also contains a small amount of impurities such as cadmium, lead, iron, calcium, magnesium and the like, is difficult to sell, and has low direct sale price. Whereby the maximum benefit of the metal value cannot be achieved.
In recent years, with the rapid development of new energy automobiles, the maturity and wide application of the ternary battery technology, the price of cobalt metal is greatly increased, and the main raw materials in the ternary precursor are cobalt, manganese and nickel.
Thirdly, the invention content:
the technical problem to be solved by the invention is as follows: in order to overcome the defects of the prior art for treating cobalt slag generated by zinc smelting, the invention provides a method for recovering cobalt and manganese from the cobalt slag generated by zinc smelting, namely the invention provides a method for producing pure cobalt manganese sulfate solution from the cobalt slag generated by zinc smelting. By adopting the technical scheme of the invention, the technical problems that the cobalt slag is difficult to sell and valuable metals are not fully utilized can be effectively solved.
In order to solve the problems, the invention adopts the technical scheme that:
the invention provides a method for producing pure cobalt manganese sulfate solution by using zinc smelting cobalt slag, which comprises the following steps:
a. firstly, sequentially carrying out acid washing and filter pressing on zinc smelting cobalt slag to obtain acid washing slag;
b. b, washing the acid washing slag obtained in the step a with water, and performing filter pressing to obtain washing slag;
c. b, sequentially carrying out reduction leaching and filter pressing on the washing slag obtained in the step b to obtain a leaching solution;
d. c, sequentially carrying out vulcanization, cadmium removal and filter pressing on the leachate obtained in the step c to obtain a vulcanized liquid;
e. d, adding an oxidant into the vulcanized liquid obtained in the step d to enable Fe in the solution to be contained2+Is oxidized into Fe3+Then adding neutralizing agent to regulate pH value of solution to make Fe3+Hydrolyzing to form precipitate, and performing filter pressing to obtain iron-removed liquid;
f. adding a fluorinating agent into the deironing liquid obtained in the step e for reaction, and performing filter pressing after the reaction to obtain a fluorinated liquid;
g. and f, extracting and phase-splitting the fluorinated liquid obtained in the step f by adopting an organic phase to obtain raffinate, wherein the raffinate is the pure cobalt manganese sulfate solution.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, acid adopted in the acid washing in the step a is sulfuric acid, and water used in the acid washing is desalted water; during acid washing, the acid washing temperature is controlled to be 80-90 ℃, the initial acidity is 50-70 g/L, and the liquid-solid ratio is 3-5: 1, the reaction time is 2-4 h.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, demineralized water is adopted during washing in the step b; the temperature during washing is normal temperature, and the liquid-solid ratio is 3-5: 1, the washing time is 0.5-1 h.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, water adopted in the reduction leaching process in the step c is desalted water; the reducing agent is hydrogen peroxide or sulfur dioxide, the leaching acid is sulfuric acid, and the liquid-solid ratio is controlled to be 3-5: 1, the actual addition of sulfuric acid is 1.5-2.0 times of the theoretical dosage, the actual addition of hydrogen peroxide is 5-6 times of the theoretical dosage, the reaction temperature is 70-80 ℃, and the reaction time is 2-3 hours.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, the vulcanizing agent adopted in the cadmium removing process in the step d is manganese sulfide, the actual addition amount of the manganese sulfide is 10-15 times of the theoretical amount, the reaction temperature is normal temperature, the pH value of the solution before vulcanization is controlled to be 0.5-1.5, and the reaction time is 1-2 hours.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, in the step e, the oxidant is hydrogen peroxide, and the neutralizer is manganese carbonate; the actual adding amount of the hydrogen peroxide is 10-20 times of the theoretical using amount, the oxidation time is 0.5-1 h, and the reaction temperature is controlled to be 80-90 ℃; and controlling the pH value of the neutralization end point to be 4.5-5.0, and controlling the reaction time to be 1-2 h.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, the fluorinating agent in the step f is manganese fluoride, the actual addition amount of the manganese fluoride is 2-3 times of the theoretical amount, the reaction time is 1.5-2 h, and the reaction temperature is 90-95 ℃.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, the organic phase in the step g is P204 or P507, the organic phase is diluted by adopting a diluent sulfonated kerosene to form the solution with the concentration of 15-20%, the organic phase is diluted and then saponified by adopting the pure cobalt manganese sulfate solution, and the organic phase is saponified according to the ratio of 1: and 1, performing 10-15-grade countercurrent extraction on the fluorinated liquid.
According to the method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag, the pure cobalt manganese sulfate solution obtained in the step g is directly used for synthesizing the ternary battery anode material after adding cobalt sulfate, manganese sulfate and nickel sulfate according to the conventional proportion.
The invention has the following positive beneficial effects:
1. cobalt slag produced by zinc smelting belongs to hazardous waste, has complex components, is difficult to treat and sell, and has low valuation coefficient; according to the technical scheme, the zinc smelting cobalt slag can be further purified to produce a pure cobalt manganese sulfate solution, and the solution can be directly used for synthesizing the ternary battery anode precursor material according to the proportion. Thereby improving the value of valuable metals in the cobalt slag in zinc smelting. Meanwhile, waste is changed into valuable, and hazardous waste output in the operation process of the zinc smelting system is reduced.
2. The invention combines the market demand according to the characteristics of the enterprise. Cobalt slag produced by zinc smelting is used for deep processing treatment to prepare a pure cobalt manganese sulfate solution, and the solution can be directly used for synthesizing a ternary battery anode precursor material according to a ratio. The method avoids the conventional cobalt-manganese separation, changes the traditional two-section extraction process into one-section extraction, and simultaneously reduces the production cost.
In conclusion, the invention has obvious economic benefit and social benefit.
Fourthly, explanation of the attached drawings:
FIG. 1 is a schematic flow chart of a method for producing a pure cobalt manganese sulfate solution by using zinc smelting cobalt slag.
The fifth embodiment is as follows:
the invention is further illustrated by the following examples, which do not limit the scope of the invention.
Example 1:
the invention relates to a method for producing pure cobalt manganese sulfate solution by using zinc smelting cobalt slag, which comprises the following detailed steps:
a. firstly, adding demineralized water into the zinc smelting cobalt slag according to the liquid-solid ratio of 3:1 for slurrying, adding concentrated sulfuric acid according to the acidity of 70g/L, heating to 85 ℃, carrying out acid pickling for 4 hours, and carrying out filter pressing to obtain pickling slag;
b. b, adding desalted water into the acid washing slag obtained in the step a according to the liquid-solid ratio of 3:1 for slurrying, then washing the acid washing slag for 1h by adopting desalted water under the normal temperature condition, and performing filter pressing to obtain washing slag;
c. b, adding desalted water into the washing slag obtained in the step b according to a liquid-solid ratio of 3:1 for slurrying, then adding concentrated sulfuric acid with 2 times of theoretical dosage, maintaining the reaction temperature at 80 ℃, slowly adding hydrogen peroxide with 5 times of theoretical dosage, reacting for 2 hours, and carrying out filter pressing after reaction to obtain a leaching solution;
d. cooling the leachate obtained in the step c to normal temperature, adjusting the pH of the leachate to 0.5, adding manganese sulfide with the theoretical dosage being 10 times that of the leachate, reacting for 1 hour, and carrying out filter pressing after the reaction to obtain a vulcanized liquid;
e. d, adding hydrogen peroxide with the theoretical dosage being 10 times of that of the vulcanized liquid obtained in the step d to react for 0.5 hour, maintaining the reaction temperature at 80 ℃, adding a neutralizing agent manganese carbonate to adjust the pH value of the solution to 4.5, reacting for 1.5 hours, and performing filter pressing to obtain a liquid after iron removal;
f. maintaining the temperature of the iron-removed liquid obtained in the step e at 90 ℃, adding manganese fluoride with 2 times of theoretical dosage, reacting for 1.5h, and performing filter pressing after the reaction to obtain a fluorinated liquid;
g. diluting the organic phase P204 into 20% by using a diluent sulfonated kerosene, then saponifying by using a pure cobalt manganese sulfate solution, and comparing the obtained product with a reference value of 1: and 1, performing 13-stage countercurrent extraction on the fluorinated liquid, and splitting phases after extraction to obtain raffinate, namely pure cobalt manganese sulfate liquid.
Example 2:
the invention relates to a method for producing pure cobalt manganese sulfate solution by using zinc smelting cobalt slag, which comprises the following detailed steps:
a. firstly, adding demineralized water into the zinc smelting cobalt slag according to the liquid-solid ratio of 4:1 for slurrying, adding concentrated sulfuric acid according to the acidity of 60g/L, heating to 90 ℃, carrying out acid washing for 3 hours, and carrying out filter pressing to obtain acid washing slag;
b. b, adding desalted water into the acid washing slag obtained in the step a according to a liquid-solid ratio of 4:1 for slurrying, then washing the acid washing slag for 1h at normal temperature by adopting the desalted water, and performing filter pressing to obtain washing slag;
c. b, adding desalted water into the washing slag obtained in the step b according to a liquid-solid ratio of 4:1 for slurrying, then adding concentrated sulfuric acid with a theoretical dosage of 1.8 times, maintaining the reaction temperature at 75 ℃, slowly adding hydrogen peroxide with a theoretical dosage of 5.5 times, reacting for 2.5 hours, and carrying out filter pressing after reaction to obtain a leaching solution;
d. cooling the leachate obtained in the step c to normal temperature, adjusting the pH of the leachate to 1.0, adding manganese sulfide with the theoretical dosage being 12 times that of the leachate, reacting for 1.5h, and carrying out filter pressing after the reaction to obtain a vulcanized liquid;
e. d, adding hydrogen peroxide with the theoretical dosage being 15 times that of the vulcanized liquid obtained in the step d to react for 0.5 hour, maintaining the reaction temperature at 85 ℃, adding a neutralizing agent manganese carbonate to adjust the pH value of the solution to 4.5, reacting for 2.0 hours, and performing filter pressing to obtain a liquid after iron removal;
f. maintaining the temperature of the iron-removed liquid obtained in the step e at 95 ℃, adding manganese fluoride with 2.2 times of theoretical dosage, reacting for 2.0 hours, and performing filter pressing after the reaction to obtain a fluorinated liquid;
g. diluting the organic phase P204 into 20% by using a diluent sulfonated kerosene, then saponifying by using a pure cobalt manganese sulfate solution, and comparing the obtained product with a reference value of 1: 1, performing 12-stage countercurrent extraction on the fluorinated liquid, and splitting phases after extraction to obtain raffinate, namely pure cobalt manganese sulfate liquid.
Example 3:
the invention relates to a method for producing pure cobalt manganese sulfate solution by using zinc smelting cobalt slag, which comprises the following detailed steps:
a. firstly, adding demineralized water into the zinc smelting cobalt slag according to the liquid-solid ratio of 5:1 for slurrying, adding concentrated sulfuric acid according to the acidity of 50g/L, heating to 90 ℃, carrying out acid washing for 2 hours, and carrying out filter pressing to obtain acid washing slag;
b. b, adding desalted water into the acid washing slag obtained in the step a according to a liquid-solid ratio of 5:1 for slurrying, then washing the acid washing slag for 1h at normal temperature by adopting the desalted water, and performing filter pressing to obtain washing slag;
c. b, adding desalted water into the washing slag obtained in the step b according to a liquid-solid ratio of 5:1 for slurrying, then adding concentrated sulfuric acid with a theoretical dosage of 1.5 times, maintaining the reaction temperature at 70 ℃, slowly adding hydrogen peroxide with a theoretical dosage of 6 times, reacting for 2 hours, and carrying out filter pressing after reaction to obtain a leaching solution;
d. cooling the leachate obtained in the step c to normal temperature, adjusting the pH of the leachate to 1.5, adding manganese sulfide with 15 times of theoretical dosage, reacting for 2 hours, and performing pressure filtration after reaction to obtain a vulcanized liquid;
e. d, adding hydrogen peroxide with the theoretical dosage being 10 times of that of the vulcanized liquid obtained in the step d to react for 0.5 hour, maintaining the reaction temperature at 80 ℃, adding a neutralizing agent manganese carbonate to adjust the pH value of the solution to 5.0, reacting for 2.0 hours, and performing filter pressing to obtain a liquid after iron removal;
f. maintaining the temperature of the iron-removed liquid obtained in the step e at 95 ℃, adding manganese fluoride with 2.5 times of theoretical dosage, reacting for 2.0 hours, and performing filter pressing after the reaction to obtain a fluorinated liquid;
g. diluting the organic phase P204 into 15% by using a diluent sulfonated kerosene, then saponifying by using a pure cobalt manganese sulfate solution, and comparing the obtained product with a reference value of 1: 1, performing 10-stage countercurrent extraction on the fluorinated liquid, and splitting phases after extraction to obtain raffinate, namely pure cobalt manganese sulfate liquid.
Claims (9)
1. The method for producing the pure cobalt manganese sulfate solution by using the zinc smelting cobalt slag is characterized by comprising the following steps of:
a. firstly, sequentially carrying out acid washing and filter pressing on zinc smelting cobalt slag to obtain acid washing slag;
b. b, washing the acid washing slag obtained in the step a with water, and performing filter pressing to obtain washing slag;
c. b, sequentially carrying out reduction leaching and filter pressing on the washing slag obtained in the step b to obtain a leaching solution;
d. c, sequentially carrying out vulcanization, cadmium removal and filter pressing on the leachate obtained in the step c to obtain a vulcanized liquid;
e. d, adding an oxidant into the vulcanized liquid obtained in the step d to enable Fe in the solution to be contained2+Is oxidized into Fe3+Then adding neutralizing agent to regulate pH value of solution to make Fe3+Hydrolyzing to form precipitate, and performing filter pressing to obtain iron-removed liquid;
f. adding a fluorinating agent into the deironing liquid obtained in the step e for reaction, and performing filter pressing after the reaction to obtain a fluorinated liquid;
g. and f, extracting and phase-splitting the fluorinated liquid obtained in the step f by adopting an organic phase to obtain raffinate, wherein the raffinate is the pure cobalt manganese sulfate solution.
2. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: the acid adopted in the acid washing in the step a is sulfuric acid, and the used water is desalted water; during acid washing, the acid washing temperature is controlled to be 80-90 ℃, the initial acidity is 50-70 g/L, and the liquid-solid ratio is 3-5: 1, the reaction time is 2-4 h.
3. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: b, adopting desalted water for washing in the step b; the temperature during washing is normal temperature, and the liquid-solid ratio is 3-5: 1, the washing time is 0.5-1 h.
4. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: the water adopted in the reduction leaching process in the step c is desalted water; the reducing agent is hydrogen peroxide or sulfur dioxide, the leaching acid is sulfuric acid, and the liquid-solid ratio is controlled to be 3-5: 1, the actual addition of sulfuric acid is 1.5-2.0 times of the theoretical dosage, the actual addition of hydrogen peroxide is 5-6 times of the theoretical dosage, the reaction temperature is 70-80 ℃, and the reaction time is 2-3 hours.
5. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: and d, adopting manganese sulfide as a vulcanizing agent in the cadmium sulfide removal process in the step d, wherein the actual addition amount of the manganese sulfide is 10-15 times of the theoretical dosage, the reaction temperature is normal temperature, the pH value of the liquid before vulcanization is controlled to be 0.5-1.5, and the reaction time is 1-2 hours.
6. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: in the step e, the oxidant is hydrogen peroxide, and the neutralizer is manganese carbonate; the actual adding amount of the hydrogen peroxide is 10-20 times of the theoretical using amount, the oxidation time is 0.5-1 h, and the reaction temperature is controlled to be 80-90 ℃; and controlling the pH value of the neutralization end point to be 4.5-5.0, and controlling the reaction time to be 1-2 h.
7. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: in the step f, the fluorinating agent is manganese fluoride, the actual addition amount of the manganese fluoride is 2-3 times of the theoretical amount, the reaction time is 1.5-2 h, and the reaction temperature is 90-95 ℃.
8. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: and g, the organic phase is P204 or P507, the organic phase is diluted to be 15-20% by adopting a diluent sulfonated kerosene, the organic phase is diluted and then saponified by adopting pure cobalt manganese sulfate solution, and the organic phase is saponified according to the ratio of 1: and 1, performing 10-15-grade countercurrent extraction on the fluorinated liquid.
9. The method for producing pure cobalt manganese sulfate solution from zinc smelting cobalt slag according to claim 1, characterized in that: and g, adding cobalt sulfate, manganese sulfate and nickel sulfate into the pure cobalt sulfate manganese solution obtained in the step g according to a conventional proportion, and directly using the pure cobalt sulfate manganese solution for synthesizing the ternary battery anode material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111850305A (en) * | 2020-07-28 | 2020-10-30 | 昆明理工大学 | Method for leaching cobalt and manganese from manganese-rich cobalt slag |
| CN113005303A (en) * | 2021-03-26 | 2021-06-22 | 陕西锌业有限公司 | Method for extracting cobalt from cadmium-poor high-cobalt liquid |
| CN114410972A (en) * | 2021-12-25 | 2022-04-29 | 河南豫光锌业有限公司 | Method for preparing cobalt sulfate from zinc smelting cobalt slag |
| CN115044773A (en) * | 2022-06-17 | 2022-09-13 | 中伟新材料股份有限公司 | Method for recovering manganese and zinc from metal-containing slag |
| CN115418486A (en) * | 2022-09-22 | 2022-12-02 | 郑州大学 | Method for recovering cobalt and manganese in zinc purification slag by combining acid leaching-precipitation flotation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111850305A (en) * | 2020-07-28 | 2020-10-30 | 昆明理工大学 | Method for leaching cobalt and manganese from manganese-rich cobalt slag |
| CN113005303A (en) * | 2021-03-26 | 2021-06-22 | 陕西锌业有限公司 | Method for extracting cobalt from cadmium-poor high-cobalt liquid |
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| CN115044773A (en) * | 2022-06-17 | 2022-09-13 | 中伟新材料股份有限公司 | Method for recovering manganese and zinc from metal-containing slag |
| CN115418486A (en) * | 2022-09-22 | 2022-12-02 | 郑州大学 | Method for recovering cobalt and manganese in zinc purification slag by combining acid leaching-precipitation flotation method |
| CN115418486B (en) * | 2022-09-22 | 2024-02-23 | 郑州大学 | Method for jointly recovering cobalt and manganese in zinc purification slag by acid leaching-precipitation flotation method |
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