CN110983053A - Method for separating nickel, cobalt and manganese in nickel, cobalt and manganese raw material with high manganese-cobalt ratio - Google Patents
Method for separating nickel, cobalt and manganese in nickel, cobalt and manganese raw material with high manganese-cobalt ratio Download PDFInfo
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- CN110983053A CN110983053A CN201911369056.3A CN201911369056A CN110983053A CN 110983053 A CN110983053 A CN 110983053A CN 201911369056 A CN201911369056 A CN 201911369056A CN 110983053 A CN110983053 A CN 110983053A
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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
- 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
- C22B7/001—Dry processes
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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
- C22B23/02—Obtaining nickel or cobalt by dry processes
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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
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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
- C22B23/06—Refining
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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
- C22B47/00—Obtaining manganese
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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
- 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
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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
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a method for separating nickel, cobalt and manganese in a nickel, cobalt and manganese raw material with a high manganese-cobalt ratio, which comprises the following steps: calcining the high manganese-cobalt-ratio nickel-cobalt-manganese raw material, mixing the calcined raw material with an acid solution, heating to 90-100 ℃, reacting for 2-3 hours to obtain a nickel-cobalt solution and high manganese leaching residues, and further removing impurities from the nickel-cobalt solution and the high manganese leaching residues to obtain a pure nickel-cobalt solution and a manganese-containing product. The process can separate nickel, cobalt and manganese, has extremely low manganese content in the nickel-cobalt liquid, reduces the loss of the nickel-cobalt when the manganese is directly removed from the nickel-cobalt liquid, has simple process and low cost, achieves the effect of recycling resources completely, and is more convenient for subsequent further purification and processing.
Description
Technical Field
The invention relates to the technical field of battery recovery, in particular to a method for separating nickel and cobalt from manganese in a nickel-cobalt-manganese raw material with a high manganese-cobalt ratio.
Background
The lithium battery anode material mainly comprises lithium cobaltate, lithium nickel cobalt manganese oxide and lithium iron phosphate, is widely applied as a novel energy battery at present, and is widely applied to digital products such as mobile phones, notebook computers and the like due to the characteristics of high safety, high capacity and the like. With the rapid development of new energy industry, the number of the produced ternary nickel-cobalt-manganese hydroxide batteries is increased, and the recycling of battery materials is urgent.
The waste batteries and the waste nickel cobalt lithium manganate ionic batteries contain a large amount of nickel, cobalt, manganese and the like, have higher recovery value, and have lower recovery rates of nickel, cobalt and manganese for the separation of nickel, cobalt and manganese in the traditional high manganese-cobalt-ratio nickel cobalt manganese raw material, so that resources cannot be completely recycled, and great resource waste is caused.
Disclosure of Invention
The invention aims to: the method for separating the nickel, the cobalt and the manganese in the nickel, the cobalt and the manganese raw materials with the high manganese-cobalt ratio can separate the nickel, the cobalt and the manganese, the content of the manganese in the nickel, the cobalt liquid is extremely low, the loss of the nickel and the cobalt when the manganese is directly removed from the nickel, the process is simple, the cost is low, the effect of recycling resources completely is achieved, and meanwhile, the follow-up further purification and processing are more convenient.
The technical scheme adopted by the invention is as follows:
in order to achieve the aim, the invention provides a method for separating nickel, cobalt and manganese in a nickel, cobalt and manganese raw material with high manganese-cobalt ratio, which comprises the following steps:
calcining the high manganese-cobalt-ratio nickel-cobalt-manganese raw material, mixing the calcined raw material with an acid solution, heating to 90-100 ℃, reacting for 2-3 hours to obtain a nickel-cobalt solution and high manganese leaching residues, and further removing impurities from the nickel-cobalt solution and the high manganese leaching residues to obtain a pure nickel-cobalt solution and a manganese-containing product.
The further impurity removal of the nickel-cobalt solution comprises the following steps: heating the nickel-cobalt solution to 60-90 ℃, slowly adding oxalic acid solid with the addition amount being 1.4-1.7 times of the mass theoretically required for nickel-cobalt precipitation, reacting for 1-2 hours, filtering to obtain nickel-cobalt oxalate solid, and precipitating nickel-cobalt solution; calcining the nickel cobalt oxalate solid at 600-650 ℃ for 20-40 min to obtain a nickel cobalt oxide solid, and washing the nickel cobalt oxide solid twice to remove other impurities such as lithium oxide and the like; preparing a dilute sulfuric acid solution with the concentration of 40-50% (volume fraction), adding nickel cobalt oxide solid, dissolving to be neutral under heating, and filtering to obtain a pure nickel cobalt sulfate salt solution.
The further impurity removal steps of the high manganese leaching slag are as follows: continuously adding the high-manganese leached residues into 200-300 g/L dilute sulfuric acid solution, heating to 90-100 ℃, slowly dropwise adding hydrogen peroxide to react for 1-2 hours, wherein the adding amount is 7-10% (volume fraction), leaching is complete, and the residual slag rate is below 2%; heating the obtained leachate to 60-90 ℃, adding a calcined high manganese-cobalt ratio nickel-cobalt-manganese raw material for neutralization until the pH value is 6-7, heating the filtered neutralized solution to 50-80 ℃, adding 20-30% of sodium hydroxide solution until the pH value is 10-14, reacting for 1-2 hours, filtering, and washing filter residues for 2 times to obtain a nickel-cobalt-manganese hydroxide product.
Preferably, the nickel cobalt manganese raw material with the high manganese-cobalt ratio is a waste nickel cobalt lithium manganate positive electrode material of the ionic battery.
Preferably, the calcination temperature of the high manganese-cobalt-ratio nickel-cobalt-manganese raw material is 300-600 ℃.
Preferably, the calcination residence time of the high manganese-cobalt-ratio nickel-cobalt-manganese raw material is 5-10 min.
Preferably, the acid solution is a dilute sulfuric acid solution.
Preferably, the concentration of the dilute sulfuric acid solution is 200-250 g/L.
Preferably, the solid-to-liquid ratio of the high manganese-cobalt-ratio nickel-cobalt-manganese raw material to the acid solution is that 100-120 g of the high manganese-cobalt-ratio nickel-cobalt-manganese raw material is dissolved in every 1L of the acid solution.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
according to the invention, the nickel-cobalt solution and the high-manganese leaching slag are separated from the high-manganese-cobalt-ratio nickel-cobalt-manganese raw material, the nickel-cobalt and the manganese are separated, the content of the manganese in the nickel-cobalt solution is very low, the loss of the nickel-cobalt during the direct removal of the manganese from the nickel-cobalt solution is reduced, the process is simple, the cost is low, the effect of full recycling of resources is achieved, and the subsequent further purification and processing are more convenient.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Calcining the high manganese-cobalt-ratio nickel-cobalt-manganese raw material at 300 ℃, wherein the calcining retention time is about 8min, mixing the calcined raw material with 200g/L of dilute sulfuric acid solution (the solid-to-liquid ratio of the high manganese-cobalt-manganese raw material to acid solution is that 100g of the high manganese-cobalt-ratio nickel-cobalt-manganese raw material is dissolved in 1L of acid solution), heating to 90 ℃, reacting for 2 hours, obtaining nickel-cobalt solution and high manganese leaching residue, and further removing impurities from the nickel-cobalt solution and the high manganese leaching residue to obtain pure nickel-cobalt solution and manganese-containing products.
The further impurity removal of the nickel-cobalt solution comprises the following steps: heating the nickel-cobalt solution to 60-90 ℃, slowly adding oxalic acid solid with the addition amount being 1.4-1.7 times of the mass theoretically required for nickel-cobalt precipitation, reacting for 1-2 hours, filtering to obtain nickel-cobalt oxalate solid, and precipitating nickel-cobalt solution; calcining the nickel cobalt oxalate solid at 600-650 ℃ for 20-40 min to obtain a nickel cobalt oxide solid, and washing the nickel cobalt oxide solid twice to remove other impurities such as lithium oxide and the like; preparing a dilute sulfuric acid solution with the concentration of 40-50% (volume fraction), adding nickel cobalt oxide solid, dissolving to be neutral under heating, and filtering to obtain a pure nickel cobalt sulfate salt solution.
The further impurity removal steps of the high manganese leaching slag are as follows: continuously adding the high-manganese leached residues into 200-300 g/L dilute sulfuric acid solution, heating to 90-100 ℃, slowly dropwise adding hydrogen peroxide to react for 1-2 hours, wherein the adding amount is 7-10% (volume fraction), leaching is complete, and the residual slag rate is below 2%; heating the obtained leachate to 60-90 ℃, adding a calcined high manganese-cobalt ratio nickel-cobalt-manganese raw material for neutralization until the pH value is 6-7, heating the filtered neutralized solution to 50-80 ℃, adding 20-30% of sodium hydroxide solution until the pH value is 10-14, reacting for 1-2 hours, filtering, and washing filter residues for 2 times to obtain a nickel-cobalt-manganese hydroxide product.
Example 2
The difference between this example and example 1 is that the high manganese cobalt ratio nickel cobalt manganese raw material is calcined at 400 ℃, the calcination retention time is about 9min, the calcined raw material is mixed with 230g/L of dilute sulfuric acid solution (the solid-to-liquid ratio of the high manganese cobalt ratio nickel cobalt manganese raw material to the acid solution is 110g of the high manganese cobalt ratio nickel cobalt manganese raw material dissolved in 1L of the acid solution), the temperature is raised to 95 ℃ for reaction for 2 hours, nickel cobalt solution and high manganese leaching residue are obtained, and the nickel cobalt solution and the high manganese leaching residue are further subjected to impurity removal to obtain pure nickel cobalt solution and manganese-containing product.
Example 3
The difference between this example and example 1 is that the high manganese cobalt ratio nickel cobalt manganese raw material is calcined at 500 ℃, the calcination retention time is about 10min, the calcined raw material is mixed with 220g/L of dilute sulfuric acid solution (the solid-to-liquid ratio of the high manganese cobalt ratio nickel cobalt manganese raw material to the acid solution is 120g of the high manganese cobalt ratio nickel cobalt manganese raw material dissolved in 1L of the acid solution), the temperature is raised to 98 ℃ for reaction for 2.5 hours, so as to obtain nickel cobalt solution and high manganese leaching residue, and the nickel cobalt solution and the high manganese leaching residue are further purified to obtain pure nickel cobalt solution and manganese-containing product.
Example 4
The difference between this example and example 1 is that the high manganese cobalt ratio nickel cobalt manganese raw material is calcined at 550 ℃, the calcination retention time is about 5min, the calcined raw material is mixed with 210g/L of dilute sulfuric acid solution (the solid-to-liquid ratio of the high manganese cobalt ratio nickel cobalt manganese raw material to the acid solution is 120g of the high manganese cobalt ratio nickel cobalt manganese raw material dissolved in 1L of the acid solution), the temperature is raised to 100 ℃ for reaction for 3 hours, nickel cobalt solution and high manganese leaching residue are obtained, and the nickel cobalt solution and the high manganese leaching residue are further subjected to impurity removal to obtain pure nickel cobalt solution and manganese-containing product.
Example 5
The difference between this example and example 1 is that the high manganese cobalt ratio nickel cobalt manganese raw material is calcined at 600 ℃, the calcination retention time is about 7min, the calcined raw material is mixed with 250g/L of dilute sulfuric acid solution (the solid-to-liquid ratio of the high manganese cobalt ratio nickel cobalt manganese raw material to the acid solution is 120g of the high manganese cobalt ratio nickel cobalt manganese raw material dissolved in 1L of the acid solution), the temperature is raised to 93 ℃ for reaction for 2.5 hours, so as to obtain nickel cobalt solution and high manganese leaching residue, and the nickel cobalt solution and the high manganese leaching residue are further subjected to impurity removal to obtain pure nickel cobalt solution and manganese-containing product.
The leaching rate of nickel is 98.2-99.5%, the leaching rate of cobalt is 92.3-93.6%, 99.2-99.5% of manganese enters high-manganese leaching slag, and the content of manganese in the high-manganese leaching slag is 41.8-43.2%.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; these modifications and substitutions do not cause the essence of the corresponding technical solution to depart from the scope of the technical solution of the embodiments of the present invention, and are intended to be covered by the claims and the specification of the present invention.
Claims (7)
1. The method for separating nickel cobalt from manganese in the nickel cobalt manganese raw material with high manganese-cobalt ratio is characterized by comprising the following steps of:
calcining the high manganese-cobalt-ratio nickel-cobalt-manganese raw material, mixing the calcined raw material with an acid solution, heating to 90-100 ℃, reacting for 2-3 hours, separating to obtain a nickel-cobalt solution and high manganese leaching residues, and further removing impurities from the nickel-cobalt solution and the high manganese leaching residues to obtain a pure nickel-cobalt solution and a manganese-containing product.
2. The method for separating nickel cobalt from manganese in the high manganese cobalt ratio nickel cobalt manganese raw material according to claim 1, wherein the high manganese cobalt ratio nickel cobalt manganese raw material is a waste nickel cobalt lithium manganate positive electrode material of an ionic battery.
3. The method for separating nickel and cobalt from manganese in the high manganese-cobalt-ratio nickel-cobalt-manganese raw material according to claim 1, wherein the calcination temperature of the high manganese-cobalt-manganese raw material is 300-600 ℃.
4. The method for separating nickel cobalt from manganese in the high manganese cobalt ratio nickel cobalt manganese raw material according to claim 1, wherein the calcination residence time of the high manganese cobalt ratio nickel cobalt manganese raw material is 5-10 min.
5. The method of claim 1, wherein the acid solution is a dilute sulfuric acid solution.
6. The method for separating nickel cobalt from manganese in the high manganese-cobalt-ratio nickel-cobalt-manganese raw material according to claim 5, wherein the concentration of the dilute sulfuric acid solution is 200-250 g/L.
7. The method of claim 1, wherein the solid-to-liquid ratio of the high-manganese-to-cobalt-manganese raw material to the acid solution is such that 100-120 g of the high-manganese-to-cobalt-nickel-manganese raw material is dissolved in 1L of the acid solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115287458A (en) * | 2022-07-28 | 2022-11-04 | 荆门市格林美新材料有限公司 | Method for recovering valuable metals in lithium-containing power battery waste |
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| CN115287458A (en) * | 2022-07-28 | 2022-11-04 | 荆门市格林美新材料有限公司 | Method for recovering valuable metals in lithium-containing power battery waste |
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