CA3211556C - Method for producing nickel sulfate solution for secondary battery from nickel cathode - Google Patents

Method for producing nickel sulfate solution for secondary battery from nickel cathode Download PDF

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CA3211556C
CA3211556C CA3211556A CA3211556A CA3211556C CA 3211556 C CA3211556 C CA 3211556C CA 3211556 A CA3211556 A CA 3211556A CA 3211556 A CA3211556 A CA 3211556A CA 3211556 C CA3211556 C CA 3211556C
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cathode
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CA3211556A1 (en
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Jae Hoon Joo
Heon Sik Choi
Tae Kyung Lee
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Kemco
Korea Zinc Co Ltd
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Korea Zinc Co Ltd
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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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    • B01D—SEPARATION
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
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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
    • 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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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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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
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B2101/00—Type of solid waste
    • B09B2101/15—Electronic waste
    • B09B2101/16—Batteries
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    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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
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Abstract

A method for producing a nickel sulfate solution includes a leaching step of leaching a nickel cathode in sulfuric acid under a temperature of 170 degrees C to 200 degrees C and a pressure of 8.5 bar to 16 bar to produce a leachate, a neutralization step of neutralizing the leachate produced in the leaching step to produce a neutralized solution, and a filtration step of filtering the neutralized solution produced in the neutralization step to produce a filtrate, wherein a nickel concentration in the neutralized solution after the neutralization step is 120 to 140 g/L.

Description

METHOD FOR PRODUCING NICKEL SULFATE SOLUTION FOR SECONDARY
BATTERY FROM NICKEL CATHODE
TECHNICAL FIELD
100011 The present invention relates to a method for producing a nickel sulfate solution for a secondary battery from a nickel cathode.
BACKGROUND
[0002] Demand for secondary batteries is increasing as the IT industry and the markets for electric vehicles and energy storage system (ESS) are expanded. Accordingly, demand for nickel sulfate, which is used as a raw material for a cathode material of a secondary battery, is also increasing.
[0003] Conventionally, a nickel sulfate solution has been produced through a leaching process and an impurity purification process using a raw material such as a nickel concentrate, a mixed hydroxide precipitate (MHP) cake containing nickel, or the like. However, when a nickel sulfate solution is produced by leaching a raw material containing nickel in such a method that oxygen gas or ozone is added as an oxidizing agent under an atmospheric pressure condition, there is a problem in that the leaching efficiency is lowered.
SUMMARY
[0004] It is an object of the present invention to provide a method for producing a nickel sulfate solution, which is capable of enhancing the leaching efficiency while adding sulfuric acid and oxygen gas and/or nitrogen gas.
[0005] According to one embodiment of the present invention, there is provided a method for producing a nickel sulfate solution, including: a leaching step of leaching a nickel cathode in sulfuric acid under a high temperature and a high pressure to produce a leachate; a neutralization step of neutralizing the leachate produced in the leaching step to produce a neutralized solution;
and a filtration step of filtering the neutralized solution produced in the neutralization step to produce a filtrate.
[0006] According to one embodiment of the present invention, oxygen gas may be added in the leaching step.
[0007] According to one embodiment of the present invention, nitrogen gas may be added in the leaching step.
[0008] According to one embodiment of the present invention, the leaching step may be carried out at 170 to 200 degrees C.
[0009] According to one embodiment of the present invention, nickel powder may be added in the neutralization step.
[0010] According to one embodiment of the present invention, a nickel concentration in the neutralized solution after the neutralization step may be 120 to 140 g/L.
[0011] According to the present invention, it is possible to provide a method for producing a nickel sulfate solution, which is capable of enhancing leaching efficiency by adding oxygen gas and/or nitrogen gas under a high temperature and a high pressure.
[0012] According to the present invention, it is possible to provide a method for producing a nickel sulfate solution, which is capable of producing a nickel sulfate solution in a safer and more efficient method by adding nitrogen gas under a high temperature and a high pressure.
BRIEF DESCRIPTION OF THE DRAWINGS
[0013] FIG. 1 is a flowchart showing a process for producing a nickel sulfate solution for a secondary battery from a nickel cathode.
[0014] FIG. 2 is a graph showing the Ni dissolution rates in Examples and Comparative Examples after a leaching step.

DETAILED DESCRIPTION
100151 Embodiments of the present disclosure are illustrated for describing the technical spirit of the present disclosure. The scope of the claims according to the present disclosure is not limited to the embodiments described below or to the detailed descriptions of these embodiments.
100161 According to an embodiment of the present invention, a method for producing a nickel sulfate solution for a secondary battery from a nickel cathode includes a leaching step of adding water, sulfuric acid (H2SO4), oxygen (02) gas and/or nitrogen (N2) gas to a nickel cathode under a high temperature and a high pressure.
100171 The method for producing a nickel sulfate solution for a secondary battery from a nickel cathode according to the present invention includes a neutralization step of adding nickel powder to a leachate.
100181 The method for producing a nickel sulfate solution for a secondary battery from a nickel cathode according to the present invention includes a filtration step of filtering a neutralized solution and separating the neutralized solution into a filtrate and a cake.
100191 Hereinafter, the method according to the present invention will be described in detail with reference to FIG. 1.
[0020] Leaching Step (S100) [0021] The leaching step (S100) may include a step of cutting a nickel cathode into an appropriate leaching size, a step of putting the cut nickel cathode into an autoclave in an amount of about 2 equivalents of a target nickel concentration, and a step of performing a reaction under a condition of adding about 1 equivalent of sulfuric acid, oxygen gas and/or nitrogen gas at a temperature of 170 degrees C to 200 degrees C and a pressure of 8.5 bar to 16 bar for 5 to 24 hours. The nickel cathode may be cut into, for example, a size of 2 to 10 cm.
As used herein, the term "target nickel concentration" may be a nickel concentration in the neutralized solution after the neutralization step (S200) described later. Such a target nickel concentration may be set to an appropriate value in consideration of the solubility and temperature-dependent crystallization of nickel. If the nickel concentration after the neutralization step is less than 120 g/L, the efficiency in the subsequent crystallization step is lowered. If the nickel concentration after the neutralization step is larger than 140 g/L, nickel may be crystallized in the neutralization step when the temperature decreases. This may cause a loss of nickel during filtration.
Preferably, the target nickel concentration may be 120 to 140 g/L. If the reaction in the leaching step (S100) is performed at a temperature of less than 170 degrees C, the solubility of nickel is low, thereby lowering the efficiency. If the temperature exceeds 200 degrees C, there is no significant increase in the dissolution rate. Therefore, preferably, the leaching step (S100) may be performed at a temperature of 170 degrees C to 200 degrees C.
[0022] In one embodiment of the present invention, if the target nickel concentration is 120 g/L, the nickel cathode may be cut into a size of 2 to 10 cm and added in an amount of 2 equivalents (240 g/L), and 1 equivalent (200 g/L) of sulfuric acid may be added.
Thereafter, the leaching step (S100) may be performed by adding oxygen gas at a temperature of 170 degrees C to 180 degrees C or by adding nitrogen gas at a temperature of 180 degrees C to 200 degrees C.
[0023] When oxygen gas is added, a reaction may occur in which the added nickel reacts with sulfuric acid to become nickel sulfate, and hydrogen ions react with oxygen gas to produce water. At this time, a reaction in which a hydrogen gas is generated may also occur simultaneously. When oxygen gas is added, oxygen gas acts as an oxidizing agent to make the nickel leaching efficiency higher than when nitrogen gas is added. Reaction formulae in the case of adding oxygen gas are represented as follows.
[0024] Ni + 112SO4 + Y202 ¨> NiSO4 +1120 ... (1) [0025] Ni + 112SO4 ¨>NiSO4 + H2 ... (2) [0026] When nitrogen gas is added, a reaction may occur in which the added nickel reacts with sulfuric acid to become nickel sulfate and generate a hydrogen gas. In this case, since nitrogen gas is an inert gas having a very low reactivity, the hydrogen gas can be removed by discharging nitrogen gas together with the hydrogen gas. Therefore, when nitrogen gas is added, safety can be achieved as compared with the case where oxygen gas is added. The reaction formula in the case of adding nitrogen gas is the same as the above reaction formula (2).
[0027] Oxygen gas and nitrogen gas may be added in the leaching step (S100) together. Nitrogen gas may reduce the partial pressure of the hydrogen gas generated when oxygen gas is added, which makes it possible to perform a safer work.
[0028] In order to accelerate the leaching of nickel, a stirrer may be installed in the autoclave to dissolve the nickel cathode while stirring.
[0029] Neutralization Step (S200) [0030] The neutralization step (S200) is a step of neutralizing the leachate to a target pH range by adding nickel powder to the leachate when the leaching reaction has proceeded in the autoclave.
[0031] Thereafter, in order to concentrate the nickel sulfate solution by evaporation, it is necessary to lower the acidity. Since nickel is no longer leached into the solution when the pH
range is 6 to 7 or more, the preferred pH range may be 5.0 to 7Ø Preferably, the solution may be neutralized to pH 6 through the neutralization step (S200). The neutralization reaction formula is the same as the above reaction formula (2).
[0032] Since the purpose of the neutralization step (S200) is to neutralize the acidity of sulfuric acid present in the leachate, an appropriate amount of nickel powder that can efficiently achieve the preferred pH may be added. In the neutralization step (S200), for example, 1.5 to 3 equivalents of nickel powder may be added. Preferably, 2 equivalents of nickel powder (e.g., 12 g/L of nickel powder if the final acidity of the leachate is 10 g,/L) may be added. In the case of using nickel powder, the neutralization reaction occurs well due to high reactivity.
Therefore, it is preferable to use nickel powder. However, the neutralizing agent is not limited to the nickel powder as long as it can achieve the purpose of neutralization.
[0033] In the leachate, when oxygen gas is added at 180 degrees C, the final acidity may be about 8 g/L, and when nitrogen gas is added at 180 degrees C, the final acidity may be about 50 g/L. In addition, when nitrogen gas is added at 200 degrees C, the final acidity may be about 38 g/L. The addition of nitrogen gas makes the final acidity higher than the addition of oxygen gas. Therefore, a larger amount of nickel powder may be required to neutralize sulfuric acid.
However, as for the risk of explosion of a hydrogen gas, the addition of nitrogen gas may be a safer method than the addition of oxygen gas.
[0034] Filtration Step (S300) [0035] Since the metallic nickel not dissolved in the leaching step (S100) and the neutralization step (S200) remains in the neutralized solution as a solid component, the neutralized solution is transferred to and filtered by a filtration device. The nickel sulfate solution as a filtrate is sent to a purification step, and the cake is put into the neutralization step again. Nickel sulfate in the filtrate is crystallized through the purification step.
[0036] Example 1 [0037] In this example, a nickel sulfate solution was produced by leaching a nickel cathode in sulfuric acid. 2 equivalents of nickel cathode, 1 equivalent of sulfuric acid, and oxygen gas were added based on the target nickel (Ni) concentration of 120 g/L. A
reaction was carried out at 170 degrees C (8.5 bar) and 180 degrees C (10.5 bar) for 24 hours. The dissolution rates according to the reaction time are shown in Table 1 below.
[0038] In the neutralization step (S200), 2 equivalents of Ni powder are added to make a solution of 120 g/L of Ni at a temperature of 90 degrees C and a pH of 6Ø
[0039] The neutralized solution was filtered, the filtered nickel sulfate solution was sent to the purification step, and the cake was put into the neutralization step (S200) again.
[0040] [Table 1]
Reaction time (hr) 0 3 10 15 20 170 Ni dissolution rate (%) 0 37 55 74 degrees C Acidity (g/L) 200 127 91 53 41 180 Ni dissolution rate (%) 0 52 79 89 95 degrees C Acidity (g/L) 200 97 42 23 10 8 [0041] Example 2 [0042] 2 equivalents of nickel cathode, 1 equivalent of sulfuric acid, and nitrogen gas rather than oxygen gas were added. A reaction was carried out at 180 degrees C (10.5 bar) and 200 degrees C (16 bar) for 24 hours. The dissolution rates according to the reaction time are shown in Table 2 below.
[0043] The neutralization step (S200) and the filtration step (S300) are the same as those of Example 1.
[0044] [Table 21 Reaction time (hr) 0 3 10 15 20 24 180 Ni dissolution rate (%) 0 38 61 69 75 degrees C Acidity (g/L) 200 125 79 63 51 50 200 Ni dissolution rate (%) 0 57 79 80 81 degrees C Acidity (g/L) 200 87 42 40 39 38 [0045] Comparative Example 1 [0046] 2 equivalents of nickel cathode, 1 equivalent of sulfuric acid, and oxygen gas were added. A reaction was carried out at 95 degrees C (and atmospheric pressure) for 24 hours.
The dissolution rates according to the reaction time are shown in Table 3 below.
[0047] The neutralization step and filtration step are the same as those of Example 1.
[0048] Comparative Example 2 [0049] 2 equivalents of nickel cathode, 1 equivalent of sulfuric acid, and ozone were added.
100501 A reaction was carried out at 95 degrees C (and atmospheric pressure) for 24 hours.
The dissolution rates according to the reaction time are shown in Table 3 below.
[0051] The neutralization step and filtration step are the same as those of Example 1.
[0052] [Table 31 Date Recite/Date Received 2024-02-23 Reaction time (hr) 0 3 10 15 20 Comparative Ni dissolution rate (%) 0 1 2 2 2 example 1 Acidity (g,/L) 200 198 197 196 Comparative Ni dissolution rate (%) 0 2 6 10 16 example 2 Acidity (g,/L) 200 197 189 180 [0053] It can be seen that the Ni dissolution rates are very low in Comparative Example 1 in which oxygen gas was added at the atmospheric pressure and Comparative Example 2 in which ozone was added at the atmospheric pressure. On the other hand, the dissolution rates are very high in Examples 1 and 2 as compared with the Comparative Examples.
[0054] FIG. 2 is a graph showing the Ni dissolution rates in the Examples and the Comparative Examples after the leaching step. The dissolution rates in the Examples and the Comparative Examples can be compared.
[0055] That is, in Examples 1 and 2, nickel sulfate solutions can be efficiently produced by adding oxygen gas or nitrogen gas under a high temperature and a high pressure.
[0056] It should be understood that the embodiments described above are illustrative in all respects and not limitative. The scope of the present invention is defined by the claims rather than the detailed description. All changes or modifications derived from the meaning and scope of the claims and equivalent concepts thereof should be construed as being included in the scope of the present invention.

Claims (4)

WHAT IS CLAIMED IS:
1. A method for producing a nickel sulfate solution, comprising:
a leaching step of leaching a nickel cathode in sulfuric acid under a temperature of 170 degrees C to 200 degrees C and a pressure of 8.5 bar to 16 bar to produce a leachate;
a neutralization step of neutralizing the leachate produced in the leaching step to produce a neutralized solution; and a filtration step of filtering the neutralized solution produced in the neutralization step to produce a filtrate, wherein a nickel concentration in the neutralized solution after the neutralization step is 120 to 140 g/L.
2. The method of Claim 1, wherein oxygen gas is added in the leaching step.
3. The method of Claim 1 or 2, wherein nitrogen gas is added in the leaching step.
4. The method of Claim 1 or 2, wherein nickel powder is added in the neutralization step.

Date Recue/Date Received 2024-02-23
CA3211556A 2023-01-11 2023-03-31 Method for producing nickel sulfate solution for secondary battery from nickel cathode Active CA3211556C (en)

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KR1020230004092A KR102527172B1 (en) 2023-01-11 2023-01-11 Manufacturing process of nickel sulfate solution for lithium ion battery from nickel cathode
KR10-2023-0004092 2023-01-11
PCT/KR2023/004406 WO2023243832A1 (en) 2023-01-11 2023-03-31 Method for producing nickel sulfate solution for secondary battery from nickel cathode

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EP4711338A1 (en) 2024-09-16 2026-03-18 Umicore Controlled autoclave dissolution of metal powders for producing high-purity metal sulfate solutions
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Family Cites Families (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1223793A (en) 1969-03-25 1971-03-03 Sumitomo Metal Mining Co Process for producing aqueous solutions of nickel sulfate
RU2178931C1 (en) 2000-11-08 2002-01-27 Закрытое акционерное общество "Компания Сезар" Method of preparation of nickelous hydroxide for storage battery industry
RU2364641C2 (en) 2006-09-27 2009-08-20 Закрытое акционерное общество "Кузбассэлемент" Method of extracting nickel from dead alkaline battery sections
CN101768665A (en) 2008-12-30 2010-07-07 厦门紫金矿冶技术有限公司 Method for reducing acid consumption during heap leaching and high-pressure leaching of nickel laterite ore
KR101191042B1 (en) 2011-12-27 2012-10-15 강호길 Process for making high purified nickel sulfate from nickel concentrates, nickel matte
CN103757254A (en) * 2013-12-29 2014-04-30 四川师范大学 Method for leaching positive pole material of waste nickel-metal hydride battery
JP6168000B2 (en) * 2014-06-17 2017-07-26 住友金属鉱山株式会社 Method for producing nickel sulfate solution
JP2017115179A (en) * 2015-12-22 2017-06-29 日本リサイクルセンター株式会社 Collection method of valuable materials
WO2019090389A1 (en) * 2017-11-10 2019-05-16 Bhp Billiton Nickel West Pty Ltd Production of high purity nickel sulfate
CN112584949A (en) 2018-09-26 2021-03-30 松下知识产权经营株式会社 Method for producing nickel particles, method for producing nickel sulfate, and method for producing positive electrode active material for secondary battery
JP7183765B2 (en) * 2018-12-20 2022-12-06 住友金属鉱山株式会社 Method and apparatus for producing nickel sulfate solution
KR102152923B1 (en) 2018-12-21 2020-09-07 케이지에너켐(주) Manufacturing Method of Highly Purified Nickel Sulfate from the raw materials of Nickel, Cobalt and Manganese Mixed Sulfide Precipitation
KR102154599B1 (en) 2019-04-30 2020-09-10 코스모에코켐(주) Method for Separation and Recovery of Valuable Metals from Cathode Active Material
JP7279546B2 (en) 2019-07-02 2023-05-23 住友金属鉱山株式会社 Nickel oxide ore leaching method and hydrometallurgical method including the same
JP7380118B2 (en) 2019-11-18 2023-11-15 住友金属鉱山株式会社 Method for producing nickel sulfate
US20220411280A1 (en) * 2019-11-27 2022-12-29 Solvay Sa A process for manufacturing nickel sulphate
JP7354845B2 (en) 2020-01-15 2023-10-03 住友金属鉱山株式会社 Method for producing nickel sulfate aqueous solution
US12597651B2 (en) * 2020-05-15 2026-04-07 Queen's University At Kingston Hydrometallurgical recycling of lithium-ion battery electrodes
KR102451443B1 (en) 2020-06-08 2022-10-07 재단법인 포항산업과학연구원 Method for preparing nickel precusor for cathod active material
EP3967661B1 (en) 2020-09-09 2023-07-26 Northvolt AB Process for preparing battery grade metal sulphate solutions
JP2023551108A (en) * 2020-11-03 2023-12-07 ハッチ リミテッド Processing method for crystallizing metal sulfates
KR102266892B1 (en) * 2021-01-26 2021-06-18 (주)세화이에스 method for recovering nickel sulfate from waste comprising nickel
AU2021441001B2 (en) * 2021-04-14 2026-03-12 Metso Finland Oy Extraction of metals from lithium-ion battery material
CN113321248B (en) * 2021-06-23 2024-05-03 湖南金源新材料股份有限公司 Method for preparing electronic grade nickel sulfate from nickel powder, crystallization device and control method of crystallization device
JP7185090B1 (en) * 2022-01-05 2022-12-06 Ｊｘ金属株式会社 Metal recovery method for lithium-ion battery waste
CN114959252A (en) * 2022-05-30 2022-08-30 金川镍钴研究设计院有限责任公司 Method for producing nickel sulfate by using high-nickel matte

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