KR20170106004A - Nickel powder fabrication method - Google Patents
Nickel powder fabrication method Download PDFInfo
- Publication number
- KR20170106004A KR20170106004A KR1020160029541A KR20160029541A KR20170106004A KR 20170106004 A KR20170106004 A KR 20170106004A KR 1020160029541 A KR1020160029541 A KR 1020160029541A KR 20160029541 A KR20160029541 A KR 20160029541A KR 20170106004 A KR20170106004 A KR 20170106004A
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- KR
- South Korea
- Prior art keywords
- nickel powder
- nickel
- active material
- alkali metal
- metal carbonate
- Prior art date
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/04—CO or CO2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/15—Nickel or cobalt
Abstract
A method for producing a nickel powder is disclosed. According to an embodiment of the present invention, there is provided a method for producing nickel powder from a cathode active material of a waste lithium ion battery, comprising: extracting the cathode active material from the waste lithium ion battery; pyrolyzing the cathode active material in a reducing gas atmosphere to oxidize There is provided a nickel powder production method comprising separating nickel and an alkali metal carbonate water and washing the nickel oxide and the alkali metal carbonate water to remove the alkali metal carbonate water and reducing the nickel oxide to form a nickel powder .
Description
An embodiment of the present invention relates to a method of manufacturing a nickel powder, and more particularly, to a method of producing a nickel powder from a spent lithium ion battery.
Nickel (Ni), which is often used as a raw material for stainless steel (STS), is an expensive metal used for various purposes. For example, nickel is also applied to nickel steel, stainless steel, nichrome steel, as well as special alloys and plating materials. In particular, magnetic fluids made of alloys of nickel, iron and cobalt are widely used as shock-absorbing fillers. In addition, since the nickel nanoparticles have a large surface area and are highly active, they are also used as a catalyst in an organic hydrogenation reaction or an exhaust gas treatment. It can also be used as a comburent in rocket solid fuels to increase combustion heat and combustion efficiency and improve oxidation stability.
Such nickel is also contained in lithium-based batteries. Most nickel-containing waste resources of lithium-based batteries generated in the country are sent to foreign countries and re-imported after being recycled. Loss of LNO generated in the process of manufacturing cathode active material of secondary battery is large every year, and studies for producing lithium tin oxide, nickel oxide and nickel metal are underway. As a method for producing nickel particles through a cathode active material precursor, a solvent extraction method, a chemical precipitation method, an electrolytic deposition method, a hydrogen reduction method, and a liquid phase reduction method are mainly applied.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart illustrating a dry reduction process of a conventional method for producing nickel metal powder from a spent lithium ion battery. FIG.
Referring to FIG. 1, a conventional nickel metal powder manufacturing method collects a waste lithium ion battery (S11), removes a case of the collected lithium ion battery, extracts a cathode material, and crushes and classifies the extracted cathode material (S12), and a raw material of LNO (Lithium Nickel Oxide) is obtained from the cathode material (S13). Then, the LNO raw material is subjected to heat treatment in an exhaust atmosphere (O2 atmosphere) (S14) S15), and Ni powder is recovered (S16). In the case of such a conventional dry flower process, LiO is generated from the LNO raw material by performing the heat treatment in the exhaust atmosphere, and LiO can not be reduced and remains as an impurity in the recovery of the nickel powder. Therefore, the purity of the finally obtained nickel powder is lowered.
In a conventional method for producing a nickel powder from a spent lithium ion battery, a liquid reduction process may be used instead of the dry reduction process. In the case of the liquid reduction process, the LNO source material is dissolved and then reduced through a compound such as an acid, which is advantageous in that the rate and yield of the reaction are lower than that of the dry reduction process. However, strong acid solution and other compounds harmful to the environment And the production process is complicated and a large amount of waste is generated. Therefore, a facility for treating the waste is required, and as a result, the production cost is lowered as a whole.
Therefore, there is a need for a novel process for improving this conventional nickel powder manufacturing process.
Embodiments of the present invention provide a method for manufacturing nickel powder that can increase the purity of final nickel powder.
In addition, embodiments of the present invention are intended to provide a process for producing environmentally friendly nickel powder.
In addition, embodiments of the present invention are intended to provide a method of manufacturing a nickel powder capable of reducing the production cost of nickel powder.
In addition, embodiments of the present invention are intended to provide a method for producing nickel powder that is simple in process and easy to be commercialized.
According to an embodiment of the present invention, there is provided a method of producing nickel powder from a cathode active material of a waste lithium ion battery, comprising: extracting the cathode active material from the waste lithium ion battery; pyrolyzing the cathode active material in a reducing gas atmosphere to oxidize There is provided a nickel powder production method comprising separating nickel and an alkali metal carbonate water and washing the nickel oxide and the alkali metal carbonate water to remove the alkali metal carbonate water and reducing the nickel oxide to form a nickel powder .
The nickel oxide may be NiO.
The cathode active material may be LiNiO 2 .
The alkali metal carbonate water may be lithium carbonate (Li 2 CO 3 ).
The lithium carbonate removed in the washing step may be recycled to lithium metal.
The reducing gas atmosphere for pyrolysis may include at least a portion of C, CO, and CO 2 .
The nickel oxide may be hydrogen (H 2 ) reduced.
According to the embodiments of the present invention, the alkali metal carbonate which can be removed by water washing by pyrolysis in a reducing gas atmosphere becomes an intermediate product, whereby the purity of the final nickel powder can be increased.
In addition, according to the embodiments of the present invention, it is possible to provide an environmentally friendly method of manufacturing a nickel powder by not using any harmful substance to the environment during the process.
Further, according to the embodiments of the present invention, no additional cost for treating harmful substances occurs, and consequently, the production cost of nickel powder can be reduced.
Further, according to the embodiments of the present invention, the entire process is simple, and commercialization is relatively easy.
1 is a flowchart showing a dry reduction process among conventional methods for producing nickel metal powder from a spent lithium ion battery
2 is a cross-sectional view of a flow regulator according to an embodiment of the present invention;
3 is an exploded cross-sectional view of a flow controller according to an embodiment of the present invention;
Hereinafter, specific embodiments of the present invention will be described with reference to the drawings. However, this is an exemplary embodiment only and the present invention is not limited thereto.
In the following description, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear. The following terms are defined in consideration of the functions of the present invention, and may be changed according to the intention or custom of the user, the operator, and the like. Therefore, the definition should be based on the contents throughout this specification.
The technical idea of the present invention is determined by the claims, and the following embodiments are merely a means for efficiently describing the technical idea of the present invention to a person having ordinary skill in the art to which the present invention belongs.
2 is a flowchart illustrating a method of manufacturing a nickel powder according to an embodiment of the present invention.
Referring to FIG. 2, a method of manufacturing a nickel powder according to an embodiment of the present invention may include a method of manufacturing a nickel powder from a cathode active material of a spent lithium ion battery. The method for producing nickel powder includes a step (S1) of extracting a positive electrode active material from a waste lithium ion battery, a step (S2) of separating the extracted positive electrode active material into nickel oxide and alkali metal carbonate by pyrolysis in a reducing gas atmosphere, And washing the alkali metal carbonate with water to remove the alkali metal carbonate by dissolution (S3), reducing the nickel oxide with the alkali metal carbonate removed (S4) to form a nickel powder (S5). Here, in the nickel powder production method described in Fig. 2, waste batteries are collected from the conventional nickel powder production method (step S11 of Fig. 1), and the extracted cathode material is pulverized, classified and filtered Step is omitted. That is, in FIG. 2, a method of manufacturing a nickel powder instead of the portion A in FIG. 1 will be described.
The cathode active material of the spent lithium ion battery may be LiNiO 2 , and the reducing gas atmosphere may include at least a portion of C, CO, and CO 2 . Li 2 CO 3 and NiO can be produced by thermal decomposition of LiNiO 2 in a reducing gas atmosphere. The formula is shown below.
When the produced Li 2 CO 3 and NiO are washed with water, Li 2 CO 3 can be dissolved in water and removed, so that only NiO can be left. When the remaining NiO is subjected to hydrogen reduction, only Ni of the metal can be formed into a powder form.
The nickel powder produced by this method may have a purity of 95 to 99%. On the other hand, when the conventional dry method, that is, LNO is heat-treated in an exhaust atmosphere (O 2 atmosphere), LiO and NiO are formed and it is difficult to remove LiO, so that the final nickel powder has a purity of 60 to 70% . Accordingly, when the nickel powder is prepared by the method of the present invention, the purity of the nickel powder can be significantly increased as compared with the prior art.
In addition, in the case of the conventional liquid reduction process, a strong acid solution and other compounds must be used as described above. According to the method of the present invention, no harmful substances may be used at all. Therefore, it is possible not only to form the nickel powder in an environmentally friendly manner, but also to reduce the production cost because there is no additional cost for treating harmful substances. Compared to the liquid-phase reduction process, the process according to one embodiment of the present invention is simple in process and relatively easy to commercialize.
FIG. 3 is a graph showing a phase of a material generated in each step of the method of manufacturing a nickel powder according to an embodiment of the present invention.
3 (b), 3 (c), and 3 (d) are graphs showing the relationship between the concentration of hydrogen in the extracted cathode active material, Represents the material after reduction.
3 (a), LiNiO 2 and NiO may be contained in the extracted cathode active material. When this is pyrolyzed in a reducing gas atmosphere, Li 2 CO 3 and NiO can be produced (FIG. 3 (b)). When the produced Li 2 CO 3 and NiO are washed with water, Li 2 CO 3 can be dissolved in water and can be removed, leaving only NiO (FIG. 3 (c)). Therefore, when the remaining NiO is subjected to hydrogen reduction, Ni metal may be generated.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is clearly understood that the same is by way of illustration and example only and is not to be taken by way of limitation, I will understand. Therefore, the scope of the present invention should not be limited to the above-described embodiments, but should be determined by equivalents to the appended claims, as well as the appended claims.
Claims (7)
Extracting the positive electrode active material from the spent lithium ion battery,
The cathode active material is pyrolyzed in a reducing gas atmosphere to separate the nickel oxide and the alkali metal carbonate,
The nickel oxide and the alkali metal carbonate water are washed with water to remove the alkali metal carbonate water,
And the nickel oxide is reduced to form a nickel powder.
Wherein the nickel oxide is NiO.
The positive electrode active material is LiNiO 2 The method of the nickel powder produced.
Wherein the alkali metal carbonate is lithium carbonate (Li 2 CO 3 ).
Wherein the lithium carbonate removed in the washing step is recycled to the lithium metal.
Wherein the reducing gas atmosphere for the pyrolysis includes at least a part of C, CO, and CO 2 .
The nickel oxide is a hydrogen (H 2) The method, the nickel powder is reduced.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020160029541A KR20170106004A (en) | 2016-03-11 | 2016-03-11 | Nickel powder fabrication method |
| PCT/KR2017/000061 WO2017155198A1 (en) | 2016-03-11 | 2017-01-03 | Method for producing nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020160029541A KR20170106004A (en) | 2016-03-11 | 2016-03-11 | Nickel powder fabrication method |
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| KR20170106004A true KR20170106004A (en) | 2017-09-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| KR1020160029541A KR20170106004A (en) | 2016-03-11 | 2016-03-11 | Nickel powder fabrication method |
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| KR (1) | KR20170106004A (en) |
| WO (1) | WO2017155198A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190091717A (en) * | 2018-01-29 | 2019-08-07 | 부경대학교 산학협력단 | Nickel powder fabrication method |
| WO2021132946A1 (en) * | 2019-12-26 | 2021-07-01 | 에스케이이노베이션 주식회사 | Method for recovering positive electrode active material precursor |
| KR20210083579A (en) * | 2019-12-27 | 2021-07-07 | 재단법인 포항금속소재산업진흥원 | Method for Collecting Valuable Metal from Cathode Materials of Waste Lithium Ion Battery |
| US11830992B2 (en) | 2019-03-27 | 2023-11-28 | Sk Innovation Co., Ltd. | Method of regenerating lithium precursor |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100325681B1 (en) * | 1999-02-03 | 2002-02-25 | 윤대근 | Transition metal recovering method from positive active materials of lithium ion cell |
| JP4385457B2 (en) * | 1999-11-19 | 2009-12-16 | 堺化学工業株式会社 | Method for producing fine spherical metal nickel fine powder |
| KR20110060040A (en) * | 2009-11-30 | 2011-06-08 | 한국지질자원연구원 | Method for making nano-particle from spent lithium ion batteries |
| JP5514844B2 (en) * | 2012-01-25 | 2014-06-04 | Ｊｘ日鉱日石金属株式会社 | Method for separating valuable metals from waste secondary batteries and method for recovering valuable metals using the same |
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- 2016-03-11 KR KR1020160029541A patent/KR20170106004A/en active Search and Examination
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- 2017-01-03 WO PCT/KR2017/000061 patent/WO2017155198A1/en active Application Filing
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190091717A (en) * | 2018-01-29 | 2019-08-07 | 부경대학교 산학협력단 | Nickel powder fabrication method |
| US11830992B2 (en) | 2019-03-27 | 2023-11-28 | Sk Innovation Co., Ltd. | Method of regenerating lithium precursor |
| WO2021132946A1 (en) * | 2019-12-26 | 2021-07-01 | 에스케이이노베이션 주식회사 | Method for recovering positive electrode active material precursor |
| KR20210083579A (en) * | 2019-12-27 | 2021-07-07 | 재단법인 포항금속소재산업진흥원 | Method for Collecting Valuable Metal from Cathode Materials of Waste Lithium Ion Battery |
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| Publication number | Publication date |
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| WO2017155198A1 (en) | 2017-09-14 |
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