WO2016190669A1 - Procédé de récupération de poudre de cobalt à partir d'oxyde de lithium-cobalt - Google Patents

Procédé de récupération de poudre de cobalt à partir d'oxyde de lithium-cobalt Download PDF

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Publication number
WO2016190669A1
WO2016190669A1 PCT/KR2016/005555 KR2016005555W WO2016190669A1 WO 2016190669 A1 WO2016190669 A1 WO 2016190669A1 KR 2016005555 W KR2016005555 W KR 2016005555W WO 2016190669 A1 WO2016190669 A1 WO 2016190669A1
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WIPO (PCT)
Prior art keywords
cobalt oxide
cobalt
lithium
pyrolysis
powder
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PCT/KR2016/005555
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English (en)
Korean (ko)
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왕제필
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부경대학교 산학협력단
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Priority claimed from KR1020160064599A external-priority patent/KR101770513B1/ko
Publication of WO2016190669A1 publication Critical patent/WO2016190669A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides; Hydroxides

Definitions

  • the present invention relates to a method for recovering cobalt powder from lithium cobalt oxide, and more particularly, to a method for recovering cobalt powder from lithium cobalt oxide obtained from a cathode material of a secondary battery.
  • Cobalt is one of transition metals, and is widely used throughout the industry as a cathode material of a secondary battery, a super heat-resistant alloy, an ultra-light alloy, a catalyst and the like. In particular, cobalt is most commonly used in the secondary battery field, and is a strategic rare metal whose total amount is dependent on imports.
  • LiCoO 2 lithium-cobalt oxide
  • the liquid phase reduction method As a method for producing cobalt particles using lithium-cobalt oxide (LiCoO 2 ), pyrolysis, gas phase condensation, hydrogen reduction, liquid phase reduction, and the like are mainly used. Among them, the liquid phase reduction method has a faster reaction rate than other processes. The yield is high and it is mainly used. In addition, when the liquid phase reduction method, there is an advantage that the particle size and shape control of the cobalt particles is easy. Nevertheless, the liquid reduction method has a problem of increasing the amount of waste solution generated due to the use of organic substances or chemicals such as strong acids, which are harmful to the environment, and increases the production cost by adding costs for the treatment of the waste solution. In addition, in the process of producing cobalt particles by the liquid phase reduction method, a large amount of intermediate products are generated, there is a disadvantage in that the production process is complicated to process them.
  • LiCoO 2 lithium-cobalt oxide
  • One object of the present invention is to provide a method for producing cobalt powder through an environmentally friendly, simple process.
  • a method for recovering cobalt powder from lithium cobalt oxide for one purpose of the present invention is to use lithium cobalt oxide (LiCoO 2 ) in an oxygen-free reducing atmosphere containing at least one of carbon dioxide (CO 2 ) and carbon monoxide (CO). Pyrolysis step, among the lithium carbonate (Li 2 CO 3 ) and cobalt oxide (CoO) produced by the pyrolysis, to remove the lithium carbonate through a water washing step to obtain cobalt oxide, and the cobalt oxide obtained in the water washing step Reducing to powder.
  • LiCoO 2 lithium cobalt oxide
  • CO 2 carbon dioxide
  • CO carbon monoxide
  • the pyrolysis may be performed at 600 ° C. to 800 ° C.
  • the pyrolysis product generated in the pyrolysis step may be composed of only lithium carbonate (LiCO 3 ) and cobalt oxide (CoO).
  • the pyrolysis step includes disposing lithium-cobalt oxide (LiCoO 2 ) together with calcium carbonate (CaCO 3 ) in a reaction chamber under anoxic conditions, and a reaction chamber in which both lithium-cobalt oxide and calcium carbonate are present. Raising the temperature in the reactor to make the reaction chamber into a carbon dioxide atmosphere, and thermally decomposing the lithium-cobalt oxide in a reducing atmosphere under anoxic conditions under a carbon dioxide atmosphere.
  • LiCoO 2 lithium-cobalt oxide
  • CaCO 3 calcium carbonate
  • the step of pyrolyzing increases the temperature of the reaction chamber with lithium-cobalt oxide (LiCoO 2 ) disposed in the reaction chamber under anoxic conditions, and the temperature of the reaction chamber is 600 ° C. to 800 ° C. Injecting at least one gas of carbon monoxide and carbon dioxide directly into the reaction chamber, and maintaining a temperature of the reaction chamber in which at least one gas of carbon monoxide and carbon dioxide is injected at 600 ° C to 800 ° C. And pyrolyzing lithium-cobalt oxide (LiCoO 2 ) in a reducing atmosphere under anoxic conditions.
  • lithium-cobalt oxide LiCoO 2
  • the reducing may be performed in a reducing atmosphere in anoxic conditions.
  • the hydrogen gas may be directly injected in a state where the temperature of the chamber in which the cobalt oxide is disposed is 800 ° C to 1,000 ° C.
  • the cobalt powder is a simple process of performing pyrolysis in a reducing atmosphere under anoxic conditions as a dry process and selectively separating only cobalt oxide in the pyrolysis product, followed by hydrogen reduction. It can be easily recovered.
  • Obtaining pyrolysis products through the pyrolysis process of lithium-cobalt oxide, which is carried out in such a dry manner, is environmentally friendly because it does not use any harmful substances to the environment, unlike the conventional liquid reduction process, and saves costs for the treatment of waste solutions. There is an advantage to this.
  • FIG. 1 is a flowchart illustrating a recovery method of cobalt powder according to an embodiment of the present invention.
  • SEM scanning electron micrograph
  • FIG. 7 is an XRD graph of a pyrolysis product formed according to Comparative Example 1.
  • FIG. 8 is an XRD graph of a pyrolysis product produced in the preparation of the present invention for comparison with the XRD analysis result of FIG. 7.
  • FIG. 9 is an XRD graph of a pyrolysis product formed in accordance with Comparative Example 2.
  • FIG. 1 is a flowchart illustrating a recovery method of cobalt powder according to an embodiment of the present invention.
  • the method for preparing cobalt powder first, pyrolysis of lithium-cobalt oxide (LiCoO 2 ) in a reducing atmosphere under anoxic conditions is performed (step S110).
  • the reducing atmosphere under anoxic conditions means an inert atmosphere substantially free of oxygen, and oxygen contained in the chamber for pyrolysis of lithium-cobalt oxide (LiCoO 2 ) for the inert atmosphere is completely discharged to the outside and nitrogen It refers to a state in which only an inert gas such as gas (N 2 ) and / or argon gas (Ar) is present in the chamber.
  • the lithium is a thermal cracking process of the cobalt oxide (LiCoO 2), a reducing atmosphere of an oxygen-free conditions, specifically lithium-temperature was raised to high temperatures the temperature of the chamber in the deployed state of cobalt oxide (LiCoO 2), a specific temperature After reaching the carbon dioxide (CO2) and / or carbon monoxide (CO) may be carried out by direct injection into the chamber is heated to a high temperature. At this time, the temperature of the chamber is preferably raised to a temperature of 600 °C to 800 °C.
  • the pyrolysis products include only lithium carbonate (Li 2 CO 3 ) and cobalt oxide (CoO) containing divalent cobalt.
  • the pyrolysis product includes only two phases of lithium carbonate (Li 2 CO 3 ) and cobalt oxide (CoO).
  • lithium cobalt oxide LiCoO 2
  • pyrolysis of lithium cobalt oxide does not occur properly, but rather lithium carbonate (Li 2 CO 3 ) and cobalt oxide when it exceeds 800 ° C.
  • pure cobalt powder from cobalt oxide is difficult to completely separate lithium carbonate and cobalt oxide in a subsequent process as a by-product other than (CoO), for example, a compound containing at least three metals other than lithium carbonate and cobalt oxide is produced. Cannot be obtained. Therefore, the pyrolysis process is preferably performed at least 600 °C, preferably from 600 °C to 800 °C.
  • the temperature of the reaction chamber is raised to 600-800 ° C. to produce carbon dioxide from calcium carbonate.
  • Carbon dioxide may be supplied to pyrolysis of lithium-cobalt oxide (LiCoO 2 ). That is, while raising the reaction chamber to the temperature for pyrolysis of lithium-cobalt oxide (LiCoO 2 ), calcium carbonate is first pyrolyzed to become carbon dioxide gas, so a separate process of injecting carbon dioxide is omitted, and inexpensive calcium carbonate is carbon dioxide. It can be used as a source of.
  • step S120 the pyrolysis product produced by the pyrolysis process is washed with water to obtain only cobalt oxide.
  • lithium carbonate and cobalt oxide may be separated through the washing process. That is, in a pyrolysis product containing only two phases, lithium carbonate is highly soluble in water and cobalt oxide is not soluble in water, and thus lithium carbonate dissolved in water from the pyrolysis product through a washing process in which the pyrolysis product is dissolved in water. And cobalt oxide in the solid phase can be selectively obtained. In this case, a drying process may be further performed on the cobalt oxide separated from the solution in which lithium carbonate is dissolved.
  • the volume ratio of water and powder in the washing step can be set to 10: 1 or more and less than 2: 8.
  • the powder refers to a pyrolysis product composed of lithium carbonate and cobalt oxide produced through a pyrolysis process, and water is preferably at least 30% or more when the total volume of water and powder is 100%. More preferably, the volume ratio of water and powder is from 10: 1 to 5: 5 so that water is at least the same volume as the powder or more may be used. In the actual experiment, it was confirmed that lithium carbonate was not completely removed when the volume ratio of water and powder was 2: 8 or 1:10.
  • the cobalt oxide separated through the washing process is reduced to recover the cobalt powder (step S130).
  • Cobalt oxide can be recovered by converting it into cobalt powder through a hydrogen reduction process.
  • the hydrogen reduction process of the cobalt oxide may be carried out at a temperature of 800 to 1,000 °C. In addition, the hydrogen reduction process may be performed for 1 to 5 hours.
  • the hydrogen reduction process may be performed by injecting hydrogen gas while the temperature of the chamber is heated to a temperature of at least 800 ° C. while injecting argon gas to maintain a reducing atmosphere in anoxic conditions.
  • a cooling process may be additionally performed. If the temperature of the hydrogen reduction step is less than 800 ° C., there is a problem that cobalt oxide which is not reduced remains. If the temperature of the hydrogen reduction step exceeds 1,000 ° C., there is a problem of lowering the energy efficiency of the reduction step. Therefore, it is preferable that the temperature of a hydrogen reduction process is 800 degreeC-1,000 degreeC.
  • the temperature of the hydrogen reduction process is reached at a temperature increase rate of 10 ° C./min while argon gas is injected at 100 cc / min.
  • the temperature may be raised so that the hydrogen reduction reaction may be performed by injecting hydrogen gas into the chamber at 100 cc / min to 500 cc / min after reaching a temperature of 800 to 1,000 ° C.
  • argon gas is injected again at 100 cc / min and cooled at a rate of 10 ° C./min.
  • a cobalt powder recovery apparatus for performing the cobalt powder recovery method described in FIG. 1, a pyrolysis chamber for pyrolyzing lithium-cobalt oxide (LiCoO 2 ), the pyrolysis chamber connected to the pyrolysis chamber
  • the apparatus for recovering cobalt powder includes a washing chamber provided with the pyrolysis product generated in the above, and a washing chamber in which the washing process of the pyrolysis product is performed, and a reducing chamber connected to the washing chamber and selectively provided with only cobalt oxide to reduce cobalt oxide.
  • the pyrolysis chamber and the reduction chamber may be set to have a reducing atmosphere under anoxic conditions for performing each process.
  • the cobalt powder may be manufactured in a simple process by a dry process including pyrolysis and hydrogen reduction steps.
  • This dry process is environmentally friendly, since it does not use any harmful substances to the environment, unlike the conventional liquid reduction process, there is an advantage that can reduce the cost for the treatment of waste solutions at source.
  • Lithium-cobalt oxide (LiCoO 2 ) was recovered from the spent battery, placed in a reaction chamber, and formed in a reducing atmosphere under anoxic conditions, and then the temperature of the chamber was raised to 600 ° C. Carbon dioxide is injected directly into the reaction chamber at the elevated temperature to make the reaction chamber into a carbon dioxide atmosphere. The pyrolysis process was performed by raising the temperature of the reaction chamber to 700 ° C. under a carbon dioxide atmosphere.
  • lithium carbonate and cobalt oxide produced by pyrolysis were dissolved in water, and only undissolved cobalt oxide was selectively recovered in powder form. At this time, the volume ratio of water, the product lithium carbonate and cobalt oxide was 8: 2.
  • a cobalt powder was prepared by performing a hydrogen reduction process on the selectively recovered cobalt oxide powder.
  • the hydrogen reduction process while raising the argon gas (Ar) at 100 cc / min at a rate of temperature increase of 10 °C / min to 800 °C, hydrogen gas (H 2 ) 300 cc in the state reaching 800 °C By injection at / min.
  • argon gas was injected again at 100 cc / min, cooled at a rate of 10 ° C./min, and finally cobalt powder was prepared.
  • XRD analysis was performed on lithium-cobalt oxide and the results are shown in FIG. 2.
  • XRD analysis was performed on each of Sample 1, which is a pyrolysis product after the pyrolysis process, Sample 2, which is a cobalt oxide obtained after the washing step with respect to the product, and Sample 3, which is a cobalt powder after the hydrogen reduction process, and the results are shown in FIG. 3A. 3B and 3C, respectively.
  • FIG. 2 is an XRD graph of lithium-cobalt oxide
  • FIGS. 3, 4 and 5 are XRD graphs of products generated at each step of FIG. 1.
  • the x axis represents the diffraction angle (2 ⁇ , unit °) and y represents intensity (unit a.u.).
  • lithium cobalt oxide As a result of XRD analysis of lithium cobalt oxide as a raw material, it can be seen that diffraction peaks appear at a diffraction angle corresponding to the crystal structure of lithium cobalt oxide (LiCoO 2 ).
  • FIG. 3 which is an XRD analysis result for Sample 1, it can be seen that diffraction peaks appear at diffraction angles corresponding to crystal structures of lithium carbonate (denoted by ⁇ ) and cobalt oxide (denoted by ⁇ ). That is, it can be seen that lithium carbonate and cobalt oxide are produced from the lithium cobalt oxide by the pyrolysis process.
  • FIG. 4 is an XRD analysis result for Sample 2, it can be seen that diffraction peaks appear at a diffraction angle corresponding to the crystal structure of cobalt oxide. That is, through the washing process, it can be confirmed that the lithium carbonate is removed so that only cobalt oxide remains.
  • SEM scanning electron micrograph
  • the molar ratio of 1M of lithium-cobalt oxide (LiCoO2) in powder form, which is a cathode material, separated from a waste lithium secondary battery is determined.
  • decomposition was performed by heat treatment in an oxidizing atmosphere (air atmosphere).
  • the heat treatment temperature was 700 ° C., and the heat treatment time was 1 hour.
  • the pyrolysis product obtained through the above pyrolysis process was analyzed through XRD. The result is shown in FIG.
  • FIG. 7 is an XRD graph of a pyrolysis product formed according to Comparative Example 1
  • FIG. 8 is an XRD graph of a pyrolysis product produced in a preparation example of the present invention for comparison with the XRD analysis result of FIG.
  • pyrolysis products of lithium-cobalt oxide (LiCoO 2 ) when pyrolyzed in an oxidizing atmosphere according to Comparative Example 1 were used .
  • 14 Co 0 .86 O structure lithium-contained it can be seen that the cobalt oxide.
  • cobalt oxide of “CoO” type is not formed. Therefore, the pyrolysis product produced in the oxidizing atmosphere cannot be separated from the lithium carbonate by only cobalt oxide inherently by washing with water.
  • the pyrolysis product generated in the pyrolysis process of the preparation example of the present invention shows an XRD peak that is accurately separated into two phases of cobalt oxide (CoO) and lithium carbonate (Li 2 CO 3 ). It can be seen that. That is, in the present invention, since a pyrolysis product including exactly two phases is formed, only cobalt oxide can be obtained by removing lithium carbonate in a subsequent washing step, and cobalt powder can be easily recovered through reduction of cobalt oxide. It can be.
  • the pyrolysis product was obtained through substantially the same process as the pyrolysis process according to the preparation example of the present invention except that the temperature for pyrolysis in the pyrolysis process was 500 ° C. XRD analysis of the pyrolysis product was carried out and the results are shown in FIG. 9.
  • FIG. 9 is an XRD graph of a pyrolysis product formed in accordance with Comparative Example 2.
  • Comparative Example 3 except that the pyrolysis product was obtained through substantially the same process as Comparative Example 2 except that the temperature for pyrolysis was 900 ° C, cobalt oxide was not produced as in Comparative Examples 1 and 2. It was confirmed that a composite oxide phase having all lithium cobalt was formed.
  • the temperature of the pyrolysis process should be more than 500 ° C and less than 900 ° C, and is carried out at 600 ° C to 800 ° C. It can be confirmed that it is preferable.

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  • Inorganic Chemistry (AREA)
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Abstract

L'invention concerne un procédé permettant de récupérer de la poudre de cobalt comprenant les étapes de : pyrolyse d'un oxyde de lithium et de cobalt (LiCoO2) dans une atmosphère réductrice exempte d'oxygène contenant du dioxyde de carbone (CO2) et/ou du monoxyde de carbone (CO) ; élimination du carbonate de lithium à partir du carbonate de lithium (Li2CO3) et de l'oxyde de cobalt (CoO), qui sont générés à partir de la pyrolyse, par un processus de lavage, pour obtenir de l'oxyde de cobalt ; et réduction de l'oxyde de cobalt, qui est obtenu dans le processus de lavage, en une poudre de cobalt.
PCT/KR2016/005555 2015-05-26 2016-05-26 Procédé de récupération de poudre de cobalt à partir d'oxyde de lithium-cobalt WO2016190669A1 (fr)

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KR10-2015-0072643 2015-05-26
KR20150072643 2015-05-26
KR10-2016-0064599 2016-05-26
KR1020160064599A KR101770513B1 (ko) 2015-05-26 2016-05-26 리튬-코발트 산화물로부터 코발트 분말의 회수 방법

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3715486A1 (fr) * 2019-03-27 2020-09-30 SK Innovation Co., Ltd. Procédé de régénération d'un précurseur de lithium
CN114433861A (zh) * 2022-01-24 2022-05-06 安徽寒锐新材料有限公司 一种草酸钴制备钴粉的方法

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KR100287974B1 (ko) * 1993-08-12 2001-05-02 칼 하인쯔 슐츠, 페터 캘레르트 코발트/산화코발트분말, 그의 제조 방법 및 그의 용도
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KR20130059126A (ko) * 2011-11-28 2013-06-05 이상로 폐 리튬 이차전지로부터의 유가금속 회수 방법
KR20140126943A (ko) * 2013-04-24 2014-11-03 타운마이닝캄파니(주) 폐 리튬 이온전지의 양극물질로부터 유가 금속을 회수하는 방법

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KR100287974B1 (ko) * 1993-08-12 2001-05-02 칼 하인쯔 슐츠, 페터 캘레르트 코발트/산화코발트분말, 그의 제조 방법 및 그의 용도
KR20110024856A (ko) * 2009-09-03 2011-03-09 타운마이닝캄파니(주) 폐 리튬 이차전지의 양극물질로부터 리튬 화합물을 회수하는 방법
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3715486A1 (fr) * 2019-03-27 2020-09-30 SK Innovation Co., Ltd. Procédé de régénération d'un précurseur de lithium
CN111755766A (zh) * 2019-03-27 2020-10-09 Sk新技术株式会社 锂前驱体的再生方法
US11830992B2 (en) 2019-03-27 2023-11-28 Sk Innovation Co., Ltd. Method of regenerating lithium precursor
CN111755766B (zh) * 2019-03-27 2024-05-03 Sk新技术株式会社 锂前驱体的再生方法
CN114433861A (zh) * 2022-01-24 2022-05-06 安徽寒锐新材料有限公司 一种草酸钴制备钴粉的方法

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