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WO2020071640A1 - Procédé et système pour régénérer un précurseur de lithium - Google Patents

Procédé et système pour régénérer un précurseur de lithium

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Publication number
WO2020071640A1
WO2020071640A1 PCT/KR2019/010914 KR2019010914W WO2020071640A1 WO 2020071640 A1 WO2020071640 A1 WO 2020071640A1 KR 2019010914 W KR2019010914 W KR 2019010914W WO 2020071640 A1 WO2020071640 A1 WO 2020071640A1
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WO
WIPO (PCT)
Prior art keywords
lithium precursor
lithium
positive electrode
active material
electrode active
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2019/010914
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English (en)
Korean (ko)
Inventor
나지예
구민수
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SK Innovation Co Ltd
Original Assignee
SK Innovation Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SK Innovation Co Ltd filed Critical SK Innovation Co Ltd
Publication of WO2020071640A1 publication Critical patent/WO2020071640A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/02—Oxides; Hydroxides
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00033—Continuous processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00479—Means for mixing reactants or products in the reaction vessels
    • B01J2219/00481—Means for mixing reactants or products in the reaction vessels by the use of moving stirrers within the reaction vessels
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the present invention relates to a lithium precursor regeneration method and a lithium precursor regeneration system. More particularly, it relates to a method and system for regenerating a lithium precursor from a waste lithium secondary battery.
  • the secondary battery is a battery that can be repeatedly charged and discharged, and has been widely applied to portable electronic communication devices such as camcorders, mobile phones, notebook PCs, etc. with the development of the information communication and display industries.
  • Examples of the secondary battery include lithium secondary batteries, nickel-cadmium batteries, and nickel-hydrogen batteries, among which lithium secondary batteries have high operating voltage and energy density per unit weight, and are advantageous for charging speed and weight reduction. In this regard, it has been actively developed and applied.
  • the lithium secondary battery may include an electrode assembly including a positive electrode, a negative electrode, and a separator (separator), and an electrolyte impregnating the electrode assembly.
  • the lithium secondary battery may further include, for example, a pouch-shaped exterior material that accommodates the electrode assembly and the electrolyte.
  • Lithium metal oxide may be used as the positive electrode active material of the lithium secondary battery.
  • the lithium metal oxide may additionally contain transition metals such as nickel, cobalt, and manganese.
  • Lithium metal oxide as the positive electrode active material may be prepared by reacting a lithium precursor and a nickel-cobalt-manganese (NCM) precursor containing nickel, cobalt, and manganese.
  • NCM nickel-cobalt-manganese
  • the expensive metals described above are used for the positive electrode active material, 20% or more of the manufacturing cost is required to manufacture the positive electrode material.
  • the recycling method of the positive electrode active material has been conducted. In order to recycle the positive electrode active material, it is necessary to recycle the lithium precursor from the waste positive electrode with high efficiency and high purity.
  • Korean Patent Publication No. 2015-0002963 discloses a method for recovering lithium using a wet method.
  • the recovery rate is excessively reduced, and many impurities may be generated from the waste liquid.
  • One object of the present invention is to provide a method for regenerating a lithium precursor with high efficiency and high yield.
  • One object of the present invention is to provide a system for regenerating a lithium precursor with high efficiency and high yield.
  • the positive electrode active material mixture collected from the waste lithium secondary battery is supplied to a continuous flow reactor. Fluid is introduced into the continuous flow reactor to produce a counter flow. A lithium precursor aqueous solution is produced by contacting the counter flow and the positive electrode active material mixture. The lithium precursor is collected from the aqueous lithium precursor solution.
  • the fluid may be supplied to the bottom of the continuous flow reactor rather than the positive electrode active material mixture to generate a counter flow.
  • a plurality of impellers continuously arranged in the longitudinal direction of the continuous flow reactor may be rotated.
  • the flow of the counter flow may be maintained through a porous plate disposed between the impellers in the continuous flow reactor.
  • a plurality of the continuous flow reactors are continuously arranged and a counter flow can be generated within each continuous flow reactor.
  • the positive electrode active material mixture may sequentially pass through a plurality of the continuous flow reactors.
  • the aqueous lithium precursor solution in collecting the lithium precursor, may be stabilized at the top of the continuous flow reactor.
  • the lithium precursor aqueous solution may be crystallized to regenerate the lithium precursor.
  • the positive electrode active material mixture may include a preliminary lithium precursor and a transition metal-containing mixture.
  • a transition metal precursor can be collected from the transition metal containing mixture.
  • the transition metal containing mixture in collecting the transition metal precursor, may be collected from the bottom of the continuous flow reactor.
  • the transition metal-containing mixture can be treated with an acid solution.
  • the transition metal-containing mixture may be flushed in collecting the transition metal-containing mixture.
  • the preliminary lithium precursor may include lithium hydroxide, lithium oxide and lithium carbonate.
  • the lithium precursor may include lithium hydroxide.
  • the positive electrode active material mixture may be produced by reducing a waste positive electrode active material.
  • the lithium precursor regeneration system includes a positive electrode active material mixture introduction part, a continuous flow reactor for hydrating a positive electrode active material mixture supplied from the positive electrode active material mixture contact with a counter flow, and the positive electrode active material reacted with the counter flow. And a lithium precursor collection section for generating a lithium precursor from the mixture.
  • the continuous flow reactor may include a plurality of impellers arranged in the longitudinal direction of the continuous flow reactor, and at least one porous plate disposed between the impellers.
  • the impellers may include a first impeller and a second impeller disposed non-parallel to each other.
  • a plurality of continuous flow reactors can be arranged continuously.
  • a lithium precursor in the form of lithium hydroxide may be regenerated through a contact reaction between a positive electrode active material mixture and a counter flow of a fluid. Therefore, it is possible to increase the contact time between the positive electrode active material mixture and the fluid to improve the lithium precursor regeneration yield, and to reduce the amount of fluid used.
  • FIG. 1 is a process flow diagram illustrating a lithium precursor regeneration method according to example embodiments.
  • FIG. 2 is a schematic schematic diagram for describing a lithium precursor regeneration system according to example embodiments.
  • FIG 3 is a perspective view for explaining the structure of the impeller and the porous plate according to the exemplary embodiments.
  • FIG. 4 is a schematic diagram illustrating an impeller according to some example embodiments.
  • 5 to 7 are simulation graphs for explaining the lithium precursor regeneration yield using a continuous flow reactor and a batch reactor.
  • Embodiments of the present invention provide a method and system for regenerating a lithium precursor with high purity and high yield from a waste lithium secondary battery, for example, through a continuous flow reactor.
  • the term "precursor” is used to generically refer to a compound containing the specific metal to provide a specific metal included in the electrode active material.
  • 1 is a process flow diagram illustrating a lithium precursor regeneration method according to example embodiments.
  • 2 is a schematic schematic diagram for describing a lithium precursor regeneration system according to example embodiments.
  • FIGS. 1 and 2 a method and system for regenerating a lithium precursor will be described together.
  • a positive electrode active material mixture may be prepared (for example, step S10).
  • the positive electrode active material mixture may be obtained from a waste lithium-containing compound obtained from a waste lithium secondary battery.
  • the waste lithium secondary battery may include an electrode assembly including a positive electrode, a negative electrode, and a separator interposed between the positive electrode and the negative electrode.
  • the positive electrode and the negative electrode may include a positive electrode active material layer and a negative electrode active material layer coated on the positive electrode current collector and the negative electrode current collector, respectively.
  • the positive electrode active material included in the positive electrode active material layer may include an oxide containing lithium and a transition metal.
  • the positive electrode active material may include a compound represented by Formula 1 below.
  • M1, M2 and M3 are transition metals selected from Ni, Co, Mn, Na, Mg, Ca, Ti, V, Cr, Cu, Zn, Ge, Sr, Ag, Ba, Zr, Nb, Mo, Al, Ga or B Can be In Formula 1, 0 ⁇ x ⁇ 1.1, 2 ⁇ y ⁇ 2.02, 0 ⁇ a ⁇ 1, 0 ⁇ b ⁇ 1, 0 ⁇ c ⁇ 1, 0 ⁇ a + b + c ⁇ 1.
  • the positive electrode active material may be NCM-based lithium oxide including nickel, cobalt, and manganese.
  • NCM-based lithium oxide as the positive electrode active material may be prepared by reacting a lithium precursor and an NCM precursor (eg, NCM oxide) with each other through, for example, a co-precipitation reaction.
  • the embodiments of the present invention can be commonly applied to a positive electrode material containing the NCM-based lithium oxide, as well as a lithium-containing positive electrode material.
  • the lithium precursor may include lithium hydroxide (LiOH), lithium oxide (Li 2 O), or lithium carbonate (Li 2 CO 3 ).
  • Lithium hydroxide may be advantageous as a lithium precursor in terms of charging / discharging characteristics, life characteristics, and high temperature stability of the lithium secondary battery.
  • a deposition reaction may be caused on the separator to weaken life stability.
  • a method of regenerating lithium hydroxide as a lithium precursor at a high selectivity may be provided.
  • the positive electrode can be recovered by separating the positive electrode from the waste lithium secondary battery.
  • the positive electrode includes a positive electrode current collector (for example, aluminum (Al)) and a positive electrode active material layer as described above, and the positive electrode active material layer may include a conductive material and a binder together with the positive electrode active material described above. .
  • the conductive material may include, for example, carbon-based materials such as graphite, carbon black, graphene, and carbon nanotubes.
  • the binder is, for example, vinylidene fluoride-hexafluoropropylene copolymer (PVDF-co-HFP), polyvinylidene fluoride (PVDF), polyacrylonitrile (polyacrylonitrile), polymethyl methacrylate and resin materials such as (polymethylmethacrylate).
  • a preliminary positive electrode active material mixture may be prepared from the recovered positive electrode.
  • the preliminary positive electrode active material mixture may be prepared in powder form through a physical method such as grinding treatment.
  • the preliminary positive electrode active material mixture includes a powder of a lithium-transition metal oxide, for example, NCM-based lithium oxide powder (eg, Li (NCM) O 2 ).
  • the anode recovered before the crushing treatment may be heat treated. Accordingly, desorption of the positive electrode current collector during the pulverization treatment may be promoted, and the binder and the conductive material may be at least partially removed.
  • the heat treatment temperature may be performed at, for example, about 100 to 500 ° C, preferably about 350 to 450 ° C.
  • the preliminary positive electrode active material mixture may be obtained after immersing the recovered positive electrode in an organic solvent.
  • the positive electrode current collector may be separated and removed by immersing the recovered positive electrode in an organic solvent, and the positive electrode active material may be selectively extracted through centrifugation.
  • the positive electrode current collector component such as aluminum is substantially completely separated and removed, and the preliminary positive electrode active material mixture having the content of carbon-based components derived from the conductive material and the binder removed or reduced can be obtained.
  • the preliminary positive electrode active material mixture (eg, waste positive electrode active material) may be reduced to generate the positive electrode active material mixture.
  • the preliminary positive electrode active material mixture may be hydrogen-reduced to form a positive electrode active material mixture.
  • the positive electrode active material mixture may include a hydrogen reduction reaction of a lithium-transition metal oxide contained in the preliminary positive electrode active material mixture.
  • the preliminary precursor mixture may include a preliminary lithium precursor and a transition metal-containing mixture.
  • the preliminary lithium precursor may include lithium hydroxide, lithium oxide and / or lithium carbonate. According to exemplary embodiments, since the preliminary lithium precursor is obtained through a hydrogen reduction reaction, the mixed content of lithium carbonate may be reduced.
  • the transition metal-containing reactant may include Ni, Co, NiO, CoO, MnO, and the like.
  • the positive electrode active material mixture may be introduced into a continuous flow reactor (eg, CSTR) 100 (eg, step S20).
  • CSTR continuous flow reactor
  • the continuous flow reactor 100 may be connected to a first flow path 102a provided as a supply portion of the positive electrode active material mixture.
  • the continuous flow reactor 100 may be connected to a second flow path 102b provided as a counter flow forming fluid supply unit, which will be described later.
  • pure water may be supplied through the second flow path 102b to generate a counter flow in the reactor body 130.
  • the first flow path 102a may be disposed above the continuous flow reactor 100 than the second flow path 102b.
  • the positive electrode active material mixture may be supplied through the first flow path 102a disposed on the second flow path 102b.
  • a positive electrode active material mixture having a higher density is supplied to the first flow path 102a disposed above the continuous flow reactor 100 than the second flow path 102b, and disposed at the lower portion of the continuous flow reactor 100.
  • a fluid having a low density is supplied to the second flow path 102b, and a counter flow (countercurrent, flow) may be formed by a difference in density between the positive electrode active material mixture and the fluid.
  • the positive electrode active material mixture is in contact with the counter flow rising from the bottom to the top of the reactor body 130, a hydration reaction may be induced. Accordingly, an aqueous lithium precursor solution may be generated (eg, step S30).
  • the continuous flow reactor 100 may include a reactor body 130 and a plurality of impellers 110 included inside the reactor body 130.
  • the impellers 110 for example, share one rotating shaft 115 and may be continuously disposed along the longitudinal direction of the reactor body 130.
  • At least one porous plate 120 may be disposed between the impellers 110.
  • the counter flow may continuously rise through a fluid continuously supplied through the second flow path 102b. Therefore, the time during which the positive electrode active material mixture stays in the reactor body 130 and the hydration reaction can be increased can improve the regeneration yield.
  • a plurality of impellers continuously arranged in the longitudinal direction of the continuous flow reactor 100 may be rotated. Therefore, the contact efficiency between the positive electrode active material mixture and the counter flow increases due to the rotation of the impellers, thereby improving the production efficiency of the lithium precursor aqueous solution.
  • the porous plate 120 is disposed between the impellers 110, the counter flow is prevented from flowing backward or turbulence, and the rise of the counter flow can be maintained. Therefore, since the contact time between the positive electrode active material mixture and the counter flow is increased, the regeneration yield of the lithium precursor through the hydration reaction may be further improved. In addition, it is possible to reduce the amount of fluid for maintaining the counter flow rise.
  • the positive electrode active material mixture may include a preliminary lithium precursor and a transition metal-containing mixture 70.
  • the preliminary lithium precursor may be converted into a lithium precursor 60 containing lithium hydroxide by hydration reaction through contact with the counter flow.
  • lithium oxide and lithium carbonate contained in the preliminary lithium precursor may be converted into lithium hydroxide.
  • the lithium precursor 60 may be substantially composed of lithium hydroxide through continuous reaction with the counter flow.
  • the lithium precursor 60 may be substantially dissolved in the counter flow containing water to rise together with the counter flow in the form of an aqueous solution.
  • the transition metal-containing mixture 70 remains in a solid state and may move to the bottom of the reactor 100 by gravity. For example, the transition metal-containing mixture 70 may settle to the bottom of the reactor 100 through pores included in the porous plate 120.
  • a distribution gradient of the lithium precursor 60 and the transition metal-containing mixture 70 may be formed inside the reactor body 130.
  • the distribution density of the lithium precursor 60 may be increased toward the upper portion of the reactor body 130.
  • a plurality of continuous flow reactors 100 may be continuously arranged.
  • a counter flow is generated in each continuous flow reactor 100, and the positive electrode active material mixture sequentially passes through a plurality of continuous flow reactors and is in continuous contact with the counter flow to induce a hydration reaction. Therefore, the conversion rate of the preliminary lithium precursor to lithium hydroxide can reach substantially 100%.
  • the transition metal-containing mixture is collected from each continuous flow reactor 100, the resolution and yield of the transition metal-containing mixture can also be improved.
  • the reactor body 130 includes a temperature-adjustable heater, and for the hydration reaction efficiency, the temperature inside the reactor body 130 may be maintained within a range of about 30 to 95 ° C.
  • a lithium precursor and a transition metal precursor may be collected from the reactor body 130 (eg, step S40).
  • the lithium precursor 60 may be recovered from the lithium precursor collection unit 150 connected to the upper portion of the reactor body 130.
  • the lithium precursor collection unit 150 may be provided as a stabilization unit of a lithium precursor aqueous solution.
  • the lithium precursor aqueous solution stays or circulates in the lithium precursor collection unit 150, and the transition metal-containing mixture 70 mixed in the lithium precursor aqueous solution is separated and removed under the reactor body 130. You can.
  • the lithium precursor collection unit 150 may have a larger diameter or cross-sectional area than the reactor body 100. Therefore, since the flow rate in the lithium precursor collection unit 150 of the lithium precursor aqueous solution decreases, the high-density transition metal-containing mixture precipitates, so that the high-purity lithium precursor can be easily collected.
  • the lithium precursor 60 collected in the lithium precursor collection unit 150 may be recovered through the first recovery channel 160a. Thereafter, the lithium precursor in the form of lithium hydroxide may be regenerated through a crystallization process or the like.
  • the transition metal-containing mixture 70 may be collected through the transition metal precursor collection unit 140.
  • the transition metal-containing mixture 70 may not be dissolved in the counter flow and may be precipitated in the transition metal precursor collection unit 140 through the porous plate 120 in a solid form.
  • the transition metal precursor collection unit 140 may be provided as a flushing or flushing section.
  • lithium or a lithium precursor remaining on the surface of the transition metal-containing mixture 70 may be washed with water by supplying water from the bottom of the reactor body 130. Accordingly, the substantially pure transition metal-containing mixture 70 may be collected in the transition metal precursor collection unit 140.
  • the transition metal-containing mixture 70 may be recovered through the second recovery channel 160b.
  • the recovered transition metal-containing mixture 70 may be acid treated through a filtration or separation process. Accordingly, transition metal precursors in the acid salt form of each transition metal can be formed.
  • sulfuric acid may be used as the acid treatment solution.
  • NiSO 4 , MnSO 4 and CoSO 4 may be recovered as the transition metal precursor, respectively.
  • the purity and recovery rate of the lithium precursor may be increased through a distribution gradient utilizing the column type continuous flow reactor 100.
  • the lithium precursor in the form of lithium hydroxide can be obtained in high yield with a small amount of water through a continuous hydration reaction using a counter flow.
  • FIG 3 is a perspective view for explaining the structure of the impeller and the porous plate according to the exemplary embodiments.
  • a plurality of impellers 110 may be arranged along the rotation axis 115 extending in the longitudinal direction of the reactor body 130.
  • a porous plate 120 may be disposed between the impellers 110.
  • Each impeller 110 may include a plurality of blades.
  • the four blades may be arranged around the rotation axis 115 such that they intersect at right angles to each other.
  • the blade arrangement shown in FIG. 3 is exemplary, and may be appropriately modified according to the shape of the reactor body 130.
  • FIG. 4 is a schematic diagram illustrating an impeller according to some example embodiments.
  • impellers may be arranged non-parallel to each other.
  • the impeller may include a first impeller 110a and a second impeller 110b.
  • the plurality of first impellers 110a and the second impellers 110b may be alternately arranged alternately along the rotation axis 115.
  • the blades of the first impeller 110a and the second impeller 110b may be disposed non-parallel to each other.
  • the first impeller 110a may be disposed substantially perpendicular to the rotating shaft 115
  • the second impeller 110b may be disposed obliquely to the rotating shaft 115.
  • 5 to 7 are simulation graphs for explaining lithium precursor regeneration yield using a continuous flow reactor (CSTR) and a batch reactor.
  • the x-axis represents the reactor residence time (hr) of the positive electrode active material mixture
  • the y-axis represents the yield (LiOH Yield) of the lithium precursor.
  • the dissolution rate constant refers to the rate at which LiOH dissolves in water, and is proportional to the dissolution concentration and the contact area with water.
  • FIG. 6 is a graph showing a change in the yield of lithium precursors according to the number of CSTRs or the number of counter flows, assuming that the dissolution rate constant of the CSTR is 2 times that of a batch reactor.

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

Un procédé pour régénérer un précurseur de lithium selon des modes de réalisation de la présente invention consiste à : fournir, à un réacteur à écoulement continu, un mélange de matériau actif de cathode collecté à partir d'une batterie secondaire au lithium usagée; l'introduction d'un fluide dans le réacteur à écoulement continu pour produire un contre-courant; la mise en contact du contre-courant avec le mélange de matériau actif de cathode pour produire une solution aqueuse de précurseur de lithium; et la collecte d'un précurseur de lithium à partir de la solution aqueuse de précurseur de lithium. La présente invention peut améliorer le rendement et l'efficacité de régénération de précurseur de lithium par l'intermédiaire d'une réaction de contact continue avec le contre-courant.
PCT/KR2019/010914 2018-10-04 2019-08-27 Procédé et système pour régénérer un précurseur de lithium Ceased WO2020071640A1 (fr)

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KR1020180118083A KR101998691B1 (ko) 2018-10-04 2018-10-04 리튬 전구체 재생 방법 및 리튬 전구체 재생 시스템
KR10-2018-0118083 2018-10-04

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