Method for separating lithium precursors and system for separating lithium precursors
By mixing the primary lithium precursor with the precipitate solution in the reactor and injecting non-reactive gas, the problem of low recovery efficiency of the positive electrode active material of the lithium secondary battery is solved, and high efficiency and high purity separation of the lithium precursor is achieved.
Patent Information
- Application Number
- CN202411821239.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2019-05-20
- Filing Date
- 2020-03-30
- Publication Date
- 2025-03-14
- Estimated Expiration
- 2040-03-30
AI Technical Summary
The prior art when recovering the positive electrode active material of lithium secondary batteries, the efficiency is low and the yield is not high, and a large amount of impurities may be generated, affecting the high-purity separation of lithium precursors.
The lithium precursor is selectively separated by mixing the primary lithium precursor with the precipitate solution in the reactor and injecting a non-reactive gas to form a precursor mixture.
High efficiency and high purity separation of lithium precursors are achieved, impurities are avoided and recycling efficiency is improved.
Smart Images

Figure CN119627284A_ABST
Abstract
Description
[0001] This application is a divisional application of a Chinese patent application with an application date of March 30, 2020, Chinese patent application number 202080037222.4 and an invention name of “Method for separating lithium precursors and system for separating lithium precursors”, and this application claims priority to patent application No. 10-2019-0058661 filed with the Korean Intellectual Property Office (KIPO) on May 20, 2019, the entire contents of which are incorporated herein by reference. Technical Field
[0002] The present invention relates to a method and a system for separating a lithium precursor from a primary precursor mixture. Background Art
[0003] With the development of information technology and display technology, secondary batteries that can be repeatedly charged and discharged have been widely used as power sources for mobile electronic devices such as camcorders, mobile phones, and notebook computers. Secondary batteries include, for example, lithium secondary batteries, nickel-cadmium batteries, and nickel-hydrogen batteries. Lithium secondary batteries are actively developed and used due to their high operating voltage and energy density per unit weight, high charging rate, compact size, and the like.
[0004] The lithium secondary battery may include an electrode assembly including a positive electrode, a negative electrode and a separator layer (separator), and an electrolyte in which the electrode assembly is immersed. The lithium secondary battery may further include a case having, for example, a pouch shape for accommodating the electrode assembly and the electrolyte.
[0005] Lithium metal oxides can be used as positive electrode active materials for lithium secondary batteries. Lithium metal oxides may further contain transition metals such as nickel, cobalt, and manganese.
[0006] Lithium metal oxide as a positive electrode active material may be prepared by reacting a lithium precursor with a nickel-cobalt-manganese (NCM) precursor containing nickel, cobalt, and manganese.
[0007] Since the above-mentioned high-cost precious metal is used in the positive electrode active material, excessively high costs are required in the manufacture of the positive electrode active material. In addition, with the recent prominence of environmental protection issues, a method for recovering the positive electrode active material has been studied. For the recovery of the positive electrode active material, it is necessary to regenerate a lithium precursor from the used positive electrode with high efficiency and high yield.
[0008] For example, Korean Published Patent Application No. 2015-0002963 discloses a method for recovering lithium using a wet process. However, lithium is recovered by wet extraction from waste liquid remaining after extraction of cobalt, nickel, etc., so the recovery rate may be excessively reduced and a large amount of impurities may be generated from the waste liquid.
[0009] [Technical purpose]
[0010] According to one aspect of the present invention, there is provided a method for separating a lithium precursor with high efficiency and high purity.
[0011] According to one aspect of the present invention, a system for separating lithium precursors with high efficiency and high purity is provided.
[0012] [Method to achieve the goal]
[0013] In the method for separating a lithium precursor according to an exemplary embodiment, a primary precursor mixture including a primary lithium precursor and a primary transition metal precursor is prepared, the primary precursor mixture is mixed with a precipitation liquid in a reactor to form a precursor mixture, and a non-reactive gas is injected into the precursor mixture.
[0014] In some embodiments, the reactor may be a fluidized bed reactor.
[0015] In some embodiments, the primary precursor mixture may be prepared by reducing a positive active material collected from a lithium secondary battery.
[0016] In some embodiments, the reduction reaction may be performed prior to forming the precursor mixture in the reactor.
[0017] In some embodiments, the primary lithium precursor may include lithium hydroxide.
[0018] In some embodiments, the primary lithium precursor may further include lithium oxide or lithium carbonate.
[0019] In some embodiments, the precursor mixture can be formed by selectively dissolving lithium hydroxide in a precipitation solution.
[0020] In some embodiments, the precipitation liquid can include water.
[0021] In some embodiments, the precipitation solution may further include dimethyl carbonate or diethyl carbonate.
[0022] In some embodiments, the mass of the precipitating liquid in the precursor mixture may be 2 to 20 times the mass of the primary lithium precursor.
[0023] In some embodiments, the precursor mixture may include a slurry or solution containing a primary precursor mixture.
[0024] In some embodiments, injecting the non-reactive gas into the precursor mixture may include pulsing the non-reactive gas.
[0025] In some embodiments, the solubility of the non-reactive gas in the precipitation liquid may be 1.5 g / L or less.
[0026] In some embodiments, the non-reactive gas may include at least one selected from nitrogen, neon, argon, krypton, and xenon.
[0027] In some embodiments, a non-reactive gas may be injected into the lower portion of the reactor.
[0028] In some embodiments, injecting the non-reactive gas may include reducing a linear velocity of the non-reactive gas at an upper portion of the reactor.
[0029] In some embodiments, the linear velocity of the non-reactive gas may be reduced to 0.1 cm / sec to 3 cm / sec.
[0030] In some embodiments, the upper portion of the reactor may include an expanded portion having an expanded diameter or an expanded width.
[0031] In some embodiments, forming the precursor mixture and injecting the non-reactive gas may be repeated in multiple cycles.
[0032] A system for separating a lithium precursor according to an exemplary embodiment includes a reactor body into which a lithium precursor is introduced, a precipitation liquid injection unit for injecting a precipitation liquid into the reactor body, a gas injection unit for injecting a non-reactive gas into a lower portion of the reactor body, and an expansion portion extending from an upper portion of the reactor body and having an expanded diameter or an expanded width.
[0033] [Effects of the Invention]
[0034] According to the above exemplary embodiments, a primary precursor mixture including a primary lithium precursor and a primary transition metal precursor may be mixed with a precipitation liquid in a reactor to form a precursor mixture, and a non-reactive gas may be injected into the precursor mixture to separate the lithium precursor with high purity and efficiency.
[0035] The non-reactive gas can disperse the primary precursor mixture in the precipitation solution, thereby selectively dissolving the lithium precursor including lithium hydroxide in the precipitation solution. In addition, the primary transition metal precursor that is not dissolved in the precipitation solution may precipitate.
[0036] Therefore, only the lithium precursor can be selectively separated from the primary precursor mixture. BRIEF DESCRIPTION OF THE DRAWINGS
[0037] Figure 1 is a process flow chart showing a method of separating a lithium precursor according to an exemplary embodiment.
[0038] Figure 2 is a schematic diagram for describing a system for separating a lithium precursor according to an exemplary embodiment. DETAILED DESCRIPTION
[0039] According to an exemplary embodiment of the present invention, a method and a system for separating a lithium precursor are provided, wherein a primary precursor mixture is mixed with a precipitation liquid in a reactor to form a precursor mixture, and a non-reactive gas is injected into the precursor mixture to separate the lithium precursor with high efficiency and high purity.
[0040] Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. However, the embodiments are provided as illustrative examples, and the spirit of the present invention is not limited to specific embodiments.
[0041] The term "precursor" in this specification is used to generally refer to a compound containing a specific metal to provide the specific metal contained in the electrode active material.
[0042] Figure 1 is a process flow diagram illustrating a method of separating a lithium precursor according to an exemplary embodiment. Figure 2 is a schematic diagram for describing a system for separating a lithium precursor according to an exemplary embodiment.
[0043] In the following, reference is made to Figure 1 and Figure 2 Together, methods and systems for separating lithium precursors are described.
[0044] Reference Figure 1 , a primary precursor mixture including a primary lithium precursor and a primary transition metal precursor may be prepared (eg, in step S10 ).
[0045] In an exemplary embodiment, the primary precursor mixture including the primary lithium precursor and the primary transition metal precursor can be obtained from the positive active material mixture collected from the lithium secondary battery. For example, the positive active material mixture can be obtained from the lithium-containing compound obtained from the lithium secondary battery.
[0046] The lithium secondary battery may include an electrode assembly including a positive electrode, a negative electrode and a separator layer 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 a positive electrode collector and a negative electrode collector, respectively.
[0047] For example, the positive electrode active material included in the positive electrode active material layer may include an oxide containing lithium and a transition metal.
[0048] In some embodiments, the positive active material may include a compound represented by Chemical Formula 1 below.
[0049] [Chemical formula 1]
[0050] Li x M1 a M2b M3 c O y
[0051] In Chemical Formula 1, M1, M2, and M3 may each independently be selected from Ni, Co, Mn, Na, Mg, Ca, Ti, V, Cr, Cu, Zn, Ge, Sr, Ag, Ba, Zr, Nb, Mo, Al, Ga, or B. In Chemical Formula 1, 0 < x ≤ 1.1, 2 ≤ y ≤ 2.02, 0 < a < 1, 0 < b < 1, 0 < c < 1, and 0 < a + b + c ≤ 1.
[0052] In some embodiments, the positive electrode active material may be an NCM-based lithium oxide containing nickel, cobalt, and manganese. The NCM-based lithium oxide as the positive electrode active material may be prepared by reacting a lithium precursor and an NCM precursor (e.g., an NCM oxide) with each other through, for example, a coprecipitation reaction.
[0053] However, generally, the embodiments of the present invention can be applied not only to positive electrode materials including NCM-based lithium oxides but also to lithium-containing electrode materials.
[0054] The lithium precursor may include lithium hydroxide (LiOH), lithium oxide (Li2O), or lithium carbonate (Li2CO3). Lithium hydroxide may be advantageous as the lithium precursor in terms of charge / discharge performance, life performance, high-temperature stability, etc. of the lithium secondary battery. For example, lithium carbonate may cause an immersion reaction on the separator layer, thereby reducing life stability.
[0055] Therefore, according to an embodiment of the present invention, a method for highly selectively separating lithium hydroxide as the lithium precursor can be provided.
[0056] For example, the positive electrode can be separated and recovered from the lithium secondary battery. The positive electrode may include a positive electrode current collector (e.g., aluminum (Al)) and a positive electrode active material layer, and the positive electrode active material layer may include a conductive material, a binder, and the above positive electrode active material.
[0057] The conductive material may include, for example, a carbon-based material such as graphite, carbon black, graphene, carbon nanotubes, etc. The binder may include a resin material such as poly(vinylidene fluoride - hexafluoropropylene) copolymer (PVDF-co-HFP), polyvinylidene fluoride (PVDF), polyacrylonitrile, polymethyl methacrylate, etc.
[0058] The positive electrode active material mixture can be prepared from the recovered positive electrode. In some embodiments, the positive electrode active material mixture can be prepared in powder form by physical methods such as grinding. The positive electrode active material mixture can include a powder of a lithium transition metal oxide, and can include, for example, an NCM-based lithium oxide powder (e.g., Li(NCM)O2).
[0059] In some embodiments, the positive electrode active material mixture may be heat treated before the grinding process. In this case, the positive electrode current collector may be more easily separated from the positive electrode before the grinding process, and the binder and the conductive material may be removed. For example, the temperature of the heat treatment may be in the range of about 100°C to about 500°C, preferably in the range of about 350°C to about 450°C.
[0060] In some embodiments, the positive electrode active material mixture can be obtained after immersing the recovered positive electrode in an organic solvent. For example, the recovered positive electrode can be immersed in an organic solvent to separate and remove the positive electrode current collector, and the positive electrode active material can be selectively extracted by centrifugation.
[0061] By the above method, the positive electrode current collector components such as aluminum can be substantially completely separated and removed, and a positive electrode active material mixture from which the content of the carbon-based components derived from the conductive material and the binder may be removed or reduced can be obtained.
[0062] In some embodiments, the primary precursor mixture can be generated by reducing the positive electrode active material mixture (eg, the positive electrode active material). For example, the primary precursor mixture can be formed by reducing the positive electrode active material mixture with hydrogen.
[0063] The hydrogen reduction reaction may be performed at a temperature of about 350°C to about 700°C, preferably about 400°C to about 550°C.
[0064] The primary precursor mixture may include a primary lithium precursor and a primary transition metal precursor which may be a product of a hydrogen reduction reaction of a lithium-transition metal oxide included in the positive electrode active material mixture.
[0065] The primary lithium precursor may include lithium hydroxide, lithium oxide and / or lithium carbonate. In an exemplary embodiment, the primary lithium precursor may be obtained by a hydrogen reduction reaction, thereby reducing the mixed content of lithium carbonate.
[0066] The primary transition metal precursor may include Ni, Co, NiO, CoO, MnO, and the like.
[0067] For example, the primary precursor mixture formed by the above-described reduction reaction may be transferred to the reactor 100 as described below.
[0068] In some embodiments, the reduction reaction may be performed in the reactor 100, and the reaction of the precursor mixture for forming the primary precursor mixture 50 and the precipitation solution 80 may be performed in the reactor 100 as described below. In this case, the formation reaction of the precursor mixture may be performed without transferring the primary precursor mixture. Therefore, the reduction in yield caused when transferring the primary precursor mixture may be prevented.
[0069] Reference Figure 1 and Figure 2 , the primary precursor mixture 50 and the precipitation solution 80 may be mixed in the reactor 100 to form a precursor mixture (eg, in step S20 ).
[0070] For example, the precursor mixture may refer to a composition including a lithium precursor formed by reacting a primary lithium precursor 60 with a precipitation solution 80 and a primary transition metal precursor 70 precipitated in the precipitation solution 80 .
[0071] In some embodiments, the reactor 100 may be a fluidized bed reactor. For example, a fluidized bed reactor may refer to a reactor in which a fluid (gas or liquid) flows through the injected primary precursor mixture 50 to cause fluidization. For example, as will be described below, the fluid may be a non-reactive gas.
[0072] For example, the primary precursor mixture 50 may be fluidized in a fluidized bed reactor, thereby increasing the contact area with the precipitation solution 80. Therefore, the reaction between the primary lithium precursor 60 and the precipitation solution 80 may be further promoted.
[0073] In addition, the primary transition metal precursor 70 precipitated in the precipitation liquid 80 may be formed in a slurry state that can be easily transferred to a subsequent reactor.
[0074] Reference Figure 2 The precipitating liquid 80 may be injected into the reactor 100 through the precipitating liquid injection unit 120. The precipitating liquid 80 may be injected into the reactor body 110 through the precipitating liquid injection unit 120.
[0075] For example, the precipitation liquid injection unit 120 may be located at an upper portion of the reactor body 110. The precipitation liquid injection unit 120 may be located at a lower portion or a middle portion of the reactor body 110.
[0076] In some embodiments, the primary lithium precursor may include lithium hydroxide. In some embodiments, the primary lithium precursor may further include lithium oxide or lithium carbonate.
[0077] In some embodiments, the precursor mixture may be formed by dissolving the primary lithium precursor 60 in the precipitation solution 80 .
[0078] For example, lithium hydroxide contained in the primary lithium precursor 60 may be selectively dissolved in the precipitation solution 80 to form a precursor mixture. For example, lithium oxide may react with the precipitation solution 80 to form lithium hydroxide, which may then be dissolved in the precipitation solution 80. For example, lithium carbonate may have a low solubility in the precipitation solution 80. Therefore, the lithium carbonate may be precipitated and removed from the primary precursor mixture.
[0079] In some embodiments, the precipitation liquid 80 may include water. For example, the primary lithium precursor 60 may be hydrated with water to form a precursor mixture including an aqueous solution having dissolved lithium hydroxide.
[0080] In some exemplary embodiments, the precipitation liquid may further include dimethyl carbonate or diethyl carbonate.
[0081] For example, dimethyl carbonate or diethyl carbonate may promote the reaction between the primary lithium precursor 60 and water. Therefore, the separation efficiency of the lithium precursor may be improved.
[0082] In some embodiments, the mass of the precipitating solution 80 in the precursor mixture may be about 2 to 20 times the mass of the primary lithium precursor 60 , preferably about 2 to 10 times the mass of the primary lithium precursor 60 .
[0083] For example, within the above range, mixing of the primary lithium precursor 60 and the precipitation solution 80 can be easily performed by a non-reactive gas as described below. Therefore, the lithium precursor can be separated with high purity and high efficiency without using an excessive amount of precipitation solution.
[0084] In some embodiments, the precursor mixture may include a slurry or solution including the primary precursor mixture 50 .
[0085] For example, the primary transition metal precursor 70, which may not be dissolved in the precipitation liquid 80, may be dispersed in the precipitation liquid 80 to form a slurry. For example, lithium hydroxide contained in the primary lithium precursor 60 may be dissolved in the precipitation liquid 80 to form a solution. Therefore, the primary transition metal precursor 70 and the primary lithium precursor 60 may be separated from each other.
[0086] Reference Figure 1 and Figure 2 , a non-reactive gas may be injected into the precursor mixture (eg, in step S30 ). For example, the non-reactive gas may be injected into the precursor mixture inside the reactor 100 through the gas injection unit 130 .
[0087] For example, a non-reactive gas may be injected into the precursor mixture to facilitate mixing of the primary precursor mixture 50 and the precipitation liquid 80 .
[0088] For example, the non-reactive gas may apply physical impact to the agglomerated primary precursor mixture 50 , so that the primary precursor mixture 50 may be uniformly dispersed in the precipitation liquid 80 .
[0089] Therefore, the contact area between the precipitation liquid 80 and the primary precursor mixture 50 can be increased, so that the precursor mixture can be formed more easily.
[0090] In some embodiments, pulses of non-reactive gas may be injected into the precursor mixture. The pulses of non-reactive gas may include a constant periodic variation of the injection rate or amount of the non-reactive gas. For example, the type of pulse may be appropriately selected according to the capacity and shape of the reactor 100.
[0091] In some exemplary embodiments, the solubility of the non-reactive gas in the precipitation liquid 80 may be 1.5 g / L or less. Low solubility of the non-reactive gas in the precipitation liquid may be advantageous, and the lower limit of the solubility is not particularly limited.
[0092] In some exemplary embodiments, the non-reactive gas may include at least one selected from nitrogen, neon, argon, krypton, and xenon, which have lower solubility and reactivity relative to the precipitation liquid.
[0093] In this case, loss of the non-reactive gas caused when the non-reactive gas is dissolved in the precipitation liquid can be prevented. In addition, the non-reactive gas may not react with the precursor mixture, thereby preventing a reduction in the yield of the lithium precursor due to a side reaction.
[0094] In some embodiments, the non-reactive gas may not include carbon dioxide (CO 2 ). Therefore, a decrease in the yield of the lithium precursor due to the reaction between carbon dioxide and lithium hydroxide may be prevented.
[0095] In some embodiments, a non-reactive gas may be injected into the lower portion of the reactor 100. For example, the non-reactive gas may be injected into the precursor mixture through the gas injection unit 130 located at the lower portion of the reactor 100.
[0096] The non-reactive gas injected into the lower portion of the reactor 100 may rise to the upper portion of the reactor 100 to promote mixing of the primary precursor mixture 50 and the precipitation liquid 80 throughout the reactor body 110 .
[0097] In some embodiments, the linear velocity (cm / sec) of the non-reactive gas injected into the precursor mixture may be about 5 cm / sec to 30 cm / sec.
[0098] Within the above range, the non-reactive gas can provide sufficient physical impact to the aggregated primary precursor mixture 50 , thereby further promoting mixing of the primary precursor mixture 50 and the precipitation liquid 80 .
[0099] In some embodiments, the non-reactive gas at the upper portion of the reactor 100 may have a reduced linear velocity (cm / sec). For example, the linear velocity may refer to the flow rate of a gas passing through per unit area.
[0100] For example, the mass of each particle of the primary precursor mixture 50 contained in the reactor 100 may be different from each other. In this case, particles of the primary precursor mixture 50 having a relatively small mass may flow out of the reactor body 110 through the non-reactive gas or may be precipitated at the upper portion of the reactor 100.
[0101] Therefore, the linear velocity (cm / sec) of the non-reactive gas at the upper portion of the reactor 100 may be reduced, so that the primary precursor mixture 50 may be effectively prevented from flowing out of the reactor body 110 or being precipitated at the upper portion of the reactor 100 .
[0102] In some embodiments, the linear velocity of the non-reactive gas at the upper portion of the reactor 100 may be reduced to about 0.1 cm / sec to 3 cm / sec. For example, the linear velocity of the non-reactive gas in the expansion portion 140 located at the upper portion of the reactor body 110 may be reduced to about 0.1 cm / sec to 3 cm / sec.
[0103] Within the above range, the primary precursor mixture 50 can be prevented from flowing out of the reactor body 110 , while mixing of the primary precursor mixture 50 and the precipitation liquid 80 is further promoted.
[0104] For example, the reactor 100 may include an expansion portion 140 extending from an upper portion of the reactor body 110 and having a diameter greater than that of the reactor body 110 .
[0105] For example, the expansion part 140 may have a larger cross-sectional area than the reactor body 110, so that the linear velocity (cm / sec) of the non-reactive gas moving from the reactor body 110 to the expansion part 140 may be reduced. In this case, the ratio of the diameter of the expansion part 140 to the diameter of the reactor body 110 may be adjusted, and thus the reduction ratio of the linear velocity (cm / sec) may be easily adjusted.
[0106] In some embodiments, the ratio of the diameter of the expansion portion 140 to the diameter of the reactor body 110 may be 2 to 10.
[0107] Within the above diameter ratio range, the primary precursor mixture 50 may be more effectively prevented from flowing out of the reactor body 110 .
[0108] In some exemplary embodiments, the forming of the precursor mixture and the injecting of the non-reactive gas may be repeated in multiple cycles.
[0109] For example, the separation efficiency and yield of the lithium precursor can be improved by repeatedly forming a precursor mixture and injecting a non-reactive gas.
[0110] For example, the formation of the precursor mixture and the injection of the non-reactive gas may be repeated, thereby reducing the content of the undissolved lithium precursor in the precipitation liquid 80. Therefore, the yield of the lithium precursor may be further improved.
[0111] For example, while repeatedly forming the precursor mixture and injecting the non-reactive gas, the injection amount of the precipitation solution 80 and the non-reactive gas may be appropriately adjusted based on the solubility of the primary lithium precursor in the precipitation solution 80 and the capacity of the reactor 100 .
[0112] For example, the injection amount of the precipitation liquid 80 and the non-reactive gas may be constant, or may be continuously increased or decreased as multiple cycles are repeated.
[0113] In one embodiment, the precipitated primary transition metal precursor 70 can be collected from the reactor 100 to form a transition metal precursor. For example, the primary transition metal precursor 70 can be reacted with an acid solution to form a transition metal precursor.
[0114] In one embodiment, sulfuric acid can be used as the acid solution. In this case, the transition metal precursor can include a transition metal sulfate. For example, the transition metal sulfate can include NiSO4, MnSO4, CoSO4, etc.
Claims
1. A method for separating a lithium precursor, comprising: preparing a primary precursor mixture comprising a primary lithium precursor and a primary transition metal precursor, wherein preparing the primary precursor mixture comprises subjecting a positive electrode active material collected from a lithium secondary battery to a reduction reaction; Mixing the primary precursor mixture with a precipitating liquid in a reactor to form a precursor mixture, such that the mass of the precipitating liquid in the precursor mixture is 2 to 20 times the mass of the primary lithium precursor; After the primary precursor mixture is mixed with the precipitation liquid, a non-reactive gas is injected from the lower part of the reactor into the precursor mixture in a slurry or solution state containing the primary precursor mixture, such that the linear velocity of the non-reactive gas injected into the precursor mixture is 5 cm / sec to 30 cm / sec; and reducing the linear velocity of the non-reactive gas at the upper portion of the reactor so that the linear velocity of the non-reactive gas becomes 0.1 cm / s to 3 cm / s, The upper portion of the reactor includes an expanded portion having an expanded diameter or an expanded width.
2. The process according to claim 1, wherein the reactor is a fluidized bed reactor.
3. The method of claim 1, wherein the reduction reaction is performed before forming the precursor mixture in the reactor.
4. The method of claim 1, wherein the primary lithium precursor comprises lithium hydroxide. The method according to claim 4 , wherein the primary lithium precursor further comprises lithium oxide or lithium carbonate.
6. The method of claim 5, wherein forming the precursor mixture comprises selectively dissolving lithium hydroxide in the precipitation solution. The method of claim 1 , wherein the precipitation liquid comprises water.
8. The method according to claim 7, wherein the precipitation solution further comprises dimethyl carbonate or diethyl carbonate.
9. The method of claim 1, wherein injecting the non-reactive gas comprises pulse injecting the non-reactive gas. 10 . The method according to claim 1 , wherein the solubility of the non-reactive gas in the precipitation liquid is 1.5 g / L or less.
11. The method according to claim 1, wherein the non-reactive gas comprises at least one selected from the group consisting of nitrogen, neon, argon, krypton, and xenon.
12. The method of claim 1, wherein forming the precursor mixture and injecting the non-reactive gas are repeated in a plurality of cycles.
13. A system for separating a lithium precursor for use in the method according to any one of claims 1 to 12, comprising: a reactor body into which a lithium precursor is introduced; A precipitation liquid injection unit, used for injecting the precipitation liquid into the reactor body; a gas injection unit for injecting a non-reactive gas into the lower portion of the reactor body; as well as An expansion portion extends from an upper portion of the reactor body and has an expanded diameter or an expanded width.
Citation Information
Patent Citations
Method of regenerating lithium precursor from used lithium secondary battery
KR101897134B1
Direct Reduced Copper Apparatus and Method therefor
KR1020170118405A