Method for manufacturing battery materials

Abstract

To provide a method for manufacturing a battery material which recovers valuable metal more efficiently.SOLUTION: The method for manufacturing a battery material disclosed herein includes: a preparation step of preparing a recovery target including at least one of Ni and Co; an acid exudation step of immersing the recovery target into an acid solution and obtaining an acid exudation solution; a neutralization-precipitation step of mixing the acid exudation solution and the neutralizer with each other and obtaining a precipitation; a solid-liquid separation step of separating the precipitation into a solid material and liquid; and an ammonia exudation step of immersing the separated precipitation in the ammonia solution including ammonium ions and obtaining an ammonia exudation solution including at least one of Ni and Co.SELECTED DRAWING: Figure 3

Description

Technical Field

[0001] The technology disclosed herein relates to a method for manufacturing battery materials.

Background Art

[0002] Lithium-ion secondary batteries are widely used in various fields. Various materials containing valuable metals such as Ni and Co are used in these lithium-ion secondary batteries. For example, lithium transition metal composite oxides such as lithium nickel composite oxide, lithium cobalt composite oxide, lithium nickel cobalt composite oxide, and lithium nickel cobalt manganese composite oxide are used as the positive electrode active material. Also, aluminum or the like is used for the positive electrode core.

[0003] In recent years, the development of recovery technologies for recovering valuable metals from used batteries and process scrap materials and reusing them as battery materials has been underway. For example, Patent Document 1 discloses an example of a recovery technology for a positive electrode plate. In the recovery method described in Patent Document 1, the object to be recovered (lithium-ion battery scrap) is leached with an acid, and at least a part of the aluminum ions is removed from the post-leaching solution obtained by the above leaching by neutralizing the post-leaching solution to obtain a post-neutralization solution, and the remaining aluminum ions are extracted from the post-neutralization solution by performing solvent extraction on the neutralization solution. Thereby, it is disclosed that cobalt (Co) and / or nickel (Ni) can be recovered from the extraction residue solution from which aluminum has been removed.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] As disclosed in the above-mentioned Patent Document 1, in the conventional technology for recovering a positive electrode plate, at least a part of aluminum ions (aluminum) is precipitated and removed as a precipitate by neutralizing an acid leachate containing the object to be recovered. By the way, some of such precipitates may contain valuable metals (Ni and / or Co). Therefore, in the conventional technology for recovering a positive electrode plate, there is a risk that such valuable metals are removed from the object to be recovered, and the valuable metals cannot be sufficiently recovered.

[0006] The present disclosure has been made in view of such circumstances, and an object thereof is to provide a method for manufacturing a battery material with an improved recovery rate of valuable metals.

Means for Solving the Problems

[0007] For the above problems, a method for manufacturing a battery material having the following configuration (hereinafter, also simply referred to as "manufacturing method") is provided.

[0008] The method for manufacturing a battery material disclosed herein includes a preparation step of preparing an object to be recovered containing at least one of Ni and Co, an acid leaching step of immersing the object to be recovered in an acid solution to obtain an acid leachate, a neutralization precipitation step of mixing the acid leachate and a neutralizing agent to obtain a precipitate, a solid-liquid separation step of performing solid-liquid separation on the precipitate, and an ammonia leaching step of immersing the separated precipitate in an ammonia solution containing ammonium ions to obtain an ammonia leachate containing at least one of the Ni and the Co.

[0009] In the manufacturing method having the above configuration, by performing ammonia leaching on the precipitate obtained in the neutralization precipitation step, Ni and / or Co in the precipitate can be separated and dissolved in the ammonia solution. Thereby, the recovery rate of valuable metals from the object to be recovered can be improved.

Brief Description of the Drawings

[0010]

Figure 1

Figure 2

Figure 3

Figure 4

DETAILED DESCRIPTION OF THE INVENTION

[0011] Hereinafter, embodiments of the technology disclosed herein will be described with reference to the drawings. In addition, matters other than those specifically mentioned in this specification and necessary for the implementation of the technology disclosed herein can be grasped as design matters of those skilled in the art based on the prior art in the relevant field. The technology disclosed herein can be implemented based on the content disclosed in this specification and the common general knowledge in the relevant field. In addition, the notation "A to B" indicating a range in this specification includes the meaning of "not less than A and not more than B", and also includes the meaning of "preferably greater than A" and "preferably less than B".

[0012] 1. Object to be recovered The method for manufacturing a battery material according to this embodiment manufactures a battery material (typically, a material for a positive electrode active material of a lithium-ion secondary battery, a precursor of a positive electrode active material, a positive electrode active material) by recovering valuable metals such as Ni and Co from a predetermined object to be recovered. An example of the object to be recovered here is a used lithium-ion secondary battery. Hereinafter, this lithium-ion secondary battery will be specifically described. FIG. 1 is a longitudinal sectional view schematically showing the internal structure of a lithium-ion secondary battery. FIG. 2 is a perspective view schematically showing the electrode body of the lithium-ion secondary battery shown in FIG. 1.

[0013] As shown in FIG. 1, the lithium-ion secondary battery 1 includes a case 10, an electrode body 20, and an electrolyte (not shown).

[0014] (1) Case The case 10 is a box-shaped container. Inside this case 10, an electrode body 20 and an electrolyte are accommodated. For the case 10, a metal material (such as aluminum (Al)) having a certain strength is used, for example. Also, a positive electrode terminal 12 and a negative electrode terminal 14 are attached to the case 10. The positive electrode terminal 12 and the negative electrode terminal 14 are connected to the electrode body 20 inside the case 10. Specifically, the positive electrode terminal 12 is connected to the positive electrode plate 30 (see FIG. 2) of the electrode body 20. Aluminum (Al) or the like is used for this positive electrode terminal 12. On the other hand, the negative electrode terminal 14 is connected to the negative electrode plate 40 of the electrode body 20. Copper (Cu) or the like is used for this negative electrode terminal 14.

[0015] (2) Electrode body The electrode body 20 is a power generation element of the lithium-ion secondary battery 1. As shown in FIG. 2, the electrode body 20 includes a positive electrode plate 30, a negative electrode plate 40, and a separator 50. Note that the electrode body 20 shown in FIG. 2 is a wound electrode body. This wound electrode body is produced by laminating the positive electrode plate 30, the negative electrode plate 40, and the separator 50 to form a long strip-shaped laminate and winding the laminate. However, the structure of the electrode body 20 is not particularly limited, and other conventionally known structures (such as a laminated electrode body) may be used.

[0016] The positive electrode plate 30 includes a positive electrode core 32 which is a conductive metal foil, and a positive electrode active material layer 34 provided on the surface of the positive electrode core 32. Aluminum (Al) or the like is used for the positive electrode core 32. Further, the positive electrode active material layer 34 is a composite material layer containing a positive electrode active material, a conductive material, a binder, and the like. The positive electrode active material is a lithium transition metal composite oxide containing at least one of nickel (Ni) and cobalt (Co). As an example of such a lithium transition metal composite oxide, a lithium nickel composite oxide, a lithium cobalt composite oxide, a lithium nickel manganese composite oxide, a lithium manganese cobalt composite oxide, a lithium nickel cobalt composite oxide, a lithium nickel manganese cobalt composite oxide, and the like can be mentioned. According to the manufacturing method according to the present embodiment, Ni and / or Co can be efficiently recovered from a recovery target containing such a lithium transition metal composite oxide. Further, examples of the conductive material include carbon materials such as acetylene black and graphite. Further, examples of the binder include resin materials such as polyvinylidene fluoride (PVdF).

[0017] On the other hand, the negative electrode plate 40 includes a negative electrode core 42 which is a conductive metal foil, and a negative electrode active material layer 44 provided on the surface of the negative electrode core 42. Copper (Cu) or the like is used for the negative electrode core 42. Further, the negative electrode active material layer 44 is a composite material layer containing a negative electrode active material, a binder, a thickener, and the like. Examples of the negative electrode active material include carbon materials such as graphite, hard carbon, and soft carbon. Further, other examples of the negative electrode active material include lithium titanate (LTO), silicon carbide, a composite containing carbon and silicon, silicon oxide (SiO X ) and the like. Examples of the binder include resin materials such as styrene butadiene rubber (SBR). Examples of the thickener include resin materials such as carboxymethyl cellulose (CMC).

[0018] Further, the separator 50 is an insulating sheet interposed between the positive electrode plate 30 and the negative electrode plate 40. For this separator 50, resin materials such as polyethylene (PE), polypropylene (PP), polyester, cellulose, polyamide, etc. are used, for example. Further, a heat-resistant layer containing an inorganic filler may be formed on the surface of the separator 50. Examples of such inorganic fillers include inorganic oxides such as aluminum oxide, magnesium oxide, silicon oxide, titanium oxide, nitrides such as aluminum nitride, silicon nitride, metal hydroxides such as calcium hydroxide, magnesium hydroxide, aluminum hydroxide, and clay minerals such as mica, talc, boehmite, zeolite, apatite, kaolin, etc.

[0019] (3) Electrolyte The electrolyte exists between the positive electrode plate 30 and the negative electrode plate 40. Thereby, charge carriers (Li ions) can be moved between the positive electrode plate 30 and the negative electrode plate 40. Examples of the electrolyte include non-aqueous electrolytes, gel electrolytes, etc. Note that the electrolyte can be used without particular limitation as long as it is an electrolyte that can be used in a lithium-ion secondary battery, and does not limit the technology disclosed herein.

[0020] As described above, as an example of the object to be recovered in the manufacturing method according to this embodiment, the lithium-ion secondary battery 1 has been described. However, the manufacturing method disclosed herein is not limited to only the method for recovering the lithium-ion secondary battery 1 having the above configuration. For example, at the manufacturing site of a lithium-ion secondary battery, a part of the positive electrode plate may be cut off when manufacturing the electrode body. Since a part of this cut-off positive electrode plate (process end material) may also contain Ni and Co, it can be an object to be recovered by the manufacturing method disclosed herein. Also, at the manufacturing site of a lithium-ion secondary battery, some defect may occur in the manufactured electrode body, making it unusable as a product. Since such an electrode body may also contain Ni and Co, it can be an object to be recovered. That is, the object to be recovered by the manufacturing method disclosed herein only needs to contain at least one of Ni and Co as a valuable metal, and is not particularly limited to a specific structure.

[0021] 2. Manufacturing Method of Battery Materials Hereinafter, a method for manufacturing a battery material according to this embodiment will be described. FIG. 3 is a flowchart for explaining the manufacturing method according to this embodiment. FIG. 4 is a flowchart for explaining in detail the solvent extraction step in FIG. 3.

[0022] As shown in FIG. 3, the method for manufacturing a battery material according to this embodiment includes a preparation step S10, an acid elution step S40, a neutralization precipitation step S50, a solid-liquid separation step S60, and an ammonia elution step S70. The method for manufacturing a battery material disclosed herein may further include a roasting step S20, a sorting step S30, a solvent extraction step S80, a Li crystallization step S90, a precursor preparation step S100, and an active material generation step S110. Further, the manufacturing method disclosed herein may further include other steps at any stage, and the other manufacturing processes may be the same as those in the prior art. Hereinafter, each step will be described.

[0023] (1) Preparation step S10 In the preparation step S10, a recovery target containing at least one of Ni and Co is prepared. As described above, the "recovery target" in the technology disclosed herein only needs to contain at least one of Ni and Co. That is, the recovery target is not limited to a completed lithium-ion secondary battery, and includes process end materials and defective parts (such as electrode bodies). Since the details of the recovery target have already been described, duplicate descriptions will be omitted.

[0024] (2) Roasting step S20 In the roasting step S20, the recovery target is heated at a predetermined temperature. Thereby, liquid components (such as electrolytes) in the recovery target can be removed, and resin components (such as binders and separators) can be carbonized. When the charged lithium-ion secondary battery 1 is used as the recovery target, the function of the battery can be stopped by performing the roasting step S20. Thereby, subsequent steps can be carried out safely. Regarding the method of the roasting step S20, the techniques used in conventional recovery techniques can be used without particular limitation, and since it does not characterize the technology disclosed herein, detailed description will be omitted.

[0025] Note that the baking process S20 is not essential and can be appropriately omitted as needed. For example, in the case of preparing a recovery target such as the process end material of the positive electrode plate 30 that does not require removal of liquid components and does not need to stop the function as a battery in the preparation process S10, the baking process S20 can be omitted, and valuable metals can still be efficiently recovered.

[0026] (3) Sorting process S30 In the sorting process S30, each member included in the recovery target is sorted. As the method of the sorting process S30, a conventionally known method can be used, and for example, sorting by a sieve, visual inspection, etc. can be performed. For example, when the process end material of the positive electrode plate 30 is the recovery target, the positive electrode core 32 may be sorted from the process end material and removed from the recovery target. Also, when the electrode body 20 is the recovery target, in addition to the positive electrode core 32, the negative electrode plate 40 may also be removed from the recovery target. Further, when the lithium-ion secondary battery 1 is the recovery target, in addition to the positive electrode core 32 and the negative electrode plate 40, the case 10 may also be removed from the recovery target. This can reduce the content of other metals (such as Al, Cu, etc.) in the recovery target, contributing to the improvement of the recovery efficiency of valuable metals (Co, Ni).

[0027] Note that in the sorting process S30, a crushing process may be performed on the recovery target as needed. This can improve the efficiency when sorting each member. For example, when the lithium-ion secondary battery 1 is the recovery target, the case 10 and the electrode body 20 may be crushed. This makes it easier to remove the case 10, the positive electrode core 32, and the negative electrode plate 40 from the recovery target.

[0028] In addition, the sorting step S30 is not a step intended to completely remove other metal components such as Al and Cu from the objects to be recovered. Although details will be described later, even if other metal components remain in the objects to be recovered, valuable metals (Ni and / or Co) and other metal components can be sufficiently separated in subsequent steps (for example, the neutralization precipitation step S50 and the ammonia leaching step S70). That is, the sorting step S30 can be appropriately omitted as necessary. For example, in the case of objects to be recovered with a low content of other metal components (such as the process end materials of the positive electrode plate 30), valuable metals can be efficiently recovered even if the sorting step S30 is omitted.

[0029] (4) Acid leaching step S40 In the acid leaching step S40, the object to be recovered after the preparation step S10 (or the roasting step S20, or the sorting step S30) is immersed in an acid solution. As a result, the valuable metals (Ni and / or Co) in the object to be recovered dissolve in the acid solution. In addition, in the acid leaching step S40, in addition to the valuable metals, other metal materials (such as Al) may also dissolve in the acid solution. That is, the acid solution (hereinafter also referred to as "acid leachate") that has undergone the acid leaching step S40 may contain, for example, Li, Al, Cu, Co, Ni, Mn, etc. Note that the procedure for acid leaching can adopt a conventionally known procedure without particular limitation. As an example, the pH of the acid solution used in the acid leaching step S40 is preferably -1.5 to 1.5 (more preferably -0.5 to 0.5). Thereby, the metal components in the object to be recovered can be preferably dissolved. Specific examples of the acid solution include inorganic acids such as sulfuric acid, nitric acid, hydrochloric acid, and phosphoric acid, and organic acids such as citric acid, ascorbic acid, oxalic acid, and acetic acid. In addition, in the acid leaching step S40, a reducing agent such as hydrogen peroxide can be added to the acid solution. Thereby, the dissolution rate of the object to be recovered into the acid solution is improved, and the acid leaching step S40 can be shortened. In addition, in the acid leaching step S40, it is preferable to perform a filtration treatment on the acid leachate after acid leaching. Thereby, undissolved components (such as carbon components) can be efficiently removed. Note that the temperature of the acid solution is preferably 50°C or higher (more preferably 55°C or higher, particularly preferably 60°C or higher). Thereby, the acid leaching step S40 can be shortened. In addition, the upper limit value of the temperature of the acid solution is not particularly limited, and it may be 90°C or lower, 85°C or lower, or 80°C or lower. The concentrations of Ni and Co (the sum of Ni and Co) in the acid leachate after the acid leaching step S40 are not particularly limited, but the higher the concentration, the more preferable from the viewpoint of productivity. Therefore, the concentrations of Ni and Co (the sum of Ni and Co) in the acid leachate are preferably 1.0 mol / L to 2.0 mol / L. The concentrations of Ni and Co (the sum of Ni and Co) in the acid leachate can be determined by ICP analysis.

[0030] (5) Neutralization precipitation step S50 In the neutralization precipitation step S50, a neutralizing agent is added to the acid leachate obtained in the acid leaching step S40 to raise the pH of the acid leachate. As a result, Al contained in the acid leachate becomes a hydroxide (Al(OH)3 ) It precipitates and settles out. As a result, a metal solution with Al approximately removed from the acid leachate containing Li, Al, Cu, Co, Ni, Mn, etc. can be obtained. Note that as the neutralizing agent used in the neutralization precipitation step S50, an alkaline solution with a pH of 11 to 15 (preferably pH 12 to 14) can be used. Specific examples of the neutralizing agent include an aqueous sodium hydroxide solution, calcium hydroxide, etc. Among them, it is preferable that the neutralizing agent contains an aqueous sodium hydroxide solution. The concentration of the neutralizing agent is not particularly limited, but from the perspective of productivity, the higher the concentration, the more preferable. Therefore, the concentration of the neutralizing agent is preferably 10 to 30 wt%.

[0031] Regarding the pH adjusted in the neutralization precipitation step S50, a pH of 5.0 or higher is preferable, a pH of 5.1 or higher is preferable, and a pH of 5.6 or higher is more preferable. When the pH of the acid leachate is low (typically less than pH 4.5), it is difficult for Al in the acid leachate to form a hydroxide. In other words, it is difficult to separate Al from the acid leachate. As the pH of the acid leachate increases, Al in the acid leachate can be precipitated as an Al hydroxide and settled. In other words, Al can be more preferably separated from the acid leachate. On the other hand, regarding the pH adjusted in the neutralization precipitation step S50, although not particularly limited, as the pH increases, a part of Ni and Co in the acid leachate may also form a hydroxide and precipitate in the metal solution. Therefore, regarding the pH adjusted in the neutralization precipitation step S50, a pH of 6.5 or lower is preferable, and a pH of 6.2 or lower is more preferable. Note that, as will be described in detail later, even when a part of Ni and Co precipitates, Ni and Co can be separated from the precipitate in a subsequent step (ammonia leaching step S70).

[0032] (6) Solid-liquid separation step S60 In the solid-liquid separation step S60, the metal solution after the neutralization precipitation step S50 and the precipitate are separated by solid-liquid separation. As a result, the precipitate and the metal solution containing valuable metals (Ni and / or Co) and other metal components can be obtained respectively. Since a conventionally known method can be used for the solid-liquid separation method, detailed description thereof is omitted here. The metal solution obtained in the solid-liquid separation step S60 is not particularly limited thereto, but by subjecting it to each subsequent recovery step (solvent extraction step S80) according to the metal components contained in the metal solution, each metal component contained in the metal solution can be recovered.

[0033] As described above, in the neutralization precipitation step S50, while Al in the acid leachate can be precipitated as a hydroxide, a part of Ni and / or Co also forms a hydroxide, and these hydroxides can also precipitate in the metal solution like the hydroxide of Al. That is, the precipitate obtained in the solid-liquid separation step S60 may contain valuable metals (Ni and / or Co) as hydroxides. In order to recover valuable metals (Ni and / or Co) from such a precipitate, for example, it is conceivable to return the precipitate to the acid leachate obtained in the acid leaching step S40 and dissolve it again. However, in this case, Al accumulates in the acid leachate (in other words, the Al concentration in the acid leachate increases), which is rather unfavorable because it leads to a decrease in the yield of valuable metals (Ni and / or Co). Here, as shown in FIG. 3, in the present embodiment, in addition to the neutralization precipitation step S50 and the solid-liquid separation step S60, an ammonia leaching step S70 is further provided. Thereby, the recovery efficiency of valuable metals (Ni and / or Co) can be significantly improved. This will be specifically described below.

[0034] (7) Ammonia leaching step S70 In the ammonia leaching step S70, the precipitate obtained by precipitation in the neutralization precipitation step S50 and separated by solid-liquid separation in the solid-liquid separation step S60 is immersed in an ammonia solution. As a result, Ni and / or Co in the precipitate can be separated, and an ammonia solution in which Ni and / or Co is dissolved (hereinafter referred to as "ammonia leachate") can be obtained. Specifically, hydroxides of Ni and Co typically form ammine complexes in an ammonia solution. Such ammine complexes dissolve in the ammonia solution. On the other hand, Al (and aluminum hydroxide) does not form an ammine complex in the ammonia solution and typically remains as a residue (precipitate) in the form of aluminum hydroxide (Al(OH) 3 ). This enables selective recovery of valuable metals (Ni and / or Co) in the precipitate. Note that the "ammonia solution" in this specification refers to an aqueous solution containing ammonium ions in water as a solvent.

[0035] As the ammonia solution, for example, a commercially available product (aqueous ammonia) may be purchased, or a solution obtained by dissolving at least a solvent containing water and an ammonia salt may be used. Examples of the ammonia salt used in the ammonia solution include ammonium hydroxide (NH 4 OH), ammonium sulfate ((NH 4 ) 2 SO 4 ), ammonium carbonate ((NH 4 ) 2 CO 3 ), ammonium bicarbonate (NH 4 HCO 3 ), ammonium chloride (NH 4 Cl), ammonium fluoride (NH 4 F), etc., which can be appropriately used. These compounds may be used alone or in combination of two or more.

[0036] In some preferred embodiments, it is preferable to include at least one selected from the group consisting of ammonium sulfate, ammonium chloride, and ammonium acetate in the above-described ammonia solution. These serve as so-called pH buffer materials for the ammonia solution. Specifically, they can lower the pH of the ammonia solution. By lowering the pH of the ammonia solution, while suppressing the dissolution of Al into the ammonia solution, Ni and Co can preferably form ammine complexes, enabling Ni and Co to be selectively and preferably dissolved in the ammonia solution. Furthermore, according to the above-described configuration, since the ammonia concentration of the ammonia solution can be increased, Ni and Co can preferably form ammine complexes and be preferably dissolved in the ammonia solution. Therefore, Ni and Co in the precipitate can be preferably selectively leached (recovered) into the ammonia solution.

[0037] In the ammonia leaching step S70, it is preferable to adjust the pH of the ammonia solution to pH 9.0 to 11.5 for ammonia leaching, and more preferably to adjust it to pH 9.5 to 10.0. As the pH of the ammonia solution decreases, Ni and Co can preferably form ammine complexes, so that these valuable metals (Ni and / or Co) can be preferably recovered. Also, when the pH is too high (typically exceeding pH 11.5), a part of Al in the precipitate forms a hydroxo complex ( 4 ) ― and begins to dissolve in the ammonia solution.

[0038] In the ammonia leaching step S70, the ammonia concentration in the ammonia solution is preferably 10 wt% or more, and more preferably 20 wt% or more. As the ammonia concentration increases, Ni and / or Co can preferably form ammine complexes, so that valuable metals (Ni and / or Co) can be recovered from the precipitate more efficiently. On the other hand, from the perspective of the high volatility of ammonia, the upper limit of the ammonia concentration in the ammonia solution is not limited to this, but is, for example, 35 wt% or less, and preferably 30 wt% or less.

[0039] Note that since ammonium ions in the ammonia solution are used for the formation of ammine complexes with Ni and / or Co, the pH and the concentration of free ammonia decrease as the ammonia leaching step progresses, compared to the initial ammonia solution (hereinafter also referred to as the "initial solution"). Therefore, an additional ammonia solution may be added during the ammonia leaching step S70. Thereby, the pH and the ammonia concentration in the ammonia solution can be maintained within a suitable range, and the valuable metals (Ni and / or Co) in the precipitate can be separated more efficiently. The pH of the additional ammonia solution may be the same as or higher than the pH of the initial solution. The ammonia concentration of the additional ammonia solution may be the same as or higher than the ammonia concentration of the initial solution. Also, the composition of the additional ammonia solution may be the same as or different from that of the initial solution.

[0040] In the ammonia leaching step S70, the temperature of the mixed solution is not particularly limited, but is preferably 25°C or higher, more preferably 40°C or higher, and particularly preferably 60°C or higher. Thereby, the time of the ammonia leaching step S70 can be shortened. On the other hand, the upper limit of the temperature of the mixed solution is not particularly limited, but is preferably 100°C or lower, more preferably 90°C or lower, and particularly preferably 80°C or lower.

[0041] Note that the leaching time in the ammonia leaching step S70 is not particularly limited because it can vary depending on, for example, the ammonia concentration and reaction temperature in the reaction solution, etc., but is generally preferably 0.5 hours or more, preferably 1 hour or more, and particularly preferably 2 hours or more. On the other hand, from the viewpoint of productivity, the leaching time is generally preferably 8 hours or less, preferably 6 hours or less, and particularly preferably 4 hours or less. Also, although not particularly limited, it is preferable to perform the ammonia leaching step S70 while stirring the ammonia solution. Thereby, since the contact area between the precipitate and the ammonia solution increases, the valuable metals (Ni and / or Co) can be efficiently dissolved in the ammonia solution. Therefore, the leaching time can be shortened.

[0042] After the ammonia leaching step S70, the ammonia leachate and the residue are separated by solid-liquid separation. As a result, an ammonia leachate in which Ni and / or Co is dissolved in an ammonia solution can be obtained. The use of the ammonia leachate is not particularly limited thereto, but for example, it can be suitably used as an alkaline solution in the precursor preparation step S100 described later. In this case, the ammonia leachate can be used as an alkaline solution as it is without going through steps such as washing. That is, there is no loss of valuable metals due to washing or re-extraction. Also, the valuable metals (Ni and / or Co) in the ammonia leachate can be used as a cathode active material precursor. Therefore, the recovery rate of the valuable metals (Ni and / or Co) contained in the object to be recovered can be improved.

[0043] As described above, in the manufacturing method disclosed herein, by leaching the precipitate obtained in the neutralization precipitation step with an ammonia solution, the valuable metals (Ni and / or Co) in the precipitate can be recovered. Conventionally, the valuable metals (Ni and / or Co) are separated by performing a neutralization precipitation step on the acid leachate that has undergone an acid leaching step. At this time, since a part of the valuable metals (Ni and / or Co) can also precipitate together with Al as a precipitate, there is a problem that loss of valuable metals occurs, or in order to reduce such loss, the pH cannot be sufficiently increased in the neutralization precipitation step and Al cannot be sufficiently separated from the acid leachate. On the other hand, in the manufacturing method disclosed herein, the valuable metals (Ni and / or Co) can be separated from the precipitate by the ammonia leaching step, and the recovery rate of such valuable metals can be improved.

[0044] (8) Solvent extraction step S80 In the solvent extraction step S80, each metal component (Ni and / or Co) is extracted from the metal solution using the solvent extraction method. Also, in the solvent extraction step S80, other metal components (such as Al) remaining in the metal solution can be separated. Specifically, as shown in FIG. 4, the solvent extraction step S80 in this embodiment includes a Co extraction step S81 and a Ni extraction step S82. Thereby, each of the Co solution and the Ni solution can be prepared. However, the solvent extraction step S80 can be appropriately added, changed, or deleted according to the metal components contained in the metal solution. This will be specifically described below.

[0045] (8-1) Co extraction step S81 In the Co extraction step S81, an organic solvent (first extraction solution) with high extractability for Co and low extractability for Li, Al, Cu, and Ni is added to the metal solution. Thereby, Co is separated from the metal solution, and a Co solution in which Co is dissolved in the first extraction solution can be obtained. Specific examples of the second extraction solution include phosphonic acid esters such as 2-ethylhexyl phosphonic acid 2-ethylhexyl (PC-88A). Also, as the first extraction solution, a mixture and dilution of these extractants may be used. And in the Co extraction step S81, the metal solution and the first extraction solution are stirred and suspended. Thereby, Co in the metal solution dissolves in the first extraction solution. Then, by allowing the two liquids to stand until they separate, a Co solution in which Co is dissolved in the first extraction solution and a metal solution from which Co has been removed can be obtained.

[0046] In the Co extraction step S81, a back-extraction treatment may be performed on the Co solution (first extraction solution containing Co) after extraction. In this back-extraction treatment, first, the Co solution (organic phase) and an acidic aqueous solution are stirred and mixed with a mixer or the like. Then, allow the two liquids to stand until they separate. Thereby, an aqueous Co solution can be obtained. Examples of the acidic aqueous solution used in the back-extraction treatment include sulfuric acid, hydrochloric acid, etc. (especially sulfuric acid).

[0047] (8-2) Ni extraction step S82 In the Ni extraction step S82, an organic solvent (second extract) having high extractability for Ni and low extractability for Li, Al, and Cu is added to the metal solution. As a result, Ni is separated from the metal solution, and an Ni solution in which Ni is dissolved in the second extract can be obtained. Specific examples of the third extract include carboxylic acid-based extractants such as neodecanoic acid and naphthenic acid. Further, a back-extraction treatment may also be performed on the Ni solution (second extract containing Ni) after extraction. Thereby, an aqueous Ni solution can be obtained. Since the procedure of the back-extraction treatment has already been described, duplicate descriptions are omitted.

[0048] (9) Li crystallization step S90 In the Li crystallization step S90, crystals of a Li compound are precipitated from the metal solution after the solvent extraction step S80. In the Li crystallization step S90, a conventionally known crystallization treatment can be employed without particular limitation. For example, in the Li crystallization step S90, sodium carbonate may be added to the metal solution. Thereby, crystals of lithium carbonate (Li 2 CO 3 ) can be precipitated. The Li compound produced in the Li crystallization step S90 is not limited to lithium carbonate. For example, if necessary, lithium hydroxide (LiOH) may be produced as the Li compound. In the production of this lithium hydroxide, first, the lithium carbonate precipitated from the metal solution is dissolved (or suspended) in a predetermined solvent. Then, calcium hydroxide is added to this solution. Thereafter, the solvent is evaporated and removed as necessary. Thereby, crystals of lithium hydroxide can be precipitated. However, in the production method disclosed herein, the Li crystallization step S90 is not essential. For example, when Li is not contained in the metal solution (in other words, when Li is not contained in the object to be recovered), the Li crystallization step S90 can also be omitted.

[0049] (10) Precursor preparation step S100 In the precursor preparation step S100, a cathode active material precursor (metal composite hydroxide) is prepared. In the precursor preparation step S100, a conventionally well-known method (such as a crystallization method etc.) can be adopted without particular limitation. For example, an aqueous solution containing a metal element source (typically a water-soluble ionic compound) is prepared. Next, an aqueous solution containing the prepared metal element source and an alkali solution (such as an ammonia solution etc.) are mixed in a reaction tank, and by stirring while controlling the pH of the mixed solution, metal composite hydroxide particles are coprecipitated and crystallized in the reaction tank, thereby implementing the process. Here, in the present embodiment, the ammonia leachate obtained in the ammonia leaching step S70 can be preferably used as the alkali solution. The ammonia leachate contains Ni and / or Co in the ammonia solution. For this reason, the ammonia leachate can be used directly as the alkali solution in the precursor preparation step S100 without the need for treatments such as washing. Therefore, Co and Ni in the ammonia solution can also be crystallized as the cathode active material precursor. That is, the valuable metals (Ni and / or Co) recovered from the precipitate in the ammonia leaching step S70 can be used efficiently.

[0050] Note that as described above, in the precursor preparation step S100, crystallization is performed while controlling the pH of the mixed solution. At this time, an alkali solution (NH 3 aqueous solution, NaOH aqueous solution etc.) can be dropped into the reaction tank. The amounts of Ni and Co in the metal solution obtained in the ammonia leaching step S70 can be determined by ICP analysis. For this reason, depending on the composition of the target cathode active material, metal components such as Ni, Co, or other Mn etc. may be added. Such metal components can be added in the form of metal sulfates, hydrates etc. Also, in this case, various metal components obtained in the solvent extraction step S80 may be used as the metal components.

[0051] (11) Active material formation step S110 In the active material formation step S110, the metal compound obtained in the precursor preparation step S100 and a Li compound (for example, Li 2 CO 3A battery material (cathode active material) is produced using, for example, etc. For example, the cathode active material precursor (metal composite hydroxide) obtained in the above precursor production step S100 and a Li compound are mixed, and the mixture is fired. Thereby, a cathode active material (lithium transition metal composite oxide) of a lithium ion secondary battery can be manufactured. Note that, as the Li compound, the Li compound obtained in the Li crystallization step S90 may be used.

[0052] As described above, the manufacturing method of the battery material according to the present embodiment has been described. As described above, in the manufacturing method according to the present embodiment, an ammonia leaching step of immersing the precipitate obtained by the neutralization precipitation step in an ammonia solution is performed. Thereby, Ni and / or Co contained in the precipitate are dissolved in the ammonia solution, and an ammonia leachate containing Ni and / or Co can be obtained. Therefore, valuable metals (Ni and / or Co) precipitated as a part of the precipitate during the neutralization precipitation step can be suitably recovered (manufactured), in other words, the recovery rate of the valuable metals can be improved. Further, the ammonia leachate obtained by the manufacturing method disclosed herein can be used as it is in the precursor production step S100 without performing steps such as washing. Thereby, valuable metals (Ni and / or Co) contained in the ammonia leachate can be used as a cathode active material precursor. Therefore, valuable metals (Ni and / or Co) can be efficiently recovered, and the recovery rate of the valuable metals can be significantly improved.

[0053] 3. Other Embodiments As described above, one embodiment of the technology disclosed herein has been described. Note that the technology disclosed herein is not limited to the above-described embodiment, and includes other embodiments in which various configurations are changed. Hereinafter, other examples of the embodiments of the technology disclosed herein will be described.

[0054] (a) Modification of the Solvent Extraction Step The specific treatment procedures in the solvent extraction step S80 can be changed as appropriate. For example, the solvent extraction step S80 in the above-described embodiment includes a Co extraction step and a Ni extraction step. Thereby, a Co solution and a Ni solution can be extracted individually. However, in the solvent extraction step S80, Ni and Co may be extracted simultaneously. Thereby, it is possible to improve the manufacturing efficiency by shortening the process.

[0055] In addition, the steps that can be included in the solvent extraction step S80 are not limited to the above-described Co extraction step and Ni extraction step. For example, when the metal solution further contains manganese (Mn) as a metal component, an Mn extraction step for extracting Mn from the metal solution can be further included in the solvent extraction step S80. The means of the Mn extraction step is not particularly limited, but it can be carried out by adding an organic solvent (third extraction solution) having high extractability for Mn and low extractability for Li, Al, Cu, Co, and Ni to the metal solution. As this third extraction solution, a phosphoric acid ester-based extractant, an oxime-based extractant, or the like can be used. Specific examples of the phosphoric acid ester-based extractant include di-2-ethylhexyl phosphoric acid (D2EHPA) and the like. Specific examples of the oxime-based extractant include 2-hydroxy-5-nonylacetophenone oxime (LIX84), 5-dodecylsalicylaldoxime (LIX860), 5-nonylsalicylaldoxime (ACORGA M5640), and the like. Further, as the third extraction solution, a mixture and dilution of these extractants may be used. Also, a back-extraction treatment may be performed on the Mn solution (third extraction solution containing Mn) after extraction. Note that since the specific extraction method and the method of the back-extraction treatment may be the same as those of the above-described Co extraction step S81 and Ni extraction step S82, the description thereof is omitted here.

[0056] (b) Omission of the solvent extraction step Also, according to the manufacturing method disclosed herein, the solvent extraction step S80 can be omitted. Specifically, as described above, in the technology disclosed herein, Al can be separated from the metal solution by the neutralization precipitation step S50. Therefore, a solution containing valuable metals (Ni and / or Co) with high purity can be obtained. Thus, when using a recovery target that does not contain Cu, such as the end material of the positive electrode plate 30, the mixed solution of valuable metals (aqueous solution containing a metal element source) used in the precursor preparation step S100 can be obtained without performing the solvent extraction step S80.

[0057] On the other hand, when Li is contained in the metal solution, as an example of means for recovering Li, the following means can be mentioned. First, when performing the roasting step S20, a non-metal chlorine compound (such as HCl) is added to the recovery target for roasting. As a result, Li in the recovery target reacts with the non-metal chlorine compound to generate LiCl. Next, a water leaching step of immersing the roasted recovery target in water is performed. Since the above LiCl is a water-soluble compound, Li can be recovered only by bringing the recovery target into contact with water. Thereby, while recovering (manufacturing) Li in the metal solution, the mixed solution of valuable metals (aqueous solution containing a metal element source) used in the precursor preparation step S100 can be obtained without performing the solvent extraction step S80. That is, the description regarding the above-described embodiments is not intended to limit each step. In the manufacturing method disclosed herein, each step may be appropriately added, deleted, or changed as necessary.

[0058] (c) Addition of Li separation step Also, in some embodiments, a Li separation step may be performed on the metal solution after the solvent extraction step S80. The Li separation step is a step of further removing Cu and Al from the metal solution to prepare a high-concentration Li solution. Thereby, in the Li crystallization step S90, a high-purity Li compound can be obtained. The means for preparing the Li solution is not particularly limited, and it is preferable to appropriately employ conventionally known means such as a solvent extraction method and an ion exchange method. Instead of the Li concentration step, only evaporation of the solvent may be performed. Even in this case, a high-concentration Li solution can be obtained.

[0059] (d) Addition of Li concentration step Moreover, a Li concentration step may be performed on the metal solution after the Li separation step. In this Li concentration step, the Li solution is heated to evaporate the solvent. As a result, a high-concentration Li solution can be obtained, so that the crystallization efficiency in the Li crystallization step S90 can be improved. Note that this Li concentration step may be performed on a metal solution that has not undergone the Li separation step. Even in this case, a high-concentration Li solution can be obtained.

[0060] [Test Example] Hereinafter, test examples related to the technology disclosed herein will be described. Note that the content of the test examples described below is not intended to limit the technology disclosed herein.

[0061] <Test Example 1: Examination of pH during neutralization precipitation step> (Example 1) [Preparation of sample] In this test, the positive electrode plate was the object to be recovered, and the following steps were performed on the object to be recovered. Specifically, as the positive electrode plate, one in which a positive electrode active material layer was coated on the surface of a positive electrode core (Al foil) was used. Note that the positive electrode active material in this test was lithium nickel cobalt manganese composite oxide (LiNi 1 / 3 Co 1 / 3 Mn 1 / 3 O 2 ) was used. Then, this positive electrode plate was crushed, and the powder passed through a sieve with an opening of 500 μm was used as a test sample. When the powder of the test sample was analyzed by ICP, the mass ratio of Al to the total amount of Ni and Co in the sample was 4 wt%.

[0062] [Acid leaching step] Next, the test sample, sulfuric acid (H 2 SO 4 )(concentration 2 mol / L) as an acid solution, and hydrogen peroxide (H 2 O 2)(A mixed solution (pH 0.01) with a concentration of 0.6 mol / L) was mixed. Then, while maintaining the acid solution at 80 °C, a stirring treatment was carried out at a stirring speed of 600 rpm for 6 hours. After stirring, the acid leachate was filtered, and the obtained acid leachate was analyzed by ICP to measure the amount of each substance of Al, Ni, and Co. Incidentally, as a result of the above ICP measurement, the concentration (sum of Ni and Co) of Ni and Co in the acid leachate was 1.0 mol / L.

[0063] [Neutralization precipitation process] The acid leachate obtained above was maintained at 25 °C, and a 10 wt% sodium hydroxide solution was dropped into the acid leachate while stirring at a stirring speed of 600 rpm. The dropping of sodium hydroxide was stopped when the pH of the acid leachate reached 5.1. After the dropping was stopped, stirring was continued at a stirring speed of 600 rpm for 10 minutes to confirm that there was no change in pH. Then, the metal solution and the precipitate were separated by solid-liquid separation by filtration.

[0064] (Example 2) In the neutralization precipitation process, the dropping of sodium hydroxide was stopped when the pH of the acid leachate reached 5.6. Otherwise, it was the same as in Example 1.

[0065] (Example 3) In the neutralization precipitation process, the dropping of sodium hydroxide was stopped when the pH of the acid leachate reached 6.2. Otherwise, it was the same as in Example 1.

[0066] [Residual rate in the metal solution in the neutralization precipitation process] The residual rates of valuable metals (Ni, Co) and Al in the metal solutions according to each example after the neutralization precipitation process were calculated. Specifically, first, ICP was performed on the metal solution to measure the amount of each substance of Ni, Co, and Al in the metal solution. Then, based on the following formulas (1) and (2), the Ni and Co residual rates in the metal solution and the Al residual rate in the metal solution compared with the acid leachate according to each example (i.e., before the neutralization precipitation process) were calculated respectively. The results are shown in Table 1. Residual ratio of Ni and Co in the metal solution (%) = {(amount of Ni substance in the metal solution + amount of Co substance in the metal solution) / (amount of Ni substance in the acid leachate + amount of Co substance in the acid leachate)} × 100…(1) Residual ratio of Al in the metal solution (%) = (amount of Al substance in the metal solution / amount of Al substance in the acid leachate) × 100…(2)

[0067] [Ratio of Ni and Co in the precipitate in the neutralization precipitation process] In addition, the ratio of the amount of valuable metals (Ni, Co) to the amount of Al in the precipitate according to each example after the neutralization precipitation process was calculated. Specifically, first, ICP was performed on the precipitate after the neutralization precipitation process to measure the amount of each substance of Ni, Co, and Al in the precipitate. Then, based on the following formula (3), the ratio of the amount of valuable metals (Ni, Co) substances in the precipitate according to each example was calculated. The results are shown in Table 1. Ratio of Ni and Co in the precipitate (%) = {(amount of Ni substance in the precipitate + amount of Co substance in the precipitate) / amount of Al substance in the precipitate} × 100…(3)

[0068]

Table 1

[0069] As shown in the results of Table 1, in Example 1 where the pH during precipitation was 5.1 in the neutralization precipitation process, the residual ratio of Al in the metal solution was 1.5%. From this, it can be seen that when the acid leachate is neutralized to a pH of 5.1, almost all of the Al contained in the acid leachate can be neutralized and precipitated. Comparing Examples 1 to 3, the higher the pH during precipitation, the lower the residual ratio of Al in the metal solution. In Example 3 where the pH during precipitation was 6.2, the residual ratio of Al in the metal solution was the lowest. On the other hand, in Example 3, the residual ratio of Ni and Co in the metal solution was the lowest, and the ratio of Ni and Co in the precipitate was the highest.

[0070] <Test Example 2: Examination of the ammonia leaching process> (Example 4) [Ammonia leaching process] Ammonia leaching was performed on the precipitate obtained by the neutralization precipitation process described above. Specifically, first, as an ammonia solution, ammonia water with a pH of 11.2 (ammonia concentration in the solution: 1.5 wt%) was prepared. Then, the precipitate according to Example 1 obtained by the above-described neutralization precipitation process was placed in the ammonia solution. Then, while maintaining the ammonia solution at 80 °C, stirring treatment was performed at a stirring speed of 600 rpm for 2 hours. When a decrease in the pH in the solution was observed during stirring, an additional ammonia solution with an ammonia concentration of 28 wt% was added to adjust the pH to 11.2. After stirring, the ammonia leachate and the residue were separated by filtration into a solid and a liquid.

[0071] (Example 5) In Example 5, the ammonia leaching step was carried out such that the pH of the ammonia solution was 12.1 (ammonia concentration in the solution: 10.0 wt%). Otherwise, it was the same as in Example 4.

[0072] (Example 6) In Example 6, ammonium sulfate ((NH 4 ) 2 SO 4 ) as a pH buffer was added to ammonia water with a pH of 12.1 (ammonia concentration in the solution: 10.0 wt%) as the ammonia solution in an amount of 2 mol / L. Thereby, the ammonia leaching step was carried out such that the pH of the ammonia solution was 9.6. Otherwise, it was the same as in Example 4.

[0073] (Examples 7 to 9) In Example 7, the ammonia leaching step was carried out using the precipitate according to Example 2. Otherwise, it was the same as in Example 4. In Example 8, the ammonia leaching step was carried out using the precipitate according to Example 2. Otherwise, it was the same as in Example 5. In Example 9, the ammonia leaching step was carried out using the precipitate according to Example 2. Otherwise, it was the same as in Example 6.

[0074] (Examples 10 to 12) In Example 10, the ammonia leaching step was performed using the precipitate according to Example 3. Other than this, it was the same as in Example 4. In Example 11, the ammonia leaching step was performed using the precipitate according to Example 3. Other than this, it was the same as in Example 5. In Example 12, the ammonia leaching step was performed using the precipitate according to Example 3. Other than this, it was the same as in Example 6.

[0075] (Example 13) In Example 13, the ammonia leaching step was performed while maintaining the temperature of the ammonia solution at 25°C. Other than this, it was the same as in Example 12.

[0076] [Residual rate of Ni and Co in the residue] The residual rates of valuable metals (Ni, Co) in the residue according to each example after the ammonia leaching step were calculated. Specifically, first, ICP was performed on the residue to measure the amounts of substances of Ni, Co, and Al in the residue. Then, based on the following formula (4), the ratio of the amount of valuable metals (Ni, Co) in the residue to the amount of Al in the residue according to each example was calculated. The results are shown in Table 2. Residual rate of Ni and Co in the residue (%) = {(Amount of Ni substance in the residue + Amount of Co substance in the residue) / Amount of Al substance in the residue} × 100…(4)

[0077] [Al leaching rate in the ammonia leaching solution] The Al leaching rate in the ammonia leaching solution according to each example after the ammonia leaching step was calculated. Specifically, first, ICP was performed on the ammonia leaching solution to measure the amount of Al substance in the ammonia leaching solution. Then, based on the following formula (5), the ratio of the amount of Al substance in the ammonia leaching solution to the amount of Al substance in the residue according to each example was calculated. The results are shown in Table 2. Al leaching rate in the ammonia leaching solution (%) = (Amount of Al substance in the ammonia leaching solution / Amount of Al substance in the residue) × 100…(5)

[0078]

Table 2

[0079] As shown in the results of Table 2, in Example 4 where the pH of the ammonia solution was 11.2, the Ni and Co ratios in the residue were significantly lower than the Ni and Co ratios in the precipitate (i.e., before the ammonia leaching step). Also, the Al leaching rate in the ammonia leachate of Example 4 was 0.2%. From this, it can be seen that in Example 4, Ni and Co in the precipitate were preferably selectively recovered by ammonia leaching. On the other hand, as shown in Example 5, when the pH of the ammonia solution was 12.1, while there was a recovery effect of Ni and Co in the precipitate by ammonia leaching, the Al leaching rate in the ammonia leachate was higher than that in Example 4. Also, when comparing Examples 4 to 6, in Example 6 where ammonium sulfate was contained in the ammonia solution, the Al leaching rate in the ammonia leachate was the lowest, and the Ni and Co ratios in the residue were the lowest.

[0080] As shown in the results of Examples 7 to 9 and Examples 10 to 12, it can be seen that even when using the precipitates according to Examples 2 and 3 with different pH values during neutralization precipitation, the same results as in Examples 4 to 6 can be obtained. From the results of Example 13, it can be seen that Ni and Co can be selectively recovered from the precipitate even when the temperature of the ammonia solution is 25°C, and Al leaching into the ammonia leachate is also suppressed. When comparing Example 12 and Example 13, the Ni and Co ratios in the residue were lower in Example 12 where the temperature of the ammonia solution was 80°C.

[0081] Although the technologies disclosed herein have been described in detail above, these are merely examples and do not limit the scope of the claims. The technologies described in the claims include various modifications and changes of the specific examples exemplified above. That is, the technologies disclosed herein include the forms described in Items 1 to 7 below.

[0082] <Item 1> A preparation step of preparing a recovery target containing at least one of Ni and Co, An acid leaching step of immersing the above recovery target in an acid solution to obtain an acid leachate, A neutralization precipitation step of mixing the above acid leachate and a neutralizing agent to obtain a precipitate, A solid-liquid separation step of separating the precipitate by solid-liquid separation, An ammonia leaching step of immersing the separated precipitate in an ammonia solution containing ammonium ions to obtain an ammonia leachate containing at least one of the above Ni and Co, and A method for manufacturing a battery material.

[0083] <Item 2> The method for manufacturing a battery material according to Item 1, wherein the pH of the ammonia solution is adjusted to 9.0 to 11.5 to perform the ammonia leaching step.

[0084] <Item 3> The method for manufacturing a battery material according to Item 1 or 2, wherein the ammonia solution contains at least one selected from the group consisting of ammonium sulfate, ammonium chloride, and ammonium acetate.

[0085] <Item 4> The method for manufacturing a battery material according to any one of Items 1 to 3, further comprising a precursor preparation step of preparing a positive electrode active material precursor using the ammonia leachate obtained in the ammonia leaching step.

[0086] <Item 5> The method for manufacturing a battery material according to any one of Items 1 to 4, wherein the ammonia leaching step is performed at a temperature of 25 to 100°C for the ammonia solution.

[0087] <Item 6> The method for manufacturing a battery material according to any one of Items 1 to 5, wherein in the neutralization precipitation step, the pH of the acid leachate is neutralized to 5.0 to 6.5.

[0088] <Item 7> The method for manufacturing a battery material according to any one of Items 1 to 6, wherein the object to be recovered contains at least one selected from the group consisting of lithium nickel composite oxide, lithium cobalt composite oxide, lithium nickel manganese composite oxide, lithium manganese cobalt composite oxide, lithium nickel cobalt composite oxide, and lithium nickel manganese cobalt composite oxide.

Description of Symbols

[0089] 1 Lithium-ion secondary battery 10 Case 12 Positive electrode terminal 14 Negative electrode terminal 20 Electrode body 30 Positive electrode plate 32 Positive electrode core 34 Positive electrode active material layer 40 Negative electrode plate 42 Negative electrode core 44 Negative electrode active material layer 50 Separator

Claims

1. A preparation step of preparing a recovery target containing at least one of Ni and Co; An acid leaching step of immersing the recovery target in an acid solution to obtain an acid leachate; A neutralization precipitation step of mixing the acid leachate and a neutralizing agent to obtain a precipitate; A solid-liquid separation step of performing solid-liquid separation on the precipitate; An ammonia leaching step of immersing the separated precipitate in an ammonia solution containing ammonium ions to obtain an ammonia leachate containing at least one of Ni and Co. A method for manufacturing a battery material.

2. The method for manufacturing a battery material according to Claim 1, wherein the ammonia leaching step is performed by adjusting the pH of the ammonia solution to 9.0 to 11.

5.

3. The method for manufacturing a battery material according to Claim 1 or 2, wherein the ammonia solution contains at least one selected from the group consisting of ammonium sulfate, ammonium chloride, and ammonium acetate.

4. The method for manufacturing a battery material according to Claim 1 or 2, further comprising a precursor preparation step of preparing a cathode active material precursor using the ammonia leachate obtained in the ammonia leaching step.

5. The method for manufacturing a battery material according to Claim 1 or 2, wherein the ammonia leaching step is performed at a temperature of 25 to 100°C for the ammonia solution.

6. The method for manufacturing a battery material according to Claim 1 or 2, wherein in the neutralization precipitation step, the pH of the acid leachate is neutralized to 5.0 to 6.

5.

7. The method for manufacturing a battery material according to Claim 1 or 2, wherein the recovery target contains at least one selected from the group consisting of lithium nickel composite oxide, lithium cobalt composite oxide, lithium nickel manganese composite oxide, lithium manganese cobalt composite oxide, lithium nickel cobalt composite oxide, and lithium nickel manganese cobalt composite oxide.

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