CN113871744B - Method for recycling waste lithium ion battery anode active material - Google Patents
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Abstract
Method for recovering waste lithium ion battery anode active materialThe method belongs to the field of wet metallurgy. With waste lithium ion battery positive active material (Li) 21.4 Ni 1.5 Co 7.6 MnO 4.5 ) The method comprises the steps of taking a deep eutectic solvent (a solution formed by ethylene glycol and oxalic acid dihydrate) as a leaching system as a raw material, obtaining a leaching solution only containing lithium and a precipitate of oxalate dihydrate of nickel, cobalt and manganese in one step after leaching is finished, and realizing efficient separation and recovery of lithium and nickel, cobalt and manganese, wherein the ethylene glycol is used as the solvent, and the oxalic acid dihydrate is used as a reducing agent and a coordination agent. Firstly, mixing, heating and stirring ethylene glycol and oxalic acid dihydrate to obtain a deep eutectic solvent. And then, mixing and stirring the lithium nickel cobalt manganese oxide powder and the prepared deep eutectic solvent under the water bath condition, thereby realizing the high-efficiency separation and recovery of lithium and nickel cobalt manganese in the anode active material of the waste lithium ion battery. The invention adopts a difunctional deep eutectic solvent consisting of glycol and oxalic acid dihydrate as a leaching system, and the recovery efficiency of lithium, nickel, cobalt and manganese reaches more than 99 percent.
Description
Technical Field
The invention belongs to the field of hydrometallurgy, and realizes the efficient separation and recovery of lithium, nickel, cobalt and manganese in a positive active material of a waste lithium ion battery by adopting a hydrometallurgy method and taking a bifunctional deep eutectic solvent (a solution formed by glycol and oxalic acid dihydrate) as a leaching system.
Background
The lithium ion battery has the advantages of large energy density, high working voltage, high charging and discharging efficiency, wide temperature application range, long service life and the like, is widely applied to various mobile devices including mobile phones, notebook computers, digital cameras, electric automobiles and the like, and is more relevant to the daily life of people. The lithium nickel cobalt manganese oxide battery has the advantages of good stability, excellent cycle performance, low cost and high capacity, and the total market proportion exceeds 50% ((1) Meng Ji, university of Kunming technology 2018, (2) Jing Ankun, beijing technology 2020).
China is the largest lithium ion battery producing country and consuming country in the world, the lithium battery output of China reaches 188.5 hundred million in 2020, and 50 million tons of waste lithium ion batteries are produced cumulatively. However, more than 50% of the waste lithium ion batteries are not recycled, causing serious environmental pollution (toxic electrolyte and heavy metals) and waste of metal resources (nickel, cobalt, manganese, lithium, etc.). Research on the recovery of waste lithium ion batteries mainly focuses on the recovery of valuable metals such as cobalt and lithium from high value-added positive electrode active materials. The traditional pyrometallurgical process causes dust pollution, and has high energy consumption and low metal recovery rate. Hydrometallurgical processes using aqueous mineral acid leaching have low energy consumption and high metal recovery, but produce large amounts of refractory acidic wastewater (y.l.yao, m.y.zhu, z.zhu, b.h.tung, y.q.fan, z.s.hua, ACS sustaineble chem.eng.11 (2018). 13611-13627.).
In the background of green chemistry, the solvent metallurgy using non-aqueous solvent as leaching system can avoid the discharge of waste water, and is concerned by researchers. Among them, a deep eutectic solvent which is a liquid phase at room temperature is formed by a quaternary ammonium salt (a hydrogen bond acceptor, mainly choline chloride) and a hydrogen bond donor (amide/carboxylic acid/organic alcohol) through hydrogen bonds, and a large number of molecules or ions (amide, carboxylic acid or halogen ion) which can coordinate with metal ions exist in the components, so that the deep eutectic solvent has the capability of dissolving a large number of metal salts and metal oxides, can be synthesized from green components and is easy to prepare, and becomes the first choice of a leaching system (e.l.smith, a.p.abbott, k.s.ryder, chem.rev.,114 (2014), 11060-11082.). So far, deep eutectic solvents have been gradually used for extracting metals from zinc-containing electric furnace dust, waste lithium ion battery positive electrode active materials, and other metal resources ((1) a.p.abbott, j.collins, i.dalryple, r.c.harris, r.microstructure, f.qiu, j.scherrer, w.r.wise, aust.j.chem.,62 (2009), 341. (2) m.k.tran, m.f.rodrigues, k.kaka, g.babu, p.m.ajayan, nat.energy,4 (2019), 339-345.). In 2019, tran et al used a deep eutectic solvent (a eutectic mixture of 1mol choline chloride and 2mol ethylene glycol, expressed as 1 choline chloride: 2 ethylene glycol) for the first time to leach lithium cobaltate. Reaction at 220 ℃ 24h, over 90% of the cobalt and lithium are leached (m.k. Tran, m.f. Rodrigues, k.kato, g.babu, p.m. Ajayan, nat. Energy,4 (2019), 339-345.). Subsequently, some research teams aimed at the leaching of lithium cobaltate, using 1 choline chloride: 2 urea, 1 choline chloride: 1-p-toluenesulfonic dihydrate and the like can achieve more than 90% of leaching efficiency by being used as a leaching system ((1) S.Wang, Z.Zhang, Z.Lu, Z.Xu, green chem.,2020,22 (14): 4473-4482. (2) M.J.Rold. N-Ruiz, M.L.Ferrer, M.C.Guti errez, F.D.Monte, ACS Sustainable chem. Eng.,8 (2020), 5437-5445.). However, a large amount of coordination components (chloride ions, amide and the like) in the leaching system can form soluble complexes with cobalt ions, so that efficient separation and recovery of lithium and cobalt cannot be realized in one step, and a complex subsequent separation process is required, so that the recovery efficiency of metal is reduced, and the process cost is increased. Therefore, aiming at the nickel-cobalt lithium manganate battery with the largest market share, the novel bifunctional deep eutectic solvent is designed to realize the significant significance of one-step efficient separation and recovery of lithium, nickel, cobalt and manganese, and the method has great economic benefit.
Disclosure of Invention
The invention aims to realize the efficient separation and recovery of lithium and nickel cobalt manganese in the anode active material (nickel cobalt lithium manganate) of the waste lithium ion battery by one step. The invention adopts a bifunctional deep eutectic solvent (a solution formed by glycol and oxalic acid dihydrate) as a leaching system, wherein the glycol is used as the solvent, the oxalic acid dihydrate is used as a reducing agent and a coordination agent, and anode active material powder (Li) is prepared by mixing 21.4 Ni 1.5 Co 7.6 MnO 4.5 ) The lithium-containing cobalt-nickel-manganese dioxide is mixed with a deep eutectic solvent, heated and stirred to complete leaching of lithium and reduction coordination of nickel, cobalt and manganese, a leaching solution only containing lithium and a dihydrate oxalate precipitate of nickel, cobalt and manganese are obtained, and one-step efficient separation and recovery of lithium, nickel, cobalt and manganese are realized.
A method for recycling the active material of the anode of a waste lithium ion battery is characterized in that a bifunctional deep eutectic solvent is used for efficiently separating and recycling lithium, nickel, cobalt and manganese, and the specific process steps are as follows:
(1) Under the condition of water bath at 40-60 ℃, mixing and stirring ethylene glycol and oxalic acid dihydrate with the molar ratio of 2:1-5:1 for 5-30min to obtain a clear and transparent bifunctional deep eutectic solvent;
(2) Mixing the bifunctional deep eutectic solvent obtained in the step (1) and the anode active material powder according to a solid-liquid ratio of 4-80g/L, stirring for 12-24h under a water bath condition of 85-95 ℃, and performing solid-liquid separation to obtain a leaching solution and a solid-phase product;
(3) Washing the solid phase product 1-3 times by respectively using deionized water and absolute ethyl alcohol, then drying the solid phase product in an oven at the temperature of 60-100 ℃ for 6-12h, and grinding to obtain the dihydrate oxalate powder of nickel, cobalt and manganese.
Further, the positive active material powder used in the step (2) is from waste lithium ion batteries of samsung, and is nickel cobalt lithium manganate (Li) obtained by adopting a pretreatment process on lithium batteries 21.4 Ni 1.5 Co 7.6 MnO 4.5 ) The pretreatment process comprises the following steps: discharging saturated sodium chloride solution, manually disassembling the anode, dissolving aluminum foil by using sodium hydroxide solution, and calcining at high temperature to remove binder impurities.
Further, the glycol in the leaching system used in the step (2) is used as a solvent, and the oxalic acid dihydrate is used as a reducing agent and a complexing agent, so that additional water, the reducing agent and the complexing agent are not required.
Further, the leaching efficiency of lithium in the step (2) is over 99%, and the obtained leaching solution only contains lithium.
Further, the solid-phase product obtained in the step (3) is a nickel-cobalt-manganese dihydrate oxalate precipitate with a nanorod structure, and the recovery efficiency of nickel-cobalt-manganese exceeds 99%.
In the research, a bifunctional deep eutectic solvent (a solution formed by ethylene glycol and oxalic acid dihydrate) is used as a leaching system, so that the efficient separation and recovery of lithium and nickel, cobalt and manganese in the positive active material of the waste lithium ion battery are realized in one step, the leaching of lithium and the reduction coordination of nickel, cobalt and manganese are completed simultaneously, and a leaching solution only containing lithium and a precipitation of oxalate dihydrate of nickel, cobalt and manganese are obtained, wherein the reaction mechanism is shown in the following formula.
2LiMO 2 (s)+8H + (aq)+3C 2 O 4 2- (aq)→2Li + (aq)+2MC 2 O 4 ·2H 2 O(s)+2CO 2 (g)
M：Ni/Co/Mn
In the high-efficiency recovery process of the anode active material of the waste lithium ion battery, glycol in a leaching system is used as a solvent, oxalic acid dihydrate is used as a reducing agent and a coordination agent, and Li in crystal lattices of the active material + First by H from oxalic acid + Substitution of Li + Is leached into solution and subsequently in H + Residual high valence transition metal ion M 3+ Oxide coating C 2 O 4 2- Reduction to M 2 + And is combined with C 2 O 4 2- And carrying out coordination reaction to generate oxalate precipitate.
The content of lithium, nickel, cobalt and manganese in the leaching solution is detected and calculated, the leaching efficiency of lithium reaches over 99 percent, and only lithium is contained in the leaching solution. And (3) detecting the washed, dried and ground solid-phase product, wherein the result shows that the product is the dihydrate oxalate of nickel, cobalt and manganese with a nano rod-shaped structure, and other impurities are not found. The invention proves that the deep eutectic solvent and the anode active material powder are mixed, heated and stirred, so that the dual-function characteristic of the deep eutectic solvent is realized in one step, namely, the high-efficiency separation and recovery of lithium, nickel, cobalt and manganese are realized, and only a lithium-containing leaching solution and a nickel, cobalt and manganese dihydrate oxalate precipitate are obtained, which has reference significance for the high-efficiency recovery of other waste lithium ion battery anode active materials.
The invention has the advantages that: aiming at the nickel cobalt lithium manganate battery with the market ratio of the current lithium battery exceeding 50%, a bifunctional deep eutectic solvent (a solution formed by ethylene glycol and oxalic acid dihydrate) is designed for the first time to serve as a leaching system, so that the efficient separation and recovery of lithium and nickel cobalt manganese in the anode active material of the waste lithium ion battery are realized in one step, the leaching efficiency of lithium and the recovery efficiency of nickel cobalt manganese both exceed 99%, a leaching solution only containing lithium and an oxalate dihydrate precipitate of nickel cobalt manganese are obtained, and the efficient recovery of the anode active material of the waste lithium ion battery is realized. The invention adopts the solution synthesized by the glycol and the oxalic acid dihydrate as a leaching system, does not need to additionally add water, a reducing agent and a coordination agent, reduces the cost of the process and has simple process flow. The method has the advantages that valuable metals are efficiently recovered from the anode active materials of the waste lithium ion batteries, so that the pressure of resources and the environment is relieved, and a new thought is provided for efficiently recovering other anode active materials of the waste lithium ion batteries.
Drawings
FIG. 1: the FT-IR spectrum of the deep eutectic solvent,
FIG. 2: XRD patterns and SEM pictures of the cathode active material,
FIG. 3: a process flow chart for efficiently separating and recovering valuable metals in the waste LIBs in one step,
FIG. 4 is a schematic view of: XRD pattern and SEM pictures of solid phase product.
Detailed Description
The leaching system is derived from the components of ethylene glycol (liquid phase) and oxalic acid dihydrate (solid phase) which are analytical pure reagents of a national reagent group, and the Fourier infrared spectrum (FT-IR) of a deep eutectic solvent (a solution formed by 5mol of ethylene glycol and 1mol of oxalic acid dihydrate) obtained by mixing and heating is shown in figure 1, so that the deep eutectic solvent contains a large amount of carboxyl groups (C = O,1746 cm) belonging to oxalic acid -1 ) Functional groups and hydroxyl groups of ethylene glycol (O-H, 3380 cm) -1 ，1082cm -1 ，1035cm -1 ) The absorption peak of the functional group and oxalic acid molecules in the deep eutectic solvent can be used as a reducing agent and a complexing agent to participate in the subsequent leaching reaction process.
Source of raw materials
The used raw material (anode active material powder) is from a waste lithium ion battery (ICR 18650-26 FM) of Samsung, and is obtained by adopting a pretreatment process (discharging with saturated sodium chloride solution, manually disassembling an anode, dissolving aluminum foil with sodium hydroxide solution and calcining at high temperature to remove impurities such as a binder) on the lithium battery. As shown in X-ray diffraction (XRD) pattern of fig. 2 (a), the obtained positive active material was found to have no other than LiCoO 2 In addition to the diffraction peaks consistent with standard cards (JCPDS: 50-0653), there are some coincidences (Li) 0.95 Ni 0.05 )Ni 0.79 Mn 0.21 )O 2 The diffraction peak of the standard card (JCPDS: 88-0657) shows that the nickel cobalt lithium manganate ternary positive electrode active material is used, the dissolved metal ion content is detected by adopting a process of aqua regia dissolution-inductive coupling plasma spectroscopy (ICP), and the chemical formula of the material is Li 21.4 Ni 1.5 Co 7.6 MnO 4.5 . As can be seen from the Scanning Electron Microscope (SEM) picture of FIG. 2 (b), the microscopic morphology of the material including irregularly shaped particles (0.1-12 μm) and spherical particles (1-5 μm) formed by aggregation of nanoparticles was consistent with the microscopic morphology of common lithium cobaltate and lithium nickel cobalt manganate, respectively, and the results of the energy spectrometer (EDS) of FIG. 2 (b) also confirmed that the raw material should be mixed lithium cobaltate and lithium nickel cobalt manganate to obtain the positive electrode active material powderAnd (4) grinding.
Example 1 (scheme FIG. 3)
(1) Mixing and stirring ethylene glycol and oxalic acid dihydrate in a molar ratio of 3:1 for 10min under the condition of 50 ℃ water bath to obtain a clear and transparent deep eutectic solvent;
(2) Mixing the deep eutectic solvent obtained in the step (1) with nickel cobalt lithium manganate powder according to a solid-to-liquid ratio of 4g/L, stirring for 12 hours under a water bath condition of 90 ℃, and then carrying out solid-liquid separation to obtain a leaching solution and a solid-phase product;
(3) Washing the solid phase product with deionized water and absolute ethyl alcohol respectively for 2 times, then drying the solid phase product in an oven at the temperature of 80 ℃ for 12 hours, and grinding to obtain nickel-cobalt-manganese dihydrate oxalate powder.
Example 2 (scheme see FIG. 3)
(1) Under the condition of 60 ℃ water bath, mixing and stirring ethylene glycol and oxalic acid dihydrate in a molar ratio of 3:1 for 30min to obtain a clear and transparent deep eutectic solvent;
(2) Mixing the deep eutectic solvent obtained in the step (1) and nickel cobalt lithium manganate powder according to a solid-to-liquid ratio of 12g/L, stirring for 16 hours under a water bath condition of 95 ℃, and performing solid-liquid separation to obtain a leaching solution and a solid-phase product;
(3) Washing the solid phase product 3 times by respectively using deionized water and absolute ethyl alcohol, then drying the solid phase product in an oven at 90 ℃ for 8h, and grinding to obtain the dihydrate oxalate powder of nickel, cobalt and manganese.
Example 3 (scheme FIG. 3)
(1) Under the condition of 60 ℃ water bath, mixing and stirring ethylene glycol and oxalic acid dihydrate in a molar ratio of 5:1 for 15min to obtain a clear and transparent deep eutectic solvent;
(2) Mixing the deep eutectic solvent obtained in the step (1) with nickel cobalt lithium manganate powder according to a solid-to-liquid ratio of 4g/L, stirring for 24 hours under a water bath condition of 85 ℃, and then carrying out solid-liquid separation to obtain a leaching solution and a solid-phase product;
(3) Washing the solid phase product 3 times by respectively using deionized water and absolute ethyl alcohol, then drying the solid phase product in an oven at 90 ℃ for 12h, and grinding to obtain the dihydrate oxalate powder of nickel, cobalt and manganese.
Detailed results of the experiment
By detecting the content of Li, ni, co and Mn in the leaching solution and calculating, the result shows that the leaching efficiency of lithium is over 99 percent, the obtained leaching solution only contains lithium, and over 99 percent of nickel, cobalt and manganese are left in the solid-phase product. As is clear from FIG. 4, the diffraction peaks in the XRD pattern of the solid phase product are in contact with monoclinic NiC 2 O 4 ·2H 2 O (JCPDS: 25-0581), orthorhombic CoC 2 O 4 ·2H 2 O (JCPDS: 25-0250) and monoclinic MnC 2 O 4 ·2H 2 The O (JCPDS: 25-0544) standard card is consistent, which indicates that the solid phase product is nickel cobalt manganese dihydrate oxalate precipitate, and SEM pictures show that the solid phase product is a nano rod-shaped structure with the particle size of 0.1-10 μm. Therefore, aiming at the nickel cobalt lithium manganate positive active material in the waste lithium ion battery, the invention adopts the bifunctional deep eutectic solvent (the solution formed by the ethylene glycol and the oxalic acid dihydrate) as the leaching system, so as to realize the high-efficiency separation and recovery of lithium and nickel cobalt manganese by one step and obtain the leaching solution only containing lithium and the oxalate dihydrate precipitate of nickel cobalt manganese.
Claims (5)
1. A method for recycling the active material of the anode of a waste lithium ion battery is characterized in that a bifunctional deep eutectic solvent is used for separating and recycling lithium, nickel, cobalt and manganese, and the specific process steps are as follows:
(1) Under the condition of water bath at 40-60 ℃, mixing and stirring ethylene glycol and oxalic acid dihydrate with the molar ratio of 2:1-5:1 for 5-30min to obtain a clear and transparent bifunctional deep eutectic solvent;
(2) Mixing the bifunctional deep eutectic solvent obtained in the step (1) and the anode active material powder according to a solid-to-liquid ratio of 4-16 g/L, stirring for 12-24h under a water bath condition of 85-95 ℃, and then carrying out solid-liquid separation to obtain a leaching solution and a solid-phase product;
washing the solid phase product 1-3 times by respectively using deionized water and absolute ethyl alcohol, then putting the solid phase product in an oven at 60-100 ℃ to dry 6-12h, and grinding to obtain the dihydrate oxalate powder of nickel, cobalt and manganese.
2. The method according to claim 1, wherein the positive active material powder used in step (2) is derived from samsung waste lithium ion battery, and is nickel cobalt lithium manganate obtained by applying a pretreatment process to lithium batteries, wherein the pretreatment process comprises: discharging saturated sodium chloride solution, manually disassembling the anode, dissolving aluminum foil by using sodium hydroxide solution, and calcining at high temperature to remove binder impurities.
3. The method for recycling the positive active material of the waste lithium ion battery according to claim 1, wherein the glycol in the leaching system used in the step (2) is a solvent, and the oxalic acid dihydrate is a reducing agent and a complexing agent, and no additional water, reducing agent and complexing agent are required.
4. The method for recycling the positive active material of the discarded lithium ion battery according to claim 1, wherein the leaching efficiency of lithium in the step (2) is more than 99%, and the resulting leaching solution contains only lithium.
5. The method for recycling the waste lithium ion battery anode active material according to claim 1, wherein the solid phase product obtained in the step (3) is a precipitation of oxalate dihydrate of nickel, cobalt and manganese with a nanorod structure, and the recycling efficiency of nickel, cobalt and manganese is more than 99%.
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| CN110396600A (en) * | 2019-07-29 | 2019-11-01 | 先进储能材料国家工程研究中心有限责任公司 | The lithium recovery process of waste and old lithium ion battery |
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