Method and system for scalable direct recycling of battery waste

Abstract

Embodiments described herein relate to methods of recycling battery waste. In some aspects, the method may include applying a first heat treatment to the battery waste material at a temperature of about 100 DEG C to about 700 DEG C, the first heat treatment decomposing at least about 80 wt% of the binder, separating the electrode material from the current collector, and applying a second heat treatment to the electrode material at a temperature of about 400 DEG C to about 1,200 DEG C to produce a regenerated electrode material, the regenerated electrode material having at least about 80 wt% of the binder. The second heat treatment decomposes at least 90 wt% of the remaining binder in the electrode material to produce a regenerated electrode material. In some embodiments, the method may include applying a surface treatment to the electrode material to remove a surface coating and / or surface impurities from the electrode material. In some embodiments, the surface treatment may include applying a solvent to the electrode material.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims the benefit of U.S. Provisional Application No. 63 / 340,612, entitled “Methods and Systems for Scalable Direct Recycling of Battery Waste,” filed on May 11, 2022, the disclosure of which is incorporated herein by reference in its entirety. Technical Field

[0003] The present disclosure relates generally to systems, apparatus, and methods for recycling energy storage devices, and more particularly to recycling of lithium-ion batteries and their components, including waste generated during manufacture, use, and disposal. Background Art

[0004] Lithium-ion batteries have high power and energy density, long cycle life, high potential, and low self-discharge rate. Therefore, they are often regarded as the most promising short-term energy storage method and are widely used in consumer electronics, electric vehicles, and grid energy storage. However, lithium-ion batteries also have several drawbacks, including limited supply of battery materials, environmental hazards during production or at the end of life, and high manufacturing costs. Summary of the invention

[0005] Embodiments described herein relate to methods for recycling battery waste. In some aspects, the method may include applying a first heat treatment to the battery waste at a temperature of about 100°C to about 700°C, the first heat treatment decomposing at least about 80% by weight of the binder, separating the electrode material from the current collector, and applying a second heat treatment to the electrode material at a temperature of about 400°C to about 1,200°C to produce a regenerated electrode material, the second heat treatment decomposing at least 90% by weight of the binder remaining in the electrode material to produce a regenerated electrode material. In some embodiments, the method may include applying a surface treatment to the electrode material to remove surface coatings and / or surface impurities from the electrode material. In some embodiments, the surface treatment may include applying a solvent to the electrode material. In some embodiments, the solvent may include citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, and / or chemical derivatives thereof.

[0006] In some embodiments, a system for directly recycling battery waste is described. The system can include one or more of the following operations (including one or more of the same operations): a thermal treatment subsystem, a separation subsystem, a surface treatment subsystem, a relithiation subsystem, a washing subsystem, a chemical purification subsystem, and a flotation subsystem. In some embodiments, the system can produce commercial grade electrode materials (such as cathode and anode materials) for reuse. BRIEF DESCRIPTION OF THE DRAWINGS

[0007] Figure 1 is a flow chart of a method for recycling battery waste according to one embodiment.

[0008] Figure 2A-2B is a diagram of a muffle furnace for thermally treating battery waste, according to one embodiment.

[0009] Figure 3A-3B is an illustration of a tube for thermally treating battery waste, according to one embodiment.

[0010] Figure 4A is a flow chart of a method for processing battery waste according to one embodiment.

[0011] Figure 4B A schematic diagram of a processing plant for treating battery waste is shown according to various embodiments.

[0012] Figure 5A is a flow chart of a method for processing battery waste according to one embodiment.

[0013] Figure 5B A schematic diagram of a processing plant for treating battery waste is shown according to various embodiments.

[0014] Figure 6 is a flow chart of a method for surface treatment of an electrode material according to one embodiment.

[0015] Figure 7 is a flow chart of a method for surface treatment of an electrode material according to one embodiment.

[0016] Figure 8 is a flow chart of a method of producing an electrode material for recycling according to one embodiment.

[0017] Fig. 9 is a decision flow chart of a method for processing electrode materials according to one embodiment.

[0018] Fig.10 is a flow chart of a method for recycling battery waste according to one embodiment.

[0019] Fig.11 The electrochemical performance of lithium titanate (LTO), an electrode material recycled by an embodiment of the present invention, compared to the original commercial electrode material (standard or STD) is shown.

[0020] Fig.12 The electrochemical performance of an electrode material, lithium nickel cobalt manganese oxide (NCM), recycled by an embodiment of the present invention compared to a virgin commercial electrode material (standard or STD) is shown.

[0021] Fig.13 The electrochemical performance of lithium iron phosphate (LFP), an electrode material recycled by an embodiment of the present invention, compared to the original commercial electrode material (standard or STD) is shown.

[0022] Fig.14 X-ray diffraction (XRD) patterns of a standard LFP electrode compared to a recycled LFP electrode and a LFP electrode after a second heat treatment are shown.

[0023] Fig.15 The discharge capacity of a standard LFP electrode over 200 cycles is shown compared to a recycled LFP electrode. DETAILED DESCRIPTION

[0024] Lithium-ion batteries generate large amounts of waste materials during their manufacture, use, and disposal. To address environmental sustainability issues associated with continued lithium-ion battery consumption, effective recycling methods can be used to recover materials for reuse, including reintroducing recycled materials in the manufacture of new lithium-ion batteries. Recycled battery materials can have the advantage of reducing greenhouse gas emissions, energy consumption, and the use of virgin materials in the battery manufacturing process.

[0025] Recycling of batteries can be achieved through at least three methods: pyrometallurgical recycling, hydrometallurgical recycling, and direct recycling. In pyrometallurgical battery recycling, batteries and battery waste are directly smelted to recover valuable metals such as Co, Ni and Cu, usually in alloy form, from the bottom of the furnace. A leaching process is usually performed to separate the recovered metals.

[0026] Smelting can be used to produce lithium cobalt oxides including LiCoO2 (also referred to herein as lithium cobalt oxide or LCO), LiMn2O4 (also referred to herein as lithium manganese oxide or LMO), and LiNi x Mn y Co z Some elements (e.g., Co, Mn, Ni) can be economically recovered from several types of cathode materials including LiFeO2 (where x+y+z=1, also referred to herein as lithium nickel cobalt manganese oxide or NCM). In some embodiments, any of x, y, or z may be zero. However, recycling LiFe t M 1-tA cathode of PO4 (where 0 < 1 < t; M = Mn, Ni, Co, V, or a metal element, or a combination of several metal elements) (LFMP) (also referred to herein as lithium iron phosphate or LFP) is generally not economically advantageous because the value of the metals recovered from LFMP batteries is low. Additionally, lithium and aluminum typically end up as slag due to melting. Extensive and costly processing is usually carried out to separate the metals before they can be used to construct new batteries. Moreover, the smelting process itself typically generates a large amount of exhaust gas, thereby increasing the total cost due to subsequent waste treatment.

[0027] Hydrometallurgical recycling processes separate and / or disassemble battery components prior to further processing. This method is also applicable to recycling nickel metal hydride (Ni-MH) batteries. For lithium-ion batteries, lithium is ultimately recovered as Li2CO3, and other major materials such as Co, Ni, and Al can also be recovered. For Ni-MH batteries, rare earth metals and nickel can be recovered. Although hydrometallurgical recycling does not involve high temperatures and high capacities, this method alters the morphology of the battery cathode material, thereby making the cathode material unsuitable for reuse without further processing. Hydrometallurgical recycling is described in more detail in U.S. Patent No. 8,846,225, titled "Reintroduction of lithium into recycled battery materials" ("the '225 patent"), which is hereby incorporated by reference in its entirety.

[0028] Compared to the two methods described above, direct recycling of batteries can recover valuable cathode materials as well as anode materials, current collectors, binders, and electrolytes. The direct recycling method includes non-destructive recycling methods and can preserve the structure, morphology, and electrochemical properties of valuable materials. Direct recycling can be suitable for recycling entire batteries, individual battery components, combinations of battery components, battery manufacturing waste, or battery disposal waste. An effective direct recycling process can have the flexibility to recycle different battery materials while also maintaining the ability to produce commercially available recycled materials.

[0029] The systems and methods described herein relate to directly recycling batteries and battery waste in an efficient and scalable manner. In this technology, batteries and battery waste are processed through several steps to separate, purify, and / or regenerate one or more recyclable battery components. These processes are designed to be scalable for recycling large quantities of batteries and battery waste.

[0030] Battery waste may include waste or waste products from the battery manufacturing process, which may include any single battery component, any combination of battery components, an entire battery at the end of its service life, a defective battery, a damaged battery, or any other form or combination thereof. In some embodiments, battery waste may include one or more cathode sheets comprising cathode material and cathode current collector (typically aluminum or similar materials). In some embodiments, the cathode sheet may additionally include a binder, a conductive additive such as carbon, an electrolyte, a lithium salt, and / or other functional additives. In some embodiments, battery waste may include one or more anode sheets comprising anode material and anode current collector (typically copper or similar materials). In some embodiments, the anode sheet may additionally include a binder, a conductive additive such as carbon, an electrolyte, a lithium salt, and / or other functional additives. In some embodiments, battery waste includes separators, packaging materials, electrical leads, and / or other battery components. In some embodiments, battery waste may be cut, shredded, ground, mixed, or otherwise combined. In some embodiments, battery waste is black matter, which may include shredded, ground, mixed, or otherwise combined battery waste, in which one or more components are partially or completely removed (e.g., the battery housing is removed). In this article, anode and / or cathode may be referred to as electrode. Anode may include anode material and anode current collector. Cathode may include cathode material and cathode current collector. Anode material and cathode material may be more generally referred to as electrode material.

[0031] In some embodiments, the electrode material may include common lithium-ion battery compositions such as LCO, LMO, NCM, lithium nickel cobalt aluminum oxide (LiNi x Co y Al z O2, where x+y+z=1), LiNi a Mn b Co c A d O2 (where a+b+c+d=1, A=Al, Zr, or Mg), LFP, LFMP, graphite, lithium titanate (Li4Ti5O 12 or LTO), or other common compositions or derivatives, or combinations thereof.

[0032] The recycling methods described herein may include one or more combinations of the following operations (including combinations of one or more of the same operations): thermal treatment operations, separation operations, surface treatment operations, relithiation operations, washing operations, chemical purification processes, and flotation processes. In some embodiments, the recycling methods produce commercial grade cathode and anode materials. In some embodiments, the recycling methods produce metal waste products, such as copper, aluminum, steel, or mixtures thereof. In some embodiments, organic materials such as carbon, electrolytes, and separators can be separated and recovered.

[0033] Figure 1 1 is a flow chart of a method 10 for recycling battery waste according to one embodiment. Battery waste may include electrode materials connected to current collectors. Electrode materials may include active materials and binders. In some embodiments, electrode materials may include conductive materials. In some embodiments, anodes and cathodes may be processed separately via method 10. In some embodiments, anodes and cathodes may be processed together via method 10. In some embodiments, input battery waste may include cathode and / or anode sheets (or mixtures thereof) comprising cathodes or anodes (in some cases, which may be mixed with binders and / or additives such as conductive carbon) and current collectors. In some embodiments, current collectors may include (composed of) aluminum and / or copper. In some embodiments, battery waste may include other components such as separators, electrolytes, lithium salts, and / or packaging. In some embodiments, method 10 may be applicable to processing battery waste containing cathodes, anodes, or mixtures thereof, or batteries with or without electrolytes supplied as input for recycling. In some embodiments, battery waste is one or more fully or partially assembled batteries (with or without electrolytes). In some embodiments, the battery waste may first be disassembled, processed into multiple parts, shredded, cut, or other processes that expose components of the battery waste for further processing. In some embodiments, this initial processing of the battery waste may include a discharge step to remove some or all of the stored energy remaining in the battery waste. In some embodiments, the discharge step may be performed using electronic discharge (e.g., resistive discharge, electronic conductive slurry or liquid discharge) and / or ionic discharge (e.g., discharge in an ion conductive solution).

[0034] As shown, method 10 optionally includes washing the electrode material to remove the binder at step 11, and removing impurities from the electrode material at step 12. Method 10 includes applying a heat treatment at step 13 to decompose the electrode material. Method 10 optionally includes treating the exhaust gas from the first heat treatment at step 14. Method 10 also includes separating the electrode material from the current collector at step 15. Method 10 optionally includes floating the electrode material to separate residual impurities from the electrode material at step 16, and applying a surface treatment to the electrode material at step 17. Method 10 also includes applying a second heat treatment at step 18 to purify the recovered electrode material. Method 10 optionally includes treating the exhaust gas from the second heat treatment.

[0035] Step 11 is optional and includes washing the electrode material to remove at least a portion of the binder. The washing utilizes a solvent to dissolve and remove at least a portion of the binder. During the washing process, most or all of the binder, current collector, and other large particle battery components are separated from the electrode powder (and any residual materials). In some embodiments, the electrode material includes a water-based binder (i.e., soluble in aqueous solution), and the washing operation can utilize an aqueous solvent (e.g., water or an alkaline solution, such as a pH of no more than about 14, no more than about 13, no more than about 12, no more than about 11, no more than about 10, no more than about 9, no more than about 8, or no more than about 7.5 including LiOH, NaOH, KOH). In some embodiments, the electrode material may include a non-aqueous binder (i.e., insoluble in aqueous solution), and the washing operation may utilize an organic or non-polar solvent. In some embodiments, the non-polar solvent may include N-methyl-2-pyrrolidone (NMP), dimethylformamide (DMF), dimethylacetamide (DMAc or DMA), dihydro-levorotatory glucosone (cyrene), or their derivatives, or any combination thereof. In some embodiments, during washing, the electrode material may be at least partially separated from the current collector. In other words, step 11 may occur at least partially simultaneously with step 15. In some embodiments, after the washing operation, other battery components such as residual carbon and other organic matter, residual adhesive, smaller current collector particles, or any other components or combinations thereof may exist with the electrode material.

[0036] In some embodiments, washing can be performed in a controlled gas environment. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can be reducing. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. In some embodiments, the gas environment can include an oxidizing environment. An oxidizing environment can help remove organic compounds. In some embodiments, during washing, air or other aforementioned gases flow along the battery waste or flow through the battery waste. In some embodiments, during washing, no gas flows along the battery waste or flows through the battery waste.

[0037] In some embodiments, gaseous environment can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , including all values ​​and scopes therebetween. In some embodiments, gaseous environment can comprise the oxygen that improves the amount. In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0038] Step 12 is optional and includes removing impurities from the electrode material. In some embodiments, step 12 may include removing some, most, or all of the residual metal fragments, such as fragments (e.g., Cu and / or Al) derived from the current collector. In some embodiments, step 12 may include modifying the surface of the electrode powder to enable easier or effective relithiation and / or regeneration. In some embodiments, step 12 may be performed before the heat treatment step (e.g., step 13) to be able to remove impurities such as Cu that cannot be removed after the heat treatment step. In this case, the heat treatment operation may oxidize these components and make them not easily removed by the purification operation. In some embodiments, step 12 may include using a weak acid or base as a solvent. In some embodiments, step 12 may include using citric acid, acetic acid, oxalic acid, or similar acids. In some embodiments, the purification operation uses ammonia or an ammonia-based solution or a similar solution. In some embodiments, step 12 may include removing residual copper and / or residual aluminum from the electrode material. Step 12 may include dissolving and removing impurities from the electrode material collected from the washing operation of step 11. In some embodiments, step 12 may include utilizing a solvent to dissolve and remove impurities. In some embodiments, step 12 may utilize an alkaline solution (eg, a solution containing LiOH, NaOH, and / or KOH).

[0039] In some embodiments, mechanical stirring, mixing techniques, and / or heating may be included to remove impurities from the electrode material. In some embodiments, during step 12, copper and / or aluminum fragments from the current collector are removed. In some embodiments, an ammonia-based solution may be used to remove impurities such as copper from the electrode material. Ammonia or ammonia-based compounds (such as ammonium chloride or ammonium hydroxide) may react with copper and dissolve copper, thereby removing copper as an impurity from the electrode material. In some embodiments, the purification operation may utilize a weakly acidic solution such as acetic acid, citric acid, oxalic acid (or other similar acids) to remove impurities, particularly metal or metal oxide impurities. In some embodiments, the purification operation may utilize other acidic solutions such as nitric acid, sulfuric acid and / or hydrochloric acid (or other similar acids) to remove impurities, particularly metal or metal oxide impurities. In many cases, the purification operation may be carefully designed so as not to affect the integrity of the electrode material.

[0040] In some embodiments, the solution for removing impurities from the electrode material can have a pH of at least about 0, at least about 0.5, at least about 1, at least about 1.5, at least about 2, at least about 2.5, at least about 3, or at least about 3.5. In some embodiments, the solution for removing impurities from the electrode material can have a pH of no more than about 4, no more than about 3.5, no more than about 3, no more than about 2.5, no more than about 2, no more than about 1.5, no more than about 1, or no more than about 0.5. Combinations of the above-mentioned pH values ​​are also possible (e.g., at least about 0 and no more than about 4 or at least about 1 and no more than about 3). In some embodiments, the solution for removing impurities from the electrode material can have a pH of about 0, about 0.5, about 1, about 1.5, about 2, about 2.5, about 3, about 3.5, or about 4.

[0041] In some embodiments, the solution used to remove impurities from the electrode material can have a pH of at least about 13, at least about 13.1, at least about 13.2, at least about 13.3, at least about 13.4, at least about 13.5, at least about 13.6, at least about 13.7, at least about 13.8, at least about 13.9, at least about 14, at least about 14.1, at least about 14.2, at least about 14.3, at least about 14.4, at least about 14.5, at least about 14.6, at least about 14.7, at least about 14.8, or at least about 14.9. In some embodiments, the solution used to remove impurities from the electrode material can have a pH of no more than about 15, no more than about 14.9, no more than about 14.8, no more than about 14.7, no more than about 14.6, no more than about 14.5, no more than about 14.4, no more than about 14.3, no more than about 14.2, no more than about 14.1, no more than about 14, no more than about 13.9, no more than about 13.8, no more than about 13.7, no more than about 13.6, no more than about 13.5, no more than about 13.4, no more than about 13.3, no more than about 13.2, or no more than about 13.1. Combinations of the above-mentioned pH values ​​are also possible (e.g., at least about 13 and no more than about 15 or at least about 13.5 and no more than about 14.5), including all values ​​and ranges therebetween. In some embodiments, the solution used to remove impurities from the electrode material can have a pH of about 13, about 13.1, about 13.2, about 13.3, about 13.4, about 13.5, about 13.6, about 13.7, about 13.8, about 13.9, about 14, about 14.1, about 14.2, about 14.3, about 14.4, about 14.5, about 14.6, about 14.7, about 14.8, about 14.9, or about 15.

[0042] In some embodiments, a purification operation can have a duration of at least about 30 seconds, at least about 1 minute, at least about 2 minutes, at least about 3 minutes, at least about 4 minutes, at least about 5 minutes, at least about 6 minutes, at least about 7 minutes, at least about 8 minutes, at least about 9 minutes, at least about 10 minutes, at least about 15 minutes, at least about 20 minutes, at least about 25 minutes, at least about 30 minutes, at least about 35 minutes, at least about 40 minutes, at least about 45 minutes, at least about 50 minutes, at least about 55 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 12 hours, at least about 14 hours, at least about 16 hours, at least about 18 hours, at least about 20 hours, at least about 25 hours, or at least about 30 hours. In some embodiments, the purification operation can have a duration of no more than about 31 hours, no more than about 26 hours, no more than about 21 hours, no more than about 19 hours, no more than about 17 hours, no more than about 15 hours, no more than about 13 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, no more than about 2 hours, no more than about 1 hour, no more than about 55 minutes, no more than about 50 minutes, no more than about 45 minutes, no more than about 40 minutes, no more than about 35 minutes, no more than about 30 minutes, no more than about 25 minutes, no more than about 20 minutes, no more than about 15 minutes, no more than about 10 minutes, no more than about 9 minutes, no more than about 8 minutes, no more than about 7 minutes, no more than about 6 minutes, no more than about 5 minutes, no more than about 4 minutes, no more than about 3 minutes, no more than about 2 minutes, or no more than about 1 minute. The combination of the above-mentioned durations is also possible (e.g., at least about 30 seconds and no more than about 31 hours or at least about 2 minutes and no more than about 4 minutes), including all values ​​and ranges therebetween. In some embodiments, the purification operation can have a duration of about 30 seconds, about 1 minute, about 2 minutes, about 3 minutes, about 4 minutes, about 5 minutes, about 6 minutes, about 7 minutes, about 8 minutes, about 9 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 12 hours, about 14 hours, about 16 hours, about 18 hours, about 20 hours, about 25 hours, or about 30 hours.

[0043] In some embodiments, the purification operation can be performed at a temperature of at least about 20°C, at least about 30°C, at least about 40°C, at least about 50°C, at least about 60°C, at least about 70°C, at least about 80°C, or at least about 90°C. In some embodiments, the purification operation can be performed at a temperature of no more than about 100°C, no more than about 90°C, no more than about 80°C, no more than about 70°C, no more than about 60°C, no more than about 50°C, no more than about 40°C, or no more than about 30°C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 20°C and no more than about 100°C or at least about 40°C and no more than about 60°C), including all values ​​and ranges therebetween. In some embodiments, the purification operation can be performed at a temperature of about 20°C, about 30°C, about 40°C, about 50°C, about 60°C, about 70°C, about 80°C, about 90°C, or about 100°C.

[0044] The purification operation can modify and optimize the surface morphology of the electrode material by removing unfavorable surface coatings or impurities (such as inactive secondary phases) from the electrode material or changing the surface structure or surface chemistry of the electrode material. These impurities can be formed in a variety of situations, including but not limited to battery manufacturing, exposure to different atmospheres or humidity, or during previous operations during the recycling process. The modification and optimization of the surface morphology of the electrode material during the purification operation can improve the performance of the recovered or regenerated electrode material. The modification and optimization of the surface morphology of the electrode material during the purification operation can also contribute to easier relithiation during subsequent heat treatment operations. The modified surface can allow lithium to be more easily introduced into the electrode structure from the lithium source.

[0045] In some embodiments, purification can be performed in a controlled gas environment. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar, or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can be reducing. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. In some embodiments, the gas environment can include an oxidizing environment. The oxidizing environment can help remove organic compounds. In some embodiments, during purification, air or other aforementioned gases flow along the battery waste or flow through the battery waste. In some embodiments, during purification, no gas flows along the battery waste or flows through the battery waste. In some embodiments, surface treatment can be performed under increased gas pressure. In some embodiments, surface treatment can be performed under reduced gas pressure.

[0046] In some embodiments, gaseous environment can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , including all values ​​and scopes therebetween. In some embodiments, gaseous environment can comprise the oxygen that improves the amount. In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0047] Step 13 includes applying a first heat treatment to decompose the electrode material. The first heat treatment can remove or decompose some or all of several components of the battery waste (including but not limited to adhesives, conductive additives such as carbon, electrolytes and / or lithium salts). The first heat treatment operation is operated at a temperature that largely or completely retains the structure of the electrode material or current collector. Some current collector materials may become oxidized during the first heat treatment. For example, copper may form copper oxide during the first heat treatment. In some embodiments, the first heat treatment may be performed in a heating chamber (e.g., an oven or a furnace). In some embodiments, the first heat treatment operation may also convert hydrophilic organic materials (such as carbon-based anode materials or conductive organic additives) into hydrophobic organic materials, which may be beneficial for subsequent flotation operations (i.e., step 16). In some embodiments, the heat treatment of step 13 may be performed before removing impurities from the electrode material in step 12. In some embodiments, the heat treatment of step 13 may be performed after removing impurities from the electrode material in step 12.

[0048] In some embodiments, the first thermal treatment may be performed at a temperature of at least about 100° C., at least about 150° C., at least about 200° C., at least about 250° C., at least about 300° C., at least about 350° C., at least about 400° C., at least about 450° C., at least about 500° C., at least about 550° C., at least about 600° C., or at least about 650° C. In some embodiments, the first thermal treatment may be performed at a temperature of no more than about 700° C., no more than about 650° C., no more than about 600° C., no more than about 550° C., no more than about 500° C., no more than about 450° C., no more than about 400° C., no more than about 350° C., no more than about 300° C., or no more than about 250° C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 200° C. and no more than about 700° C. or at least about 400° C. and no more than about 600° C.), including all values ​​and ranges therebetween. In some embodiments, the first heat treatment may be performed at a temperature of about 100°C, about 150°C, about 200°C, about 250°C, about 300°C, about 350°C, about 400°C, about 450°C, about 500°C, about 550°C, about 600°C, about 650°C, or about 700°C.

[0049] In some embodiments, a first heat treatment is performed on battery waste containing polyvinylidene fluoride (PVDF). Isothermal degradation of the PVDF binder begins at about 300-400°C. The heat treatment can be performed above 400°C to ensure thermal degradation of the PVDF. The PVDF binder thermally decomposes at such temperatures and gasifies with any electrolyte solvent residues (e.g., EC, DMC, EMC, DEC, and PC) present. Such heat treatment conditions can effectively burn off the PVDF binder while largely or completely retaining the structural and compositional integrity of other battery components (such as electrode materials or current collector materials).

[0050] In some embodiments, the binder is a water-soluble binder. In some embodiments, the binder is styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA) or a derivative thereof, or a mixture thereof, and is thermally decomposed during the first heat treatment above the thermal decomposition temperature of the binder.

[0051] In some embodiments, the first thermal treatment can be performed in a controlled gas environment. Various gas environments can react with different battery components in different ways, resulting in different outputs of the heating operation. In some embodiments, the gas environment is inert. In some embodiments, the gas environment can include N2, Ar, or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment is a reducing environment. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. A reducing or inert environment can prevent oxidation of certain battery components (such as copper current collectors). In some embodiments, the gas environment can include an oxidizing environment. An oxidizing environment can help remove organic compounds. In some embodiments, air or other aforementioned gases flow through the heating chamber. In some embodiments, no gas flows through the heating chamber.

[0052] In some embodiments, the environment of heating chamber can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , comprise all values ​​and scopes therebetween.In some embodiments, gaseous environment can comprise the oxygen of raising amount.In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0053] In some embodiments, the first thermal treatment can have a duration of at least about 30 seconds, at least about 1 minute, at least about 2 minutes, at least about 3 minutes, at least about 4 minutes, at least about 5 minutes, at least about 6 minutes, at least about 7 minutes, at least about 8 minutes, at least about 9 minutes, at least about 10 minutes, at least about 15 minutes, at least about 20 minutes, at least about 25 minutes, at least about 30 minutes, at least about 35 minutes, at least about 40 minutes, at least about 45 minutes, at least about 50 minutes, at least about 55 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 12 hours, at least about 14 hours, at least about 16 hours, at least about 18 hours, or at least about 20 hours. In some embodiments, the first thermal treatment can have a duration of no more than about 21 hours, no more than about 19 hours, no more than about 17 hours, no more than about 15 hours, no more than about 13 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, no more than about 2 hours, no more than about 1 hour, no more than about 55 minutes, no more than about 50 minutes, no more than about 45 minutes, no more than about 40 minutes, no more than about 35 minutes, no more than about 30 minutes, no more than about 25 minutes, no more than about 20 minutes, no more than about 15 minutes, no more than about 10 minutes, no more than about 9 minutes, no more than about 8 minutes, no more than about 7 minutes, no more than about 6 minutes, no more than about 5 minutes, no more than about 4 minutes, no more than about 3 minutes, no more than about 2 minutes, or no more than about 1 minute. The combination of the above-mentioned duration is also possible (for example, at least about 30 seconds and be no more than about 21 hours or at least about 2 minutes and be no more than about 4 minutes), comprises all values ​​and scopes between them.In some embodiments, the first thermal treatment can have the duration of about 30 seconds, about 1 minute, about 2 minutes, about 3 minutes, about 4 minutes, about 5 minutes, about 6 minutes, about 7 minutes, about 8 minutes, about 9 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 12 hours, about 14 hours, about 16 hours, about 18 hours, about 20 hours or about 21 hours.

[0054] In some embodiments, during the first thermal treatment in step 13, at least about 80 wt %, at least about 81 wt %, at least about 82 wt %, at least about 83 wt %, at least about 84 wt %, at least about 85 wt %, at least about 86 wt %, at least about 87 wt %, at least about 88 wt %, at least about 89 wt %, at least about 90 wt %, at least about 91 wt %, at least about 92 wt %, at least about 93 wt %, at least about 94 wt %, at least about 95 wt %, at least about 96 wt %, at least about 97 wt %, at least about 98 wt %, or at least about 99 wt % of the binder can be removed from the battery waste. In some embodiments, no more than about 100 wt %, no more than about 99 wt %, no more than about 98 wt %, no more than about 97 wt %, no more than about 96 wt %, no more than about 95 wt %, no more than about 94 wt %, no more than about 93 wt %, no more than about 92 wt %, no more than about 91 wt %, or no more than about 90 wt %, no more than about 89 wt %, no more than about 88 wt %, no more than about 87 wt %, no more than about 86 wt %, no more than about 85 wt %, no more than about 84 wt %, no more than about 83 wt %, no more than about 82 wt %, or no more than about 81 wt % of the binder may be removed from the battery waste during the first thermal treatment of step 13. Combinations of the above-mentioned weight percentages are also possible (e.g., at least about 80 wt % and no more than about 100 wt % or at least about 85 wt % and no more than about 95 wt %), including all values ​​and ranges therebetween. In some embodiments, during the first thermal treatment in step 13, about 80 weight percent, about 81 weight percent, about 82 weight percent, about 83 weight percent, about 84 weight percent, about 85 weight percent, about 86 weight percent, about 87 weight percent, about 88 weight percent, about 89 weight percent, about 90 weight percent, about 91 weight percent, about 92 weight percent, about 93 weight percent, about 94 weight percent, about 95 weight percent, about 96 weight percent, about 97 weight percent, about 98 weight percent, about 99 weight percent, or about 100 weight percent of the binder can be removed from the battery waste.

[0055] Step 14 is optional and includes treating the waste gas from the first thermal treatment. In some embodiments, the treatment may include purifying the waste gas (e.g., via a purification operation). In some embodiments, the purification may be via scrubbing (i.e., using a gas scrubber). In some embodiments, the waste gas may be purified via a scrubber. After the gas treatment, the purified gas may be released into the atmosphere or captured.

[0056] In some embodiments, step 14 can be used to meet specific environmental standards or remove a certain amount of harmful or undesirable materials discharged from the thermal treatment operation. In some embodiments, step 14 can include a gas scrubbing operation. In some embodiments, the purification operation removes acidic components from the exhaust gas. In some embodiments, the purification operation removes organic compounds, including volatile organic compounds (VOC), fluorocarbons (fluorocarbons), or hydrofluorocarbons. In some embodiments, the purification operation utilizes a thermal oxidizer to remove VOC.

[0057] Step 15 includes separating the electrode material from the current collector. During step 15, the battery waste can be separated into one or more components or groups of components. In some embodiments, the separation is performed by a particle size separation method (such as screening) by utilizing the particle size difference between the electrode material and the current collector. In some embodiments, the current collector can be divided into smaller pieces before step 15. In some embodiments, the separation of the electrode material and the current collector can be via a physical method. In some embodiments, the physical method can include vibration, ultrasonic treatment, liquid washing / rinsing, gas injection, or any combination thereof. In some embodiments, the current collector and the electrode material can be collected separately. In some embodiments, the separated electrode material can include other components such as residual organic matter (e.g., carbon or carbon compound) or current collector (e.g., aluminum or copper). In some embodiments, the separated electrode material can contain a small amount of other components such as residual organic matter (e.g., carbon or carbon compound) or current collector (e.g., aluminum or copper). In some embodiments, the electrode material (together with any additives mixed with the electrode material) and the current collector (or other battery components of larger particles) can be physically separated from each other and collected separately. Removing the binder from the electrode in the previous operation can facilitate the effective separation of the electrode material and the current collector.

[0058] Step 16 is optional, and includes flotation of the electrode material to separate residual impurities. During step 16, froth flotation is used to separate residual impurities from the electrode material based on hydrophobicity. In some embodiments, a mixture of cathode and anode materials (if the electrode material contains both) can be separated via a flotation operation. Flotation separation includes a solvent (e.g., polar solvent, such as water) mixed with a reinforcing agent (e.g., kerosene) and a foaming agent (e.g., long-chain alcohol, 4-methyl-2-pentanol, pine oil) that promotes the hydrophobicity of other materials. The reinforcing agent preferentially combines with the hydrophobic component. The solvent is aerated to produce a foam mainly comprising reinforcing agent, foaming agent and hydrophobic components. The foam can be separated from the solution via scraping or any other surface collection method. The hydrophilic component is then collected separately from the solution. In these cases, the cathode material has a hydrophobicity level different from some other components. For example, cathode materials such as LiCoO2 tend to be hydrophilic, while some anode materials such as graphite tend to be hydrophobic. Therefore, the anode material can be removed from the foam, and the cathode material can be collected from the solution below the foam. In some embodiments, other additives such as pH adjusters (e.g., sodium carbonate, sodium hydroxide, lithium carbonate, and lithium hydroxide), deflocculating agents, and inhibitors (for increasing the hydrophilicity of specific compounds, such as lime, sodium cyanide, and dextrin) may be used to further facilitate separation. Additional descriptions of froth flotation processes can be found in U.S. Patent No. 11,631,909, filed on November 26, 2019, and entitled “Methods and Systems for Scalable Direct Recycling of Batteries” (“the '909 patent”), the disclosure of which is incorporated herein by reference in its entirety.

[0059] Step 17 is optional and includes applying a surface treatment to the electrode material. The surface treatment can modify and optimize the surface morphology of the electrode material by removing unfavorable surface coatings or impurities (such as inactive secondary phases) from the electrode material or changing the surface structure or surface chemistry of the electrode material. These impurities can be formed in a variety of situations, including but not limited to battery manufacturing, exposure to different atmospheres or humidity, or during previous operations during the recycling process. The modification and optimization of the surface morphology of the electrode material during the surface treatment operation can improve the performance of the electrode material recovered or regenerated. The modification and optimization of the surface morphology of the electrode material during the surface treatment operation can also contribute to easier relithiation during subsequent heat treatment operations. The modified surface can allow lithium to be more easily introduced into the electrode structure from a lithium source. In some embodiments, the surface treatment can include adding a weak acid or a weak base to the electrode material. In some embodiments, the surface treatment can include adding an acid or a base to the electrode material. The acid can include acetic acid, citric acid, oxalic acid, malic acid, ascorbic acid, or any combination thereof. The base can include ammonia, LiOH, NaOH, KOH, or any combination thereof.

[0060] In some embodiments, applying the surface treatment to the electrode material can have a duration of at least about 30 seconds, at least about 1 minute, at least about 2 minutes, at least about 3 minutes, at least about 4 minutes, at least about 5 minutes, at least about 6 minutes, at least about 7 minutes, at least about 8 minutes, at least about 9 minutes, at least about 10 minutes, at least about 15 minutes, at least about 20 minutes, at least about 25 minutes, at least about 30 minutes, at least about 35 minutes, at least about 40 minutes, at least about 45 minutes, at least about 50 minutes, at least about 55 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 12 hours, at least about 14 hours, at least about 16 hours, at least about 18 hours, at least about 20 hours, at least about 25 hours, or at least about 30 hours. In some embodiments, applying a surface treatment to an electrode material can have a duration of no more than about 31 hours, no more than about 26 hours, no more than about 21 hours, no more than about 19 hours, no more than about 17 hours, no more than about 15 hours, no more than about 13 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, no more than about 2 hours, no more than about 1 hour, no more than about 55 minutes, no more than about 50 minutes, no more than about 45 minutes, no more than about 40 minutes, no more than about 35 minutes, no more than about 30 minutes, no more than about 25 minutes, no more than about 20 minutes, no more than about 15 minutes, no more than about 10 minutes, no more than about 9 minutes, no more than about 8 minutes, no more than about 7 minutes, no more than about 6 minutes, no more than about 5 minutes, no more than about 4 minutes, no more than about 3 minutes, no more than about 2 minutes, or no more than about 1 minute. The combination of the above-mentioned duration is also possible (for example, at least about 30 seconds and no more than about 31 hours or at least about 2 minutes and no more than about 4 minutes), including all values ​​and ranges therebetween. In some embodiments, applying surface treatment to the electrode material can have a duration of about 30 seconds, about 1 minute, about 2 minutes, about 3 minutes, about 4 minutes, about 5 minutes, about 6 minutes, about 7 minutes, about 8 minutes, about 9 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 12 hours, about 14 hours, about 16 hours, about 18 hours, about 20 hours, about 25 hours or about 30 hours.

[0061] In some embodiments, applying a surface treatment to an electrode material may be performed at a temperature of at least about 20°C, at least about 30°C, at least about 40°C, at least about 50°C, at least about 60°C, at least about 70°C, at least about 80°C, or at least about 90°C. In some embodiments, applying a surface treatment to an electrode material may be performed at a temperature of no more than about 100°C, no more than about 90°C, no more than about 80°C, no more than about 70°C, no more than about 60°C, no more than about 50°C, no more than about 40°C, or no more than about 30°C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 20°C and no more than about 100°C or at least about 40°C and no more than about 60°C), including all values ​​and ranges therebetween. In some embodiments, applying a surface treatment to an electrode material may be performed at a temperature of about 20°C, about 30°C, about 40°C, about 50°C, about 60°C, about 70°C, about 80°C, about 90°C, or about 100°C.

[0062] In some embodiments, the solution used in the surface treatment can have a pH of at least about 5, at least about 6, at least about 7, or at least about 8, at least about 9, at least about 10, or at least about 11. In some embodiments, the solution used to remove impurities from the electrode material can have a pH of no more than about 12, no more than about 11, no more than about 10, no more than about 9, no more than about 8, no more than about 7, or no more than about 6. The combination of the pH values ​​mentioned above is also possible (e.g., at least about 5 and no more than about 12 or at least about 6 and no more than about 8), including all values ​​and ranges therebetween. In some embodiments, the solution can have a pH of about 5, about 6, about 7, about 8, or about 9.

[0063] In some embodiments, the surface treatment can be performed in a controlled gas environment. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar, or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can be reducing. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. In some embodiments, the gas environment can include an oxidizing environment. The oxidizing environment can help remove organic compounds. In some embodiments, during the surface treatment, air or other aforementioned gases flow along the battery waste or flow through the battery waste. In some embodiments, during the surface treatment, no gas flows along the battery waste or flows through the battery waste. In some embodiments, the surface treatment can be performed under increased gas pressure. In some embodiments, the surface treatment can be performed under reduced gas pressure.

[0064] In some embodiments, gaseous environment can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , including all values ​​and scopes therebetween. In some embodiments, gaseous environment can comprise the oxygen that improves the amount. In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0065] In step 18, a second heat treatment step completes the recovery of the electrode material. The second heat treatment can increase the purity of the recovered electrode material. In some embodiments, residual carbon and residual organic compounds can be thermally decomposed and gasified during step 18. In addition, the electrode material can experience lithium loss in a variety of situations, including but not limited to battery manufacturing, exposure to different atmospheres or humidity, or during previous operations during the recycling process. In some embodiments, the second heat treatment operation may include a re-lithiation operation to restore the lithium concentration in the electrode material to a commercially available stoichiometry. In some embodiments, re-lithiation may include uniformly mixing the electrode material with an additional lithium source (e.g., LiOH, Li2CO3) before, during, and / or after the heat treatment. The re-lithiation of the active material can then be completed via solid-state synthesis during the heat treatment. Such synthesis may be in the form of repairing structural damage to the electrode material.

[0066] In some embodiments, the stoichiometric lithium loss of the electrode material before lithiation may be about 0% to about 10%, about 10% to about 20%, about 20% to about 30%, about 30% to about 40%, or about 40% to about 50%. In some embodiments, common elemental quantification or structural tools (such as inductively coupled plasma mass spectrometry or X-ray diffraction) or electrochemical methods (such as open circuit voltage or capacity measurement) are used to quantify the lithium loss of the electrode material before relithiation. In some embodiments, the delithiation operation can be performed without a second heat treatment operation. In some embodiments, before the second heat treatment operation, the electrode material can undergo a grinding step to reduce the particle size of the electrode material or break up agglomerates.

[0067] In some embodiments, step 18 may include a delithiation operation to remove excess lithium from the electrode material. In some embodiments, the delithiation operation may include washing the electrode material in a solvent capable of removing and dissolving excess lithium. In some embodiments, the solvent may include water. In some embodiments, the electrode material may be washed in an aqueous solution.

[0068] In some embodiments, the second heat treatment operation of step 18 can be performed in a controlled gas environment. Different gas environments can react with various battery components in different ways, resulting in different products. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar or any other similar gas. In some embodiments, the gas environment can be a reducing gas environment. Reduction or inert environment can contribute to better performance of specific electrode materials such as LFP. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO.

[0069] In some embodiments, the gaseous environment can be an oxidizing environment.Oxidizing environment can contribute to the better performance of specific electrode materials such as mixed transition metal cathodes (for example, various compositions of lithium nickel cobalt manganese oxide).In some embodiments, the oxidizing environment includes oxygen.In some embodiments, the oxidizing environment can include oxygen with a concentration higher than that of ambient air.In some embodiments, the oxidizing environment can include at least about 25 volume %, at least about 30 volume %, at least about 35 volume %, at least about 40 volume %, at least about 45 volume %, at least about 50 volume %, at least about 55 volume %, at least about 60 volume %, at least about 65 volume %, at least about 70 volume %, at least about 75 volume %, at least about 80 volume %, at least about 85 volume %, at least about 90 volume % or at least about 95 volume % of oxygen.In some embodiments, the oxidizing environment can include pure oxygen.In some embodiments, the oxidizing environment can include at least about 99 volume %, at least about 99.9 volume %, at least about 99.99 volume % or at least about 99.999 volume % of oxygen. In some embodiments, reducing gas, air, and / or oxidizing gas may be flowed through the heating chamber where the second thermal treatment is performed during step 18. In some embodiments, no gas is flowed through the heating chamber.

[0070] The second heat treatment operation can be performed at various temperatures and different time lengths. These parameters can vary depending on the type of material being processed during the heat treatment operation. In some embodiments, the second heat treatment operation is performed at a temperature of at least about 400°C, at least about 500°C, at least about 600°C, at least about 700°C, at least about 800°C, at least about 900°C, at least about 1,000°C, or at least about 1,100°C. In some embodiments, the second heat treatment operation is performed at a temperature of no more than about 1,200°C, no more than about 1,100°C, no more than about 1,000°C, no more than about 900°C, no more than about 800°C, no more than about 700°C, no more than about 600°C, or no more than about 500°C. The combination of the above-mentioned temperatures is also possible (for example, at least about 400°C and no more than about 1,200°C or at least about 600°C and no more than about 900°C), including all values ​​and ranges therebetween. In some embodiments, the second thermal treatment operation may be performed at a temperature of about 400°C, about 500°C, about 600°C, about 700°C, about 800°C, about 900°C, about 1,000°C, about 1,100°C, or about 1,200°C.

[0071] In some embodiments, the second thermal treatment can have a duration of about 1 hour to about 2 hours, about 2 hours to about 3 hours, about 3 hours to about 4 hours, about 4 hours to about 5 hours, about 5 hours to about 7 hours, about 7 hours to about 10 hours, or about 10 hours to about 15 hours. In some embodiments, the second thermal treatment can have a duration of at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, or at least about 14 hours. In some embodiments, the second thermal treatment can have a duration of no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours. The combination of the above-mentioned duration is also possible (for example, at least about 1 hour and no more than about 15 hours or at least about 4 hours and no more than about 10 hours), including all values ​​and scopes therebetween. In some embodiments, the second thermal treatment can have a duration of about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours or about 15 hours.

[0072] In some embodiments, the temperature, duration, and atmosphere of the second heat treatment may depend on the cathode material. For example, an LFP electrode may be regenerated at a temperature of about 450°C to about 800°C for a duration of about 1 hour to about 12 hours. In addition, an NCM electrode may be regenerated at a temperature of about 600°C to about 900°C for a duration of about 3 hours to about 15 hours.

[0073] In some embodiments, the second thermal treatment may include a thermal treatment operation including a relithiation process that may be performed using an excess lithium method. The excess lithium method may reduce or eliminate the need to accurately quantify the lithium deficiency of the electrode material before applying the regeneration method 10. The method may include mixing the lithium-deficient electrode material with a lithium source that exceeds the stoichiometric lithium deficiency of the electrode material. The electrode material mixed with the excess lithium source may then be subjected to a thermal treatment operation. The thermal treatment operation may be performed within one or more temperature ranges mentioned above for the second thermal treatment and may be capable of relithiating the electrode material.

[0074] In some embodiments, the second thermal treatment can result in vaporization of at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt%, at least about 99 wt%, at least about 99.5 wt%, at least about 99.9 wt%, at least about 99.99 wt%, or at least about 99.999 wt% of the binder initially present in the electrode material prior to performing method 10. In some embodiments, the second thermal treatment can result in vaporization of at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt%, at least about 99 wt%, at least about 99.5 wt%, at least about 99.9 wt%, at least about 99.99 wt%, or at least about 99.999 wt% of the binder initially present in the electrode material prior to performing method 10. In some embodiments, the second thermal treatment can result in vaporization of all or substantially all of the binder initially present in the electrode material prior to performing method 10.

[0075] After the second heat treatment, the electrode material can undergo a washing process in a solvent. The solvent can dissolve and / or remove any excess lithium from the electrode material. In some embodiments, the solvent can include water. In some embodiments, an aqueous solution or a water-based solution can be used to wash the electrode material. In some embodiments, the electrode material can undergo a third heat treatment operation (not shown). This heat treatment operation can complete a regeneration process and improve the performance of the electrode material. In some embodiments, the third heat treatment operation can be performed at a temperature within the same range as the second heat treatment operation mentioned above.

[0076] Step 19 is optional and includes treating the waste gas from the second thermal treatment. In some embodiments, the treatment may include purifying the waste gas (e.g., via a purification operation). In some embodiments, the purification may be via scrubbing (i.e., using a gas scrubber). In some embodiments, the waste gas may be purified via a scrubber. After the gas treatment, the purified gas may be released into the atmosphere or captured.

[0077] In some embodiments, step 19 can be used to meet specific environmental standards or remove a certain amount of harmful or undesirable materials discharged from the thermal treatment operation. In some embodiments, step 19 can include a gas scrubbing operation. In some embodiments, the purification operation removes acidic components from the waste gas. In some embodiments, the purification operation removes organic compounds, including VOCs, fluorocarbons, or hydrofluorocarbons. In some embodiments, the purification operation utilizes a thermal oxidizer to remove VOCs.

[0078] In some embodiments, method 10 can produce purified and regenerated cathode or anode materials. In some embodiments, method 10 can produce purified and regenerated cathode or anode materials by separating cathode or anode materials from other battery components (such as current collectors, separators, packaging, electrolytes, lithium salts, or certain additives). In some embodiments, method 10 can produce commercial-grade electrode materials without the need for precise quantification of lithium deficiency prior to relithiation. In some embodiments, method 10 can be used to separate, purify, and regenerate cathode and / or anode powders from other battery waste components.

[0079] In some embodiments, method 10 can produce functional cathode and / or anode materials. In some embodiments, current collectors, separators, packaging materials and other battery components can undergo further classification and separation for recycling. In some embodiments, magnetic separation can be used to separate ferrous metals from other materials. In some embodiments, eddy current separation can be used to separate non-ferrous metals from other materials. In some embodiments, density-based separation can be used to separate materials of different densities.

[0080] Figure 2A-2B is a diagram of a muffle furnace 120 for thermally treating battery waste, according to one embodiment. Figure 2A A perspective view of the muffle furnace 120 is shown, and Figure 2BA detailed schematic diagram of a muffle furnace 120 is shown. As shown, the muffle furnace 120 includes a gas inlet 121, a gas outlet 122, a thermocouple 123, and a muffle 124. In operation, battery waste or a portion thereof can be placed in the muffle furnace 120. Gas flows into the muffle furnace 120 via the gas inlet 121 and flows out of the muffle furnace 120 via the gas outlet 122. The gas can have any composition described above with reference to the first heat treatment, the second heat treatment, and / or the third heat treatment of method 10. Thermocouple 123 measures the temperature inside the muffle furnace 120, while the muffle furnace 124 maintains the heat inside the muffle furnace 120 during operation.

[0081] The flow rate of gas into and out of the muffle 120 can be controlled to affect the gas environment inside the muffle 120. In some embodiments, the flow rate of gas into and out of the muffle 120 can be at least about 1 SCCM, at least about 5 SCCM, at least about 10 SCCM, at least about 50 SCCM, at least about 100 SCCM, at least about 500 SCCM, at least about 1,000 SCCM, at least about 5,000 SCCM, at least about 10,000 SCCM, at least about 50,000 SCCM, at least about 100,000 SCCM, or at least about 500,000 SCCM. In some embodiments, the gas flow rate into and out of the muffle furnace 120 may be no more than about 1,000,000 SCCM, no more than about 500,000 SCCM, no more than about 100,000 SCCM, no more than about 50,000 SCCM, no more than about 10,000 SCCM, no more than about 5,000 SCCM, no more than about 1,000 SCCM, no more than about 500 SCCM, no more than about 100 SCCM, no more than about 50 SCCM, no more than about 10 SCCM, or no more than about 5 SCCM. Combinations of the above-mentioned gas flow rates are also possible (e.g., at least about 1 SCCM and no more than about 1,000,000 SCCM or at least about 500 SCCM and no more than about 50,000 SCCM), including all values ​​and ranges therebetween. In some embodiments, the gas flow rate into and out of the muffle furnace 120 may be about 1 SCCM, about 5 SCCM, about 10 SCCM, about 50 SCCM, about 100 SCCM, about 500 SCCM, about 1,000 SCCM, about 5,000 SCCM, about 10,000 SCCM, about 50,000 SCCM, about 100,000 SCCM, about 500,000 SCCM, or about 1,000,000 SCCM.

[0082] Figure 3A-3B is a diagram of a tube furnace 220 for thermally treating battery waste according to one embodiment. Figure 3A A perspective view of a tube furnace 220 is shown, and Figure 3B Detailed schematic diagram of tube furnace 220 is shown. As shown, tube furnace 220 includes gas inlet 221 and gas outlet 222. In some embodiments, gas inlet 221 and gas outlet 222 can be the same as described above with reference to Figure 2A-2B The gas inlet 121 and gas outlet 222 described are the same or substantially similar.

[0083] In some embodiments, a roller kiln (not shown) can be used for the thermal treatment operation. The roller kiln can have gas inflow and outflow to achieve various gas environments or gas flows during the thermal treatment. In some embodiments, a rotary kiln can be used for the thermal treatment operation. The rotary kiln can have gas inflow and outflow to achieve various gas environments or gas flows during the thermal treatment.

[0084] Figure 4A 310 is a flow chart of a method 310 for processing battery waste according to one embodiment. In some embodiments, method 310 may include separation operations performed in a dry manner without the aid of added liquid. As shown, method 310 optionally includes rotary screening of the battery waste at step 311, oscillating and screening the battery waste at step 312, and applying air jet sieve to the battery waste at step 313. Method 310 includes collecting dust from the exhaust at step 314, applying ultrasonic frequencies to the current collector to remove residues at step 315, and processing the electrode material via a crusher and / or a mill at step 316.

[0085] Step 311 is optional and includes rotary screening of battery waste. In some embodiments, rotary screening can be via a drum screen. Rotary screening can separate electrode materials from current collectors. In some embodiments, method 310 may include oscillating and ultrasonic screening (step 312), air jet screening (step 313), or other similar separation methods instead of or in addition to rotary screening of battery waste. Step 311 produces two material streams by screening or other similar separations based on particle size, one mainly including electrode materials (together with any additives mixed with electrode materials), and the other mainly including current collectors (or other larger particles of battery components). In some embodiments, rotary screening (drum screen), oscillation and ultrasonic screening and / or air jet screening can be operated without the use of liquid.

[0086] In some embodiments, step 311, step 312, and / or step 313 may generate waste gas. Step 314 includes collecting dust from the waste gas. In some embodiments, the waste gas stream may be treated and / or purified. In some embodiments, the treatment and / or purification of the waste gas stream may include collecting dust via a dust collector. In some embodiments, the waste gas stream treatment may include the above reference Figure 1 Any of the procedures described in steps 14 and 19.

[0087] In step 315, the material stream discharged from the rotary screening, oscillation and screening, and / or gas screening is further processed via ultrasonic treatment, and the material stream mainly includes the current collector (or other larger particle battery components) and residues. Ultrasonic treatment helps to further separate any residual small particle materials from the current collector. In some embodiments, the current collector stream can be further separated from other components based on the chemical, physical, and / or ferromagnetic properties of the current collector material. For example, the current collector stream can be processed via magnetic separation, eddy current separation, and / or density-based separation. In some embodiments, the current collector stream may not be subjected to an ultrasonic separation step, but may undergo separation based on the metal or other physical / chemical properties of the current collector (e.g., magnetic separation, eddy current separation, and / or density-based separation).

[0088] In step 316, the electrode material may undergo a comminution and / or grinding process to reduce the particle size and / or agglomeration of the electrode material. This may produce smaller particle size electrode material for further processing. In some embodiments, residual powder from exhaust dust collection may be added to the smaller particle size electrode material stream before and / or after the electrode material is fed to the crusher and / or mill.

[0089] Figure 5A is a flow chart of a method 410 for treating battery waste according to one embodiment. Method 410 is a wet separation method. As shown, method 410 includes washing the battery waste in an agitated washing tank at step 411, and optionally applying ultrasonic frequencies to the battery waste in a sonication tank at step 412. The method also includes filtering the electrode powder and decanting the waste stream at step 413, optionally purifying the decanted waste stream at step 414, drying the filtered electrode powder to form a dried electrode powder at step 415, optionally feeding the purified waste stream to an agitated washing tank and / or sonication tank at step 416, and applying ultrasonic frequencies to the current collector at step 417 to remove residues.

[0090] In some embodiments, any one of steps 411-417 can be performed in a controlled gas environment. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar, or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can be reducing. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. In some embodiments, the gas environment can include an oxidizing environment. An oxidizing environment can help remove organic compounds. In some embodiments, during steps 411-417, air or other aforementioned gases flow along the battery waste or flow through the battery waste. In some embodiments, during steps 411-417, no gas flows along the battery waste or flows through the battery waste.

[0091] In some embodiments, gaseous environment can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , including all values ​​and scopes therebetween. In some embodiments, gaseous environment can comprise the oxygen that improves the amount. In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0092] Step 411 includes washing the battery waste in a stirred washing tank. In some embodiments, the stirred washing tank may include an added liquid. In some embodiments, the added liquid may include water and / or a water-based solvent. In some embodiments, the added liquid may include a non-aqueous solvent, such as NMP, DMF, dimethylacetamide (DMAc or DMA), dihydro-levulinic ketone, or their derivatives, or their mixtures. In some embodiments, step 411 may be performed in a stirred washing tank, a washing tank using ultrasonic treatment and stirring for material deagglomeration, and / or other similar liquid-assisted separation processes.

[0093] In some embodiments, method 410 may include applying ultrasonic frequencies to the battery waste in a sonication tank at step 412. In some embodiments, sonication may be performed at least partially simultaneously with the washing at step 411. In some embodiments, sonication may be performed in the same container as the washing at step 411. In some embodiments, sonication may be performed at a different location than the washing at step 411.

[0094] Step 411 and / or step 412 may produce material streams by screening or other similar size-based separation, one comprising primarily electrode material (along with any additives mixed with the electrode material) and the other comprising primarily current collector (or other larger particle battery components).

[0095] In step 413, the material stream comprising primarily electrode material is screened while the waste stream is decanted. Step 413 removes liquid from the electrode material. Step 414 is optional and includes purifying the decanted waste stream. In some embodiments, the decanted waste stream can be purified via purification, neutralization, filtration, or any combination thereof to produce purified liquid for reuse.

[0096] Step 415 includes drying the filtered electrode powder to form a dried electrode powder. In some embodiments, drying can be via an oven. In some embodiments, drying can be via a furnace. Step 416 is optional and includes feeding the purified waste stream (i.e., washing the cell) to an agitated wash tank and / or sonication tank.

[0097] The material stream, which primarily includes the current collector (or other larger particles of battery components) and residues, is further processed via ultrasonic treatment at step 417. In some embodiments, step 417 may include the above-referenced Figure 4A Any processing steps of step 315 described.

[0098] Figure 5B A diagram of a processing plant for processing battery waste is shown according to various embodiments. As shown, Figure 5B Included are agitation wash tank 460 and sonication tank 470. In some embodiments, agitation wash tank 460 can be used in step 411 described above. In some embodiments, sonication tank 470 can be used in step 412 and / or step 417 described above.

[0099] Figure 65 is a flow chart of a method 510 for surface treating an electrode material. The method 510 is for treating a dried electrode powder. As shown, the method 510 includes applying a surface treatment to the electrode material while stirring at step 511, filtering the electrode powder and decanting a waste stream at step 512, optionally purifying the decanted waste stream at step 513, drying the filtered electrode powder to form a dried electrode powder at step 514, and optionally applying the purified waste stream to the surface treatment at step 515.

[0100] In some embodiments, any one of steps 511-515 can be performed in a controlled gas environment. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar, or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can be reducing. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. In some embodiments, the gas environment can include an oxidizing environment. An oxidizing environment can help remove organic compounds. In some embodiments, during steps 511-515, air or other aforementioned gases flow along the battery waste or flow through the battery waste. In some embodiments, during steps 511-515, no gas flows along the battery waste or flows through the battery waste.

[0101] In some embodiments, gaseous environment can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , including all values ​​and scopes therebetween. In some embodiments, gaseous environment can comprise the oxygen that improves the amount. In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0102] Step 511 includes applying a surface treatment to the electrode material while stirring. In some embodiments, the electrode material may be subjected to a separation operation (e.g., in accordance with the above reference Figure 1 Surface treatment is performed on the electrode material collected by the step 15 described above (separation performed in step 15 described above). In some embodiments, surface treatment can be performed on the electrode material collected from another previous operation. In some embodiments, surface treatment can be performed on the electrode material directly received in the direct recycling process. In the surface treatment operation, the electrode material is washed with a solvent to modify the surface of the electrode material. This modified surface can result in better performance of the electrode material ultimately recovered by the recycling process. In some embodiments, the solvent can include a weak acid (e.g., acetic acid, citric acid, oxalic acid, etc.).

[0103] In some embodiments, the acid concentration in the solvent may be at least about 1 wt %, at least about 2 wt %, at least about 3 wt %, at least about 4 wt %, at least about 5 wt %, at least about 6 wt %, at least about 7 wt %, at least about 8 wt %, at least about 9 wt %, at least about 10 wt %, at least about 11 wt %, at least about 12 wt %, at least about 13 wt %, at least about 14 wt %, at least about 15 wt %, at least about 16 wt %, at least about 17 wt %, at least about 18 wt %, or at least about 19 wt %. In some embodiments, the acid concentration in the solvent may be no more than about 20 wt%, no more than about 19 wt%, no more than about 18 wt%, no more than about 17 wt%, no more than about 16 wt%, no more than about 15 wt%, no more than about 14 wt%, no more than about 13 wt%, no more than about 12 wt%, no more than about 11 wt%, no more than about 10 wt%, no more than about 9 wt%, no more than about 8 wt%, no more than about 7 wt%, no more than about 6 wt%, no more than about 5 wt%, no more than about 4 wt%, no more than about 3 wt%, or no more than about 2 wt%. Combinations of the above-mentioned acid percentages are also possible (e.g., at least about 1 wt% and no more than about 20 wt%, or at least about 2.5 wt% and no more than about 5 wt%, or at least about 10 wt% and no more than about 20 wt%, or at least about 5 wt% and no more than about 10 wt%), including all values ​​and ranges therebetween. In some embodiments, the acid concentration in the solvent may be about 1 wt %, about 2 wt %, about 3 wt %, about 4 wt %, about 5 wt %, about 6 wt %, about 7 wt %, about 8 wt %, about 9 wt %, about 10 wt %, about 11 wt %, about 12 wt %, about 13 wt %, about 14 wt %, about 15 wt %, about 16 wt %, about 17 wt %, about 18 wt %, about 19 wt %, or about 20 wt %.

[0104] The acid concentration can be optimized to dissolve any undesirable surface coatings on the electrode material, but the leaching of the electrode material itself is limited, thereby largely or completely preserving the bulk electrode material composition and structure. In some embodiments, the solvent is another stronger acid, such as nitric acid, sulfuric acid, hydrochloric acid, or other similar acids. In some embodiments, the solid-to-liquid ratio of the electrode material to the solvent may be at least about 2.5 g / 100 mL, at least about 3 g / 100 mL, at least about 4 g / 100 mL, at least about 5 g / 100 mL, at least about 6 g / 100 mL, at least about 7 g / 100 mL, at least about 8 g / 100 mL, at least about 9 g / 100 mL, at least about 10 g / 100 mL, at least about 11 g / 100 mL, at least about 12 g / 100 mL, at least about 13 g / 100 mL, at least about 14 g / 100 mL, at least about 15 g / 100 mL, at least about 16 g / 100 mL, at least about 17 g / 100 mL, at least about 18 g / 100 mL, or at least about 19 g / 100 mL. In some embodiments, the solid-to-liquid ratio of the electrode material to the solvent may be no more than about 20 g / 100 mL, no more than about 19 g / 100 mL, no more than about 18 g / 100 mL, no more than about 17 g / 100 mL, no more than about 16 g / 100 mL, no more than about 15 g / 100 mL, no more than about 14 g / 100 mL, no more than about 13 g / 100 mL, no more than about 12 g / 100 mL, no more than about 11 g / 100 mL, no more than about 10 g / 100 mL, no more than about 9 g / 100 mL, no more than about 8 g / 100 mL, no more than about 7 g / 100 mL, no more than about 6 g / 100 mL, no more than about 5 g / 100 mL, no more than about 4 g / 100 mL, or no more than about 3 g / 100 mL. Combinations of the above-mentioned solid-to-liquid ratios of electrode material to solvent are also possible (e.g., at least about 2.5 g / mL and no more than about 20 g / 100 mL or at least about 5 g / 100 mL and no more than about 10 g / 100 mL), including all values ​​and ranges therebetween. In some embodiments, the solid-to-liquid ratio of the electrode material to the solvent may be at least about 2.5 g / 100 mL, about 3 g / 100 mL, about 4 g / 100 mL, about 5 g / 100 mL, about 6 g / 100 mL, about 7 g / 100 mL, about 8 g / 100 mL, about 9 g / 100 mL, about 10 g / 100 mL, about 11 g / 100 mL, about 12 g / 100 mL, about 13 g / 100 mL, about 14 g / 100 mL, about 15 g / 100 mL, about 16 g / 100 mL, about 17 g / 100 mL, about 18 g / 100 mL, about 19 g / 100 mL, or about 20 g / 100 mL.

[0105] In some embodiments, surface treatment is performed at room temperature. In some embodiments, surface treatment is performed at a temperature higher than the above but below the boiling point of the solvent. In some embodiments, surface treatment is performed under increased pressure, and can be performed in a pressure vessel. These temperatures can be at room temperature or at a temperature up to the boiling point of the solvent under this pressure. In some embodiments, surface treatment can be performed at about 30 ° C, about 40 ° C, about 50 ° C, about 60 ° C, about 70 ° C, about 80 ° C, about 90 ° C, about 100 ° C, about 110 ° C, about 120 ° C, about 130 ° C, about 140 ° C, about 150 ° C, about 160 ° C, about 170 ° C, about 180 ° C, about 190 ° C or about 200 ° C (including all values ​​and scopes therebetween). In some embodiments, the surface treatment can be performed at about 0.1 bar (gauge pressure), about 0.3 bar, about 0.4 bar, about 0.5 bar, about 0.6 bar, about 0.7 bar, about 0.8 bar, about 0.9 bar, about 1 bar, about 1.5 bar, about 2 bar, about 2.5 bar, about 3 bar, about 3.5 bar, about 4 bar, about 4.5 bar, about 5 bar, about 5.5 bar, about 6 bar, about 6.5 bar, about 7 bar, about 7.5 bar, about 8 bar, about 8.5 bar, about 9 bar, about 9.5 bar, or about 10 bar (including all values ​​and ranges therebetween).

[0106] In some embodiments, the mechanical stirring or agitation of step 511 can be used to improve contact and process efficiency. In some embodiments, a washing operation is followed after the surface treatment is completed to remove residual surface treatment solvent. Step 512 includes filtering the electrode powder and decanting the waste stream from the filtration. Filtration can produce a wet electrode powder.

[0107] Step 513 is optional and includes purifying the decanted waste stream. In some embodiments, step 513 may include the above reference Figure 5A Any process parameters of step 414 described above. Step 514 includes drying the filtered electrode powder to form a dried electrode powder. Drying can remove any residual liquid. In some embodiments, the dried electrode powder can be sieved. Step 515 is optional and includes applying the purified waste liquid stream to the surface treatment. In other words, the purified waste liquid can be added to the solvent used for the surface treatment in step 511.

[0108] Figure 7610 is a flow chart of a method 610 for surface treatment of electrode materials according to one embodiment. Method 610 can be used for wet separation of electrode materials from current collectors and surface treatment. As shown, method 610 optionally includes washing battery waste in an agitated washing tank in step 611, and applying ultrasonic frequencies to the battery waste in an acoustic treatment tank in step 612. Method 610 includes applying surface treatment to electrode powder in step 613, filtering the electrode powder and decanting the waste stream in step 614, optionally purifying the decanted waste stream in step 615, drying the filtered electrode powder in step 616 to form a dried electrode powder, optionally applying the waste stream to the agitated washing tank and / or the acoustic treatment tank in step 617, and optionally applying ultrasonic frequencies to the current collector in step 618 to remove residues.

[0109] In some embodiments, the surface treatment can be performed in a controlled gas environment. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar, or other similar gases. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can be reducing. In some embodiments, the gas environment can include a mixture of H2, Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO. In some embodiments, the gas environment can include an oxidizing environment. An oxidizing environment can help remove organic compounds. In some embodiments, during the surface treatment, air or other aforementioned gases flow along the battery waste or flow through the battery waste. In some embodiments, during the surface treatment, no gas flows along the battery waste or flows through the battery waste.

[0110] In some embodiments, gaseous environment can comprise about 0 volume %, about 1 volume %, about 2 volume %, about 3 volume %, about 4 volume %, about 5 volume %, about 6 volume %, about 7 volume %, about 8 volume %, about 9 volume %, about 10 volume %, about 12 volume %, about 13 volume %, about 14 volume %, about 15 volume %, about 16 volume %, about 17 volume %, about 18 volume %, about 19 volume %, about 20 volume %, about 21 volume %, about 22 volume %, about 23 volume %, about 24 volume %, or about 25 volume % O , including all values ​​and scopes therebetween. In some embodiments, gaseous environment can comprise the oxygen that improves the amount. In some embodiments, gaseous environment can comprise pure oxygen or high purity oxygen. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, including all values ​​and ranges therebetween.

[0111] In some embodiments, step 611 and step 612 can be performed at least partially simultaneously to separate the electrode material from the current collector. Washing the battery waste in the agitated washing tank and / or applying ultrasonic frequencies to the battery waste in the sonication tank can be performed at least partially simultaneously. Step 611 and / or step 612 utilizes liquid to assist in separating the electrode material from the current collector. After the electrode material is separated from the current collector, the electrode material can be separated from the current collector as described above. Figure 6 The processing of the described method 510 is performed the same or substantially similarly.

[0112] Step 613 includes applying a surface treatment to the electrode powder. In some embodiments, step 613 may be similar to the above-referenced Figure 6 Step 614 includes filtering the electrode powder and decanting the waste stream. In some embodiments, step 614 may be the same as described above with reference to Figure 6 Step 615 is optional and includes purifying the decanted waste stream. In some embodiments, step 615 can be the same as described above with reference to Figure 6 Step 616 includes drying the filtered electrode powder to form a dried electrode powder. In some embodiments, step 616 can be the same as described above with reference to Figure 6 Step 514 is the same or substantially similar as described.

[0113] Step 617 is optional and includes applying the purified waste stream to the agitated wash tank and / or the sonication tank. In some embodiments, step 617 can be the same as described above with reference to Figure 6 The purified waste stream may provide a solvent suitable for agitation and / or sonication. Step 618 is optional and includes applying an ultrasonic frequency to the current collector to remove residue from the current collector. In some embodiments, step 618 may be the same as described above with reference to Figure 5A Step 417 is the same or substantially similar as described.

[0114] Figure 8 710 is a flow chart of a method 710 for producing a recycled electrode material according to one embodiment. Method 710 can be used to recycle a variety of battery wastes as described above. In some embodiments, the battery waste comprises LCO, NCM waste cathode waste, NCA waste cathode waste, LFP waste cathode waste, and / or LTO waste anode waste. In some embodiments, the battery waste may include cathode and / or anode materials (with or without additives and / or adhesives) on a current collector. In some embodiments, the battery waste may include other battery components, such as packaging or separators. In some embodiments, the battery waste may include electrolytes or lithium salts.

[0115] As shown, method 710 includes applying a first thermal treatment in step 711 to decompose the electrode material, optionally treating exhaust gas from the first thermal treatment in step 712, separating the electrode material from other battery waste in step 713, optionally applying a surface treatment to the electrode material in step 714, filtering and drying the electrode material and decanting the waste stream in step 715, purifying the decanted waste stream in step 716, grinding and mixing the electrode material in step 717, and applying a second thermal treatment in step 718 to purify the recovered electrode material.

[0116] Step 711 includes applying a first thermal treatment to decompose the electrode material. In some embodiments, the first thermal treatment may partially or completely degrade the battery waste components, such as the binder, electrolyte, lithium salt, or packaging material. In some embodiments, step 711 may have the same characteristics as described above with reference to Figure 1 In step 712, the exhaust gas from the first thermal treatment is optionally treated. In some embodiments, the exhaust gas can be scrubbed, purified, and / or filtered to remove any harmful or undesirable compounds (e.g., hydrogen fluoride, hydrofluorocarbons, fluorocarbons, and / or VOCs) to emit a cleaner gas. In some embodiments, step 712 can have the same process parameters as described above with reference to Figure 1 Any process parameters of step 14 as described.

[0117] Step 713 includes separating the electrode material from other battery waste (e.g., current collectors, packaging, separators). In some embodiments, separation of the electrode material from other battery waste can include dry separation methods, including rotary screening, oscillation, sonication screening, and / or air jet screening. In some embodiments, separation of the electrode material from other battery waste can include wet separation methods, including agitation washing and / or sonication. In some embodiments, step 713 can have the same characteristics as described above with reference to Figure 1 Any process parameters described for step 15.

[0118] Step 714 is optional and includes applying a surface treatment to the electrode material. The surface treatment changes the surface properties of the electrode material. In some embodiments, step 714 may have the same Figure 1 Any process parameters of step 17 described above. Step 715 includes filtering and drying the electrode material and decanting the waste stream. In some embodiments, step 715 may include the above reference Figure 7 Any process parameters of step 614 and step 616 are described.

[0119] Step 716 includes purifying the decanted waste stream. In some embodiments, the waste stream may include an aqueous solution. In some embodiments, the aqueous solution may be neutralized and precipitated to form a purified water stream. In some embodiments, step 716 may include the above-referenced Figure 6 Any process parameters of step 513 described above. Step 717 includes grinding and mixing the electrode material. In some embodiments, the electrode material can be ground and mixed after the surface treatment of step 714. In some embodiments, if the electrode material is determined to be lithium deficient, a predetermined amount of a lithium source can be mixed with the electrode material. In some embodiments, an additional washing process can be applied to remove excess lithium from the electrode material.

[0120] Step 718 includes applying a second thermal treatment to purify the recovered electrode material. In some embodiments, step 718 can produce a commercial grade recycled electrode powder. In some embodiments, the second thermal treatment can be performed at a temperature of at least about 500°C, at least about 510°C, at least about 520°C, at least about 530°C, at least about 540°C, at least about 550°C, at least about 560°C, at least about 570°C, at least about 580°C, at least about 590°C, at least about 600°C, at least about 610°C, at least about 620°C, at least about 630°C, at least about 640°C, at least about 650°C, at least about 660°C, at least about 670°C, at least about 680°C, or at least about 690°C. In some embodiments, the second thermal treatment may be performed at a temperature of no more than about 700° C., no more than about 690° C., no more than about 680° C., no more than about 670° C., no more than about 660° C., no more than about 650° C., no more than about 640° C., no more than about 630° C., no more than about 620° C., no more than about 610° C., no more than about 600° C., no more than about 590° C., no more than about 580° C., no more than about 570° C., no more than about 560° C., no more than about 550° C., no more than about 540° C., no more than about 530° C., no more than about 520° C., or no more than about 510° C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 500° C. and no more than about 700° C. or at least about 550° C. and no more than about 650° C.), including all values ​​and ranges therebetween. In some embodiments, the second heat treatment can be performed at a temperature of about 500°C, about 510°C, about 520°C, about 530°C, about 540°C, about 550°C, about 560°C, about 570°C, about 580°C, about 590°C, about 600°C, about 610°C, about 620°C, about 630°C, about 640°C, about 650°C, about 660°C, about 670°C, about 680°C, about 690°C, or about 700°C.

[0121] In some embodiments, the electrode material derived from the recovery of the second thermal treatment can include LFP. In some embodiments, the second thermal treatment can be performed in an inert environment (for example, including nitrogen). In some embodiments, the second thermal treatment can have a duration of at least about 3 hours, at least about 3.5 hours, at least about 4 hours, at least about 4.5 hours, at least about 5 hours or at least about 5.5 hours. In some embodiments, the second thermal treatment can have a duration of no more than about 6 hours, no more than about 5.5 hours, no more than about 5 hours, no more than about 4.5 hours, no more than about 4 hours or no more than about 3.5 hours. The combination of the above-mentioned duration is also possible (for example, at least about 3 hours and no more than about 6 hours or at least about 3.5 hours and no more than about 5.5 hours), including all values ​​and scopes between them. In some embodiments, the second thermal treatment can have a duration of about 3 hours, about 3.5 hours, about 4 hours, about 4.5 hours, about 5 hours, about 5.5 hours or about 6 hours.

[0122] In some embodiments, the electrode material containing nickel or cobalt (such as LCO or NCM) can be treated by a second heat treatment operation at a temperature of at least about 700°C, at least about 750°C, at least about 800°C, at least about 850°C, at least about 900°C, or at least about 950°C. In some embodiments, the second heat treatment operation can be carried out at a temperature of no more than about 1,000°C, no more than about 950°C, no more than about 900°C, no more than about 850°C, no more than about 800°C, or no more than about 750°C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 700°C and no more than about 1,000°C or at least about 800°C and no more than about 900°C), including all values ​​and ranges therebetween. In some embodiments, the second heat treatment operation can be carried out at a temperature of about 700°C, about 750°C, about 800°C, about 850°C, about 900°C, about 950°C, or about 1,000°C. In some embodiments, the second heat treatment operation may be performed in air or a high oxygen environment.

[0123] In some embodiments, the second thermal treatment can have a duration of at least about 8 hours, at least about 8.5 hours, at least about 9 hours, at least about 9.5 hours, at least about 10 hours, at least about 10.5 hours, at least about 11 hours, at least about 11.5 hours, at least about 12 hours, at least about 12.5 hours, at least about 13 hours, at least about 13.5 hours, at least about 14 hours, or at least about 14.5 hours. In some embodiments, the second thermal treatment can have a duration of no more than about 15 hours, no more than about 14.5 hours, no more than about 14 hours, no more than about 13.5 hours, no more than about 13 hours, no more than about 12.5 hours, no more than about 12 hours, no more than about 11.5 hours, no more than about 11 hours, no more than about 10.5 hours, no more than about 10 hours, no more than about 9.5 hours, no more than about 9 hours, or no more than about 8.5 hours. The combination of the duration of the second heat treatment time mentioned above is also possible (for example, at least about 8 hours and no more than about 15 hours or at least about 10 hours and no more than about 12 hours), including all values ​​and scopes therebetween. In some embodiments, the second heat treatment can have a duration of about 8 hours, about 8.5 hours, about 9 hours, about 9.5 hours, about 10 hours, about 10.5 hours, about 11 hours, about 11.5 hours, about 12 hours, about 12.5 hours, about 13 hours, about 13.5 hours, about 14 hours, about 14.5 hours, or about 15 hours.

[0124] Fig. 9 is a decision flow chart of a method 810 for processing electrode materials according to one embodiment. In some embodiments, the method 810 can be used to directly recycle battery waste. In some embodiments, the method 810 can be used to recycle battery waste containing spent graphite anodes.

[0125] As shown, method 810 includes determining whether the electrode binder is water soluble at step 801. If not, method 810 continues at step 811 to apply a heat treatment to decompose the electrode material, at step 812 to separate the electrode material from other battery waste, and at step 813 to apply the electrode material to a battery manufacturing process. If the binder is water soluble, method 810 continues at step 861 to wash the battery waste and the electrode material, at step 862 to separate the electrode material from other battery waste, and at step 863 to filter and dry the electrode material.

[0126] Step 801 includes determining whether the battery waste or a subset of the battery waste is water soluble. In some embodiments, the battery waste or its subset can be subjected to a dissolution test in water to determine whether there is a water soluble adhesive or a water insoluble adhesive. In some embodiments, the type of adhesive is known in advance. In some embodiments, the battery waste is tested using an experiment, spectroscopy, spectrometry or other similar tests to determine whether there is a water soluble or water insoluble adhesive. In some embodiments, the test can be a gas chromatography, mass spectrometry, Raman spectroscopy, Fourier transform infrared spectroscopy, energy dispersive x-ray spectroscopy or other similar tests or a combination thereof.

[0127] If the binder is water soluble, step 861 includes washing the battery waste including the electrode material. In some embodiments, washing can be via an aqueous solvent (e.g., water). In some embodiments, step 861 can have the same characteristics as described above with reference to Figure 7 Any process parameters of step 611 described above. Step 862 includes separating the electrode material from other battery waste. In some embodiments, step 862 may include the above reference Figure 8 Any process parameters of step 713 described above. Step 863 includes filtering and drying the electrode material. In some embodiments, step 863 may include the above reference Figure 8 Any process parameters of step 715 described above. Filtration and drying can produce an electrode material, such as a graphite electrode material. In some embodiments, the electrode material can additionally undergo a surface treatment operation to modify the surface of the electrode material. In some embodiments, the surface treatment operation can have the same properties as described above with reference to Figure 8 Any characteristics of step 714 described above. In some embodiments, the electrode material can additionally undergo a heat treatment operation to regenerate the electrode material. In some embodiments, the heat treatment operation can have the same characteristics as described above with reference to Figure 1 Any characteristics of the first heat treatment operation of step 13 and / or the second heat treatment operation of step 18 are described.

[0128] For battery waste with a water-insoluble binder, method 810 includes applying a heat treatment at step 811 to decompose the electrode material. The heat treatment may partially or completely remove or degrade the water-insoluble binder (e.g., PVDF). In some embodiments, the battery waste is heat treated to a temperature of at least about 400°C, at least about 450°C, at least about 500°C, or at least about 550°C. In some embodiments, the battery waste is heat treated at a temperature of no more than about 600°C, no more than about 550°C, no more than about 500°C, or no more than about 400°C. Combinations of the above-mentioned battery waste heat treatment temperatures are also possible (e.g., at least about 400°C and no more than about 600°C or at least about 450°C and no more than about 550°C), including all values ​​and ranges therebetween. In some embodiments, the battery waste is heat treated at a temperature of about 400°C, about 450°C, about 500°C, about 550°C, or about 600°C. In some embodiments, the heat treatment is performed under an inert gas as described above. In some embodiments, the exhaust gas generated during the thermal process is scrubbed, washed, purified, and / or filtered to remove any harmful or undesirable compounds (eg, hydrogen fluoride).

[0129] Step 812 includes separating the electrode material from other battery waste. In some embodiments, the separation operation uses a dry method (such as rotary screening, oscillation and sonication screening, and air jet screening) to separate the current collector or other battery waste components from the electrode powder (which may include additives still present in the electrode powder). Step 812 may include separating the electrode material from the current collector. In some embodiments, the current collector may include a copper sheet and the electrode material may include graphite. The separated electrode material (e.g., in the form of a powder) is collected as an output in the recycling process. In some embodiments, the separation of the electrode material from other battery waste may have the same method as described above with reference to Figure 8 Any process parameters of step 713 are described.

[0130] In some embodiments, the electrode material may undergo additional surface treatment operations to modify the electrode material surface. In some embodiments, the electrode material may undergo additional heat treatment operations to regenerate the electrode material. These surface treatments and / or heat treatment processes may include any process parameters of the above-mentioned surface treatment processes and / or heat treatment processes.

[0131] Fig.10 is a flow chart of a method 910 for recycling battery waste according to one embodiment. In some embodiments, the method 910 can be used in a system or facility. In some embodiments, the method 910 can be used to recycle Li x M yPO4 electrode material, wherein M is at least one transition metal and x and y are integers. In some embodiments, method 910 can be used to recycle LFMP or other similar LFP or LFMP compounds and / or their derivatives. In some embodiments, battery waste can include cathode materials (with or without adhesives) on current collectors. In some embodiments, battery waste can include other battery components, such as packaging or separators. In some embodiments, battery waste can include anodes. In some embodiments, battery waste can include electrolytes and / or lithium salts. In some embodiments, battery waste can include cathode additives such as conductive carbon.

[0132] As shown, method 910 includes applying a first heat treatment at step 911 to at least partially degrade the battery waste, separating the electrode material from other battery waste at step 912, and optionally applying a second heat treatment at step 913 to at least partially remove electrode additives from the electrode material. Method 910 optionally includes mixing and grinding the electrode material at step 914. Method 910 also includes applying a third heat treatment in a reducing environment at step 915. Method 910 optionally includes mixing and grinding the electrode material at step 916, and applying a fourth heat treatment at step 917. Method 910 also includes reducing the size of the electrode material at step 918.

[0133] In step 911, method 910 includes applying a first thermal treatment to at least partially degrade battery waste. The first thermal treatment can partially or completely remove battery waste components (such as adhesives, electrolytes and lithium salts) or degrade battery waste components. The temperature of the first thermal treatment can decompose and / or degrade at least a portion of the battery waste component. The decomposed and / or degraded part of the battery waste component can then be removed (for example, via gasification). In some embodiments, the first thermal treatment can be performed in an inert gas environment. In some embodiments, the first thermal treatment can be performed in a reducing gas environment. In some embodiments, the gas environment can include gases such as CO2, CO, N2, Ar, H2, or mixtures thereof. In some embodiments, the first thermal treatment can be performed in an oxidizing gas environment. In some embodiments, the first thermal treatment can be performed in air. In some embodiments, the first thermal treatment can be performed in a high oxygen environment (e.g., at least about 20% by volume, at least about 25% by volume, at least about 30% by volume, at least about 35% by volume, at least about 40% by volume, at least about 45% by volume, at least about 50% by volume, at least about 55% by volume, at least about 60% by volume, at least about 65% by volume, at least about 70% by volume, at least about 75% by volume, at least about 80% by volume, at least about 85% by volume, at least about 90% by volume, or at least about 95% by volume of oxygen, including all values ​​and ranges therebetween). In some embodiments, the first thermal treatment can be performed in a pure oxygen environment. In some embodiments, the first thermal treatment can be performed in an environment with at least about 96% by volume, at least about 97% by volume, at least about 98% by volume, at least about 99% by volume, at least about 99% by volume, at least about 99.9% by volume, at least about 99.99% by volume, or at least about 99.999% by volume of oxygen.

[0134] In some embodiments, the first thermal treatment can be at a temperature of at least about 300°C, at least about 350°C, at least about 400°C, at least about 450°C, at least about 500°C, or at least about 550°C, at least about 600°C, at least about 650°C, at least about 700°C, at least about 750°C, at least about 800°C, at least about 850°C, at least about 900°C, at least about 950°C, at least about 1,000°C, at least about 1,050°C, or at least about 1,100°C. In some embodiments, the first thermal treatment may be at a temperature of no more than about 1,150° C., no more than about 1,100° C., no more than about 1,050° C., no more than about 1,000° C., no more than about 950° C., no more than about 900° C., no more than about 850° C., no more than about 800° C., no more than about 750° C., no more than about 700° C., no more than about 650° C., no more than about 600° C., no more than about 550° C., no more than about 500° C., no more than about 450° C., no more than about 400° C., or no more than about 350° C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 300° C. and no more than about 1,150° C. or at least about 500° C. and no more than about 800° C.), including all values ​​and ranges therebetween. In some embodiments, the first heat treatment can be at a temperature of about 300°C, about 350°C, about 400°C, about 450°C, about 500°C, about 550°C, about 600°C, about 650°C, about 700°C, about 750°C, about 800°C, about 850°C, about 900°C, about 950°C, about 1,000°C, about 1,050°C, about 1,100°C, or about 1,150°C.

[0135] In some embodiments, the first thermal treatment can have at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours or at least about 15 hours of duration. In some embodiments, the first thermal treatment can have no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours or no more than about 2 hours of duration. The combination of the duration of the first thermal treatment mentioned above is also possible (for example, at least about 1 hour and no more than about 16 hours or at least about 4 hours and no more than about 8 hours), including all values ​​and scopes between them. In some embodiments, the first thermal treatment can have a duration of about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0136] Step 912 includes separating the electrode material from other battery waste components. In some embodiments, other battery waste components may include current collectors and / or separators. In some embodiments, the electrode material may include electrode powder. In some embodiments, separation may be via a dry separation method. In some embodiments, separation may be via rotary screening, vibration, sonication screening, air jet screening, or any combination thereof. In some embodiments, separation may include a wet separation method. In some embodiments, separation may include agitation washing, sonication, or any combination thereof.

[0137] Step 913 is optional, and includes a second thermal treatment to at least partially remove electrode additives from electrode materials. In some embodiments, the second thermal treatment may be contained in an oxidizing gas environment to decompose and / or degrade battery waste components such as adhesives, electrolytes, lithium salts, anodes, and / or electrode additives. In some embodiments, the second thermal treatment may be performed in air. In some embodiments, the second thermal treatment may be performed in a high oxygen environment (e.g., at least about 20% by volume, at least about 25% by volume, at least about 30% by volume, at least about 35% by volume, at least about 40% by volume, at least about 45% by volume, at least about 50% by volume, at least about 55% by volume, at least about 60% by volume, at least about 65% by volume, at least about 70% by volume, at least about 75% by volume, at least about 80% by volume, at least about 85% by volume, at least about 90% by volume, or at least about 95% by volume of oxygen, including all values ​​and ranges therebetween). In some embodiments, the second thermal treatment may be performed in a pure oxygen environment. In some embodiments, the second heat treatment can be performed in an environment having at least about 96 volume %, at least about 97 volume %, at least about 98 volume %, at least about 99 volume %, at least about 99 volume %, at least about 99.9 volume %, at least about 99.99 volume %, or at least about 99.999 volume % oxygen.

[0138] In some embodiments, the second thermal treatment may partially or completely remove additives from the electrode, including conductive carbon. In some embodiments, the second thermal treatment may partially or completely remove anode graphite from the electrode material. In some embodiments, the conductive carbon and / or graphite in the battery waste may be partially or completely oxidized during the second thermal treatment and generate CO or CO2. In some embodiments, the electrode material may be partially or completely oxidized after the second thermal treatment. In some embodiments, the LFP electrode material may be partially or completely oxidized during the second thermal treatment and may generate an oxidized cathode product. In some embodiments, the oxidized cathode product may include Fe2O3, Fe3O4, Li3Fe2(PO4)3, LiFeP2O7FePO4, Li3PO4, Li2CO3, LiOH, or any combination thereof.

[0139] In some embodiments, the second heat treatment can be at a temperature of at least about 300°C, at least about 350°C, at least about 400°C, at least about 450°C, at least about 500°C, or at least about 550°C, at least about 600°C, at least about 650°C, at least about 700°C, at least about 750°C, at least about 800°C, at least about 850°C, at least about 900°C, at least about 950°C, at least about 1,000°C, at least about 1,050°C, or at least about 1,100°C. In some embodiments, the second thermal treatment may be at a temperature of no more than about 1,150° C., no more than about 1,100° C., no more than about 1,050° C., no more than about 1,000° C., no more than about 950° C., no more than about 900° C., no more than about 850° C., no more than about 800° C., no more than about 750° C., no more than about 700° C., no more than about 650° C., no more than about 600° C., no more than about 550° C., no more than about 500° C., no more than about 450° C., no more than about 400° C., or no more than about 350° C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 300° C. and no more than about 1,150° C. or at least about 500° C. and no more than about 800° C.), including all values ​​and ranges therebetween. In some embodiments, the second heat treatment can be at a temperature of about 300°C, about 350°C, about 400°C, about 450°C, about 500°C, about 550°C, about 600°C, about 650°C, about 700°C, about 750°C, about 800°C, about 850°C, about 900°C, about 950°C, about 1,000°C, about 1,050°C, about 1,100°C, or about 1,150°C.

[0140] In some embodiments, the second thermal treatment can have at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours or at least about 15 hours of duration. In some embodiments, the second thermal treatment can have no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours or no more than about 2 hours of duration. The combination of the duration of the first thermal treatment mentioned above is also possible (for example, at least about 1 hour and no more than about 16 hours or at least about 4 hours and no more than about 8 hours), including all values ​​and scopes between them. In some embodiments, the second heat treatment can have a duration of about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0141] In some embodiments, the second thermal treatment can partially or completely oxidize any additional materials or impurities in the battery waste. In some embodiments, the aluminum in the battery waste can be partially or completely oxidized. In some embodiments, the copper in the battery waste can be partially or completely oxidized. In some embodiments, the iron in the battery waste can be partially or completely oxidized. In some embodiments, the oxidation of impurities such as Al, Cu, or Fe can improve the performance of the cathode product finally recovered, reduce or eliminate any conductive impurities to avoid short circuit or otherwise damage the battery and / or promote the further removal of impurities.

[0142] In some embodiments, the first thermal treatment of step 911 and the second thermal treatment of step 913 can be combined into a single thermal treatment before separation in step 912. Such a single thermal treatment can partially or completely decompose and / or degrade some battery waste components, such as binders, electrolytes, lithium salts, anode materials, and / or conductive carbon. In some embodiments, the first thermal treatment of step 911 and / or the second thermal treatment of step 913 can partially or completely oxidize cathode materials.

[0143] In some embodiments, the waste generated during the first thermal treatment and / or the second thermal treatment may be scrubbed, purified, and / or filtered to remove any harmful or undesirable compounds (e.g., hydrogen fluoride, hydrofluorocarbons, fluorocarbons, and / or volatile organic compounds (VOCs)) to discharge a cleaner gas, as described above with reference to Figure 1 as described in steps 14 and 18.

[0144] In some embodiments, the electrode material can undergo additional reduction and regeneration to generate commercially available recycled materials. In some embodiments, the oxidized cathode product can undergo further reduction and regeneration to form commercially available recycled materials. In step 914, the electrode material is optionally subjected to a mixing and grinding process. In some embodiments, additives such as lithium sources (e.g., Li2CO3, LiOH) and / or reducing agents (e.g., carbon or organic compounds such as glucose, graphite, or starch) can be added during step 914 to facilitate mixing and grinding. In some embodiments, adding glucose, graphite, or starch during thermal treatment can be used to partially or completely decompose glucose, graphite, or starch to form a carbon coating on the cathode, which can result in improved electrochemical performance. In some embodiments, mixing and grinding can be performed via wet mixing with equipment such as nano-bead mills, planetary ball mills, pot-type tumbling mills, or any combination thereof.

[0145] In some embodiments, the size and morphology of the electrode material can be controlled during the mixing and grinding of step 914. In some embodiments, the grinding media can have a size of at least about 0.01 mm, at least about 0.05 mm, at least about 0.1 mm, at least about 0.5 mm, at least about 1 mm, at least about 5 mm, at least about 10 mm, or at least about 50 mm. In some embodiments, the grinding media can have a size of no more than about 100 mm, no more than about 50 mm, no more than about 10 mm, no more than about 5 mm, no more than about 1 mm, no more than about 0.5 mm, no more than about 0.1 mm, or no more than about 0.05 mm. Combinations of the above-mentioned grinding media sizes are also possible (e.g., at least about 0.01 mm and no more than about 100 mm or at least about 0.01 mm and no more than about 0.1 mm or at least about 0.1 mm and no more than about 1 mm or at least about 1 mm and no more than about 10 mm or at least about 10 mm and no more than about 100 mm), including all values ​​and ranges therebetween. In some embodiments, the grinding media can have a size of about 0.01 mm, about 0.05 mm, about 0.1 mm, about 0.5 mm, about 1 mm, about 5 mm, about 10 mm, about 50 mm, or about 100 mm.

[0146] In some embodiments, the grinding and mixing of step 914 can be for a duration of at least about 30 seconds, at least about 36 seconds, at least about 1 minute, at least about 6 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 9 hours, at least about 10 hours, at least about 20 hours, at least about 30 hours, at least about 40 hours, at least about 50 hours, at least about 60 hours, at least about 70 hours, at least about 80 hours, or at least about 90 hours. In some embodiments, the grinding and mixing of step 914 can be a duration of no more than about 100 hours, no more than about 90 hours, no more than about 80 hours, no more than about 70 hours, no more than about 60 hours, no more than about 50 hours, no more than about 40 hours, no more than about 30 hours, no more than about 20 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, no more than about 2 hours, no more than about 1 hour, no more than about 30 minutes, no more than about 6 minutes, or no more than about 36 seconds. Combinations of the above-mentioned durations are also possible (e.g., at least about 30 seconds and no more than about 100 hours or at least about 5 hours and no more than about 50 hours), including all values ​​and ranges therebetween. In some embodiments, the grinding and mixing of step 914 can be for a duration of about 30 seconds, about 36 seconds, about 1 minute, about 6 minutes, about 30 minutes, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 9 hours, about 10 hours, about 20 hours, about 30 hours, about 40 hours, about 50 hours, about 60 hours, about 70 hours, about 80 hours, about 90 hours, or about 100 hours.

[0147] In some embodiments, the rotation speed of the mixing and grinding process of step 914 may be at least about 0 rpm, at least about 1 rpm, at least about 5 rpm, at least about 10 rpm, at least about 100 rpm, at least about 500 rpm, at least about 1,000 rpm, at least about 2,000 rpm, at least about 5,000 rpm, at least about 10,000 rpm, or at least about 20,000 rpm. In some embodiments, the rotation speed of the mixing and grinding process of step 914 may be no more than about 50,000 rpm, no more than about 20,000 rpm, no more than about 10,000 rpm, no more than about 5,000 rpm, no more than about 2,000 rpm, no more than about 1,000 rpm, no more than about 5,000 rpm, no more than about 1,000 rpm, no more than about 500 rpm, no more than about 100 rpm, no more than about 10 rpm, no more than about 5 rpm, or no more than about 1 rpm. Combinations of the above-mentioned rotational speeds are also possible (e.g., at least about 0 rpm and no more than about 50,000 rpm or at least about 100 rpm and no more than about 10,000 rpm), including all values ​​and ranges therebetween. In some embodiments, the rotational speed of the mixing and grinding process of step 914 may be about 0 rpm, about 1 rpm, about 5 rpm, about 10 rpm, about 100 rpm, about 500 rpm, about 1,000 rpm, about 2,000 rpm, about 5,000 rpm, about 10,000 rpm, or about 20,000 rpm. In some embodiments, the rotation speed of the mixing and grinding process can be about 0 rpm to about 100 rpm, about 100 rpm to about 500 rpm, about 500 rpm to about 1,000 rpm, about 1,000 rpm to about 2,000 rpm, about 2,000 rpm to about 5,000 rpm, about 5,000 rpm to about 10,000 rpm, about 10,000 rpm to about 20,000 rpm, and about 20,000 rpm to 50,000 rpm.

[0148] In some embodiments, dispensing agents (dispensers) such as water, ethanol or other organic solvents can be added to improve the performance of mixing. In some embodiments, the drying process after wet mixing can be performed using equipment such as spray dryer, stirring dryer, conical dryer, vacuum rotary dryer, roller scraper dryer, flash dryer or any combination thereof. In some embodiments, the form and particle size of the electrode material can be controlled by adjusting the feed rate and / or drying temperature during the mixing process. In some embodiments, the form and particle size of the electrode material can be controlled by adjusting the feed rate and / or drying temperature after the mixing process. In some embodiments, the mixing and grinding of step 914 can be performed using equipment such as air jet mill, high-speed mixer, ball mill or any combination thereof via dry mixing.

[0149] Step 915 includes applying a third heat treatment to the electrode material in a reducing environment. In some embodiments, the third heat treatment can form olivine FePO4 (or other derivatives, such as MPO4, wherein M is at least one transition metal) and a lithium salt. In some embodiments, if the electrode material lacks lithium, a predetermined amount of lithium source can be mixed with the electrode material (e.g., an oxidized cathode product) during the third heat treatment. In some embodiments, the third heat treatment can be performed in an inert environment. In some embodiments, the third heat treatment can be performed in an inert or reducing gas environment to reduce the oxidized cathode product. In some embodiments, the added reducing agent can be equal to or exceed the stoichiometric amount to completely reduce the electrode material. In some embodiments, the reducing agent can include glucose. In some embodiments, the third heat treatment can completely reduce iron to form a reduced iron compound.

[0150] In some embodiments, the third heat treatment can be at a temperature of at least about 300°C, at least about 350°C, at least about 400°C, at least about 450°C, at least about 500°C, or at least about 550°C, at least about 600°C, at least about 650°C, at least about 700°C, at least about 750°C, at least about 800°C, at least about 850°C, at least about 900°C, at least about 950°C, at least about 1,000°C, at least about 1,050°C, or at least about 1,100°C. In some embodiments, the third thermal treatment may be at a temperature of no more than about 1,150° C., no more than about 1,100° C., no more than about 1,050° C., no more than about 1,000° C., no more than about 950° C., no more than about 900° C., no more than about 850° C., no more than about 800° C., no more than about 750° C., no more than about 700° C., no more than about 650° C., no more than about 600° C., no more than about 550° C., no more than about 500° C., no more than about 450° C., no more than about 400° C., or no more than about 350° C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 300° C. and no more than about 1,150° C. or at least about 500° C. and no more than about 800° C.), including all values ​​and ranges therebetween. In some embodiments, the third heat treatment can be at a temperature of about 300°C, about 350°C, about 400°C, about 450°C, about 500°C, about 550°C, about 600°C, about 650°C, about 700°C, about 750°C, about 800°C, about 850°C, about 900°C, about 950°C, about 1,000°C, about 1,050°C, about 1,100°C, or about 1,150°C.

[0151] In some embodiments, the 3rd thermal treatment can have at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours or at least about 15 hours of duration.In some embodiments, the 3rd thermal treatment can have no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours or no more than about 2 hours of duration.The combination of the duration of the first thermal treatment mentioned above is also possible (for example, at least about 1 hour and no more than about 16 hours or at least about 4 hours and no more than about 8 hours), including all values ​​and scopes between them. In some embodiments, the third heat treatment can have a duration of about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0152] Step 916 is optional and includes mixing and grinding the electrode material. In some embodiments, step 916 can include any of the process parameters described above for step 914. Therefore, certain aspects of step 916 are not described in further detail herein.

[0153] Step 917 is optional and includes a fourth thermal treatment. In some embodiments, the fourth thermal treatment can completely reduce iron (or other corresponding elements in MPO4) to form olivine LiFePO4 (or other LFP derivatives such as LFMP). In some embodiments, the fourth thermal treatment can have any parameters the same as the third thermal treatment described above with reference to step 915. In some embodiments, the fourth thermal treatment can be performed in an inert or reducing gas environment to reduce the oxidized cathode product. In some embodiments, the fourth thermal treatment can form olivine LiFePO4 (or other derivatives, such as LFMP). In some embodiments, the fourth thermal treatment can be performed in an inert or reducing environment. In some embodiments, the third thermal treatment of step 915 and the fourth thermal treatment of step 917 can be combined into a single thermal treatment step.

[0154] In some embodiments, the fourth thermal treatment can be at a temperature of at least about 300°C, at least about 350°C, at least about 400°C, at least about 450°C, at least about 500°C, or at least about 550°C, at least about 600°C, at least about 650°C, at least about 700°C, at least about 750°C, at least about 800°C, at least about 850°C, at least about 900°C, at least about 950°C, at least about 1,000°C, at least about 1,050°C, or at least about 1,100°C. In some embodiments, the fourth thermal treatment may be at a temperature of no more than about 1,150° C., no more than about 1,100° C., no more than about 1,050° C., no more than about 1,000° C., no more than about 950° C., no more than about 900° C., no more than about 850° C., no more than about 800° C., no more than about 750° C., no more than about 700° C., no more than about 650° C., no more than about 600° C., no more than about 550° C., no more than about 500° C., no more than about 450° C., no more than about 400° C., or no more than about 350° C. Combinations of the above-mentioned temperatures are also possible (e.g., at least about 300° C. and no more than about 1,150° C. or at least about 500° C. and no more than about 800° C.), including all values ​​and ranges therebetween. In some embodiments, the fourth heat treatment can be at a temperature of about 300°C, about 350°C, about 400°C, about 450°C, about 500°C, about 550°C, about 600°C, about 650°C, about 700°C, about 750°C, about 800°C, about 850°C, about 900°C, about 950°C, about 1,000°C, about 1,050°C, about 1,100°C, or about 1,150°C.

[0155] In some embodiments, the 4th thermal treatment can have at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours or at least about 15 hours of duration. In some embodiments, the 4th thermal treatment can have no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours or no more than about 2 hours of duration. The combination of the duration of the first thermal treatment mentioned above is also possible (for example, at least about 1 hour and no more than about 16 hours or at least about 4 hours and no more than about 8 hours), including all values ​​and scopes between them. In some embodiments, the fourth thermal treatment can have a duration of about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0156] Step 18 includes reducing the size of the electrode material. In some embodiments, the size reduction process may include grinding or milling. In some embodiments, the size reduction process may reduce the size of the electrode material particles (e.g., LFP cathode material) to a D50 value of less than about 100 μm, less than about 75 μm, less than about 50 μm, less than about 25 μm, less than about 10 μm, less than about 5 μm, less than about 2 μm, less than about 1 μm, less than about 0.5 μm, less than about 0.2 μm, or less than about 0.1 μm. In some embodiments, the size reduction process may be performed via an air jet mill.

[0157] In some embodiments, the methods described herein may include other processes described herein. In some embodiments, the methods described herein may include separation, purification, filtration, drying, washing, and surface treatment processes described herein. In some embodiments, the methods described herein may include at least one of a purification step (as described above), a filtration step (as described above), a drying step (as described above), and / or a surface treatment step (as described above) after separation (e.g., step 15). In some embodiments, the methods described herein may include at least one of a purification step (as described above), a filtration step (as described above), a drying step (as described above), and / or a surface treatment step (as described above) after the first heat treatment (e.g., step 13) and / or the second heat treatment (e.g., step 18). In some embodiments, the methods described herein may include at least one of a purification step (as described above), a filtration step (as described above), a drying step (as described above), and / or a surface treatment step (as described above) after mixing / grinding (e.g., in step 717).

[0158] Example

[0159] Example 1: The electrochemical performance of different electrode materials (LTO anode, NCM cathode and LFP cathode) recycled from waste electrode scrap was compared with that of the original electrode material (standard). The electrochemical performance was measured in a CR-2032 type button cell comprising a lithium metal electrode, a polypropylene separator, an electrode made of recycled or standard material and an electrolyte of 1M LiPF6 in EC / DMC (3:7 by volume). The recycled or standard electrode was prepared by mixing 80 weight percent (wt%) of recycled powder with 10 wt% PVDF and 10 wt% conductive carbon. The button cell was charged and discharged at a 1C rate (nC rate means that the charge / discharge process is completed in 1 / n hour). Fig.11 The cycling performance of the recycled LTO material is shown compared to the cycling performance of the standard LTO material. Figure 8 The embodiment of the direct recycling process of the invention recycles LTO material from waste LTO scrap. No significant capacity fade is observed for the recycled LTO material after 150 cycles, while the standard LTO material shows about 12% capacity fade.

[0160] Embodiment 2: Fig.12 The cycling performance of the recycled NCM material is shown in comparison with that of the standard NCM material. Fig. 9Embodiments of the direct recycling process of recycling NCM materials from waste NCM waste products. The NCM materials were treated with 5 volume % acetic acid at room temperature for 20 minutes. The solid loading was 10 g / 100 ml. Compared with the standard NCM material, the recycled NCM without surface treatment showed a slightly lower initial discharge capacity, but a slower capacity decay rate. The recycled NCM material with surface treatment showed similar initial discharge capacity and better capacity retention.

[0161] Embodiment 3: Fig.13 The cycling performance of the recycled LFP material is shown compared to the cycling performance of the standard LFP material. Fig. 9 In an embodiment of a direct recycling process, LFP material is recycled from waste LFP waste. Overall, the recycled LFP material shows very similar recycling performance compared to standard LFP material.

[0162] Example 4: Spent LFP cathode waste was subjected to a first heat treatment at an airflow of 5 to 50 standard cubic feet per hour (SCFH). The first heat treatment was performed between 300°C and 500°C for 1 hour. Due to the decomposition of the binder, the cathode electrode powder was peeled off from the current collector. The LFP electrode powder was separated from the Al current collector. The LFP powder was subjected to a second heat treatment at an airflow of 5 to 50 SCFH. The second heat treatment was performed between 400°C and 700°C for 1 hour. After the second heat treatment, the electrode powder turned red, indicating the formation of oxidized cathode products. Fig.14 It is shown that the XRD pattern of the electrode powder after the second heat treatment changes significantly compared to the standard LFP powder. Li3Fe2(PO4)3, LiFeP2O7 and Fe2O3 phases appear after the second heat treatment, indicating oxidation of the electrode material. The carbon content in the electrode material also drops to 0.03-0.1 wt % (compared to 2-3 wt % without the second heat treatment). Next, 0.62 g of glucose and 0.06 g of LiOH·H2O are mixed into 4.5 g of electrode powder collected after the second heat treatment. The mixing process is carried out using a planetary ball mill with the addition of 18 ml of water. After drying, a uniform powder mixture is collected. The electrode powder is then subjected to a third heat treatment to complete the regeneration process. The third heat treatment is performed between 600°C and 700°C for 3 hours under a N2 flow.

[0163] The electrochemical performance of the recycled LFP material was measured in a CR-2032 type button cell containing a lithium metal counter electrode, a polypropylene separator, and an electrolyte of 1M LiPF6 in EC / DMC (3:7 by volume). The working electrode was prepared by mixing 80 weight percent (wt%) of the recycled powder with 10 wt% PVDF and 10 wt% conductive carbon. The button cell was charged and discharged at 1C rate. Fig.15 It is shown that the recycled LFP material provides a capacity comparable to that of the standard LFP cathode material at 1C rate.

[0164] Various concepts can be embodied as one or more methods, in which at least one embodiment has been provided. The actions performed as part of the method can be ordered in any suitable manner. Therefore, embodiments that perform actions in a sequence different from that shown can be constructed, which can include performing some actions simultaneously, even if shown as sequential actions in the illustrative embodiments. In other words, it should be understood that such features may not be limited to a specific execution order, but are limited to any number of threads, processes, services, servers, etc. that can be performed continuously, asynchronously, concurrently, in parallel, simultaneously, synchronously, etc. in a manner consistent with the present disclosure. Therefore, some of these features may be contradictory because they cannot exist in a single embodiment at the same time. Similarly, some features are applicable to one aspect of the innovation, but not to other aspects.

[0165] In addition, the present disclosure may include other innovations not currently described. Applicants reserve all rights to such innovations, including the right to implement such innovations, submit additional applications, continuations, continuations in part, divisions, and the like. Therefore, it should be understood that the advantages, implementation schemes, embodiments, functions, features, logic, operations, organizations, structures, topologies, and / or other aspects of the present disclosure should not be considered as limitations on the disclosure as defined by the implementation schemes or limitations on the equivalents of the implementation schemes. Depending on the specific expectations and / or features of individual and / or business users, database configurations and / or relational models, data types, data transmission and / or network frameworks, grammatical structures, and the like, various embodiments of the technology disclosed herein can be implemented in a manner that achieves a large amount of flexibility and customization as described herein.

[0166] As defined and used herein, all definitions should be understood to control over dictionary definitions, definitions in documents incorporated by reference, and / or ordinary meanings of the defined terms.

[0167] As used herein, in certain embodiments, the term "about" or "approximately" indicates a range of 10% plus or minus that value when preceding a numerical value. Where a range of values ​​is provided, it is understood that, unless the context clearly specifies otherwise, each intermediate value (accurate to one tenth of the unit of the lower limit) between the upper and lower limits of the range and any other specified values ​​or intermediate values ​​within the specified range are included in the present disclosure. The upper and lower limits of these smaller ranges may be independently included in smaller ranges that are also included in the present disclosure, subject to any specifically excluded limitations within the specified range. Where a specified range includes one or both of the limits, ranges excluding one or both of those included limits are also included in the present disclosure.

[0168] As used herein in the specification and embodiments, the phrase "and / or" should be understood to mean "either or both" of the elements so combined, i.e., elements that exist in combination in some cases and separately in other cases. Multiple elements listed with "and / or" should be interpreted in the same manner, i.e., "one or more" of the elements so combined. In addition to the elements specifically identified by the "and / or" clause, other elements may optionally be present, whether related or unrelated to those specifically identified. Therefore, as a non-limiting example, when used in conjunction with open language such as "comprising", reference to "A and / or B" may refer to only A (optionally including elements other than B) in one embodiment; only B (optionally including elements other than A) in another embodiment; both A and B (optionally including other elements) in yet another embodiment, etc.

[0169] As used herein in the specification and in the embodiments, "or" should be understood to have the same meaning as "and / or" as defined above. For example, when separating the items in the list, "or" or "and / or" should be interpreted as inclusive, that is, including at least one of a plurality of elements or element lists, and also including more than one, and optionally additional unlisted items. Only explicitly opposite indicating terms, such as "only one of them" or "just one of them", or when used in the embodiments, "consisting of..." will refer to including just one element in a plurality of elements or element lists. Generally speaking, when the front is an exclusive term, as used herein, the term "or" should only be interpreted as indicating exclusive alternative forms (that is, "one or the other but not two"), such as "any", "one of them", "only one of them" or "just one of them". When used in the embodiments, "consisting essentially of..." should have its ordinary meaning used in the field of patent law.

[0170] As used herein in the specification and embodiments, the phrase "at least one" with respect to a list of one or more elements should be understood to mean at least one (at least one) element selected from any one or more (one or more) elements in the list of elements, but does not necessarily include at least one of each and every element specifically listed in the list of elements, and does not exclude any combination of elements in the list of elements. This definition also allows that elements other than the elements specifically identified in the list of elements to which the phrase "at least one" refers may optionally be present, whether related or unrelated to those specifically identified elements. Thus, as a non-limiting example, "at least one of A and B" (or equivalently "at least one of A or B", or equivalently "at least one of A and / or B") may refer to at least one (optionally including more than one) A without B (and optionally including elements other than B) in one embodiment; to at least one (optionally including more than one) B without A (and optionally including elements other than A) in another embodiment; to at least one (optionally including more than one) A, and at least one (optionally including more than one) B (and optionally including other elements) in yet another embodiment; etc.

[0171] In the embodiments and the above description, all transitional phrases such as "comprising", "including", "carrying", "having", "containing", "involving", "containing", "comprising", etc. should be understood as open, that is, meaning including but not limited to. As set forth in Section 2111.03 of the United States Patent Office Manual of Patent Examining Procedures, Section 2111.03, only the transitional phrases "consisting of" and "consisting essentially of" shall be closed or semi-closed transitional phrases, respectively.

[0172] Although the specific embodiments of the present disclosure have been summarized above, many alternatives, modifications and variations will be apparent to those skilled in the art. Therefore, the embodiments set forth herein are intended to be illustrative rather than restrictive. Various changes may be made without departing from the spirit and scope of the present disclosure. Where the above methods and steps indicate that specific events occur in a particular order, those of ordinary skill in the art who benefit from the present disclosure will recognize that the order of specific steps may be modified and that such modifications conform to variations of the present invention. In addition, when possible, specific steps may be performed simultaneously in a parallel process, as well as sequentially as described above. Embodiments have been specifically shown and described, but it should be understood that various changes in form and detail may be made.

Claims

1. A method for recycling a certain amount of battery waste, the battery waste including electrode materials and current collectors, the electrode materials including active materials and binders, the method comprising: Applying a first heat treatment to the battery waste at a temperature of about 100 °C to about 700 °C, the first heat treatment decomposing at least about 80 wt% of the binder; Separating the electrode materials from the current collectors; And Applying a second heat treatment to the electrode materials at a temperature of about 400 °C to about 1,200 °C to produce recycled electrode materials, the second heat treatment decomposing at least 90 wt% of the remaining binder in the electrode materials to produce recycled electrode materials.

2. The method according to claim 1, further comprising: Applying a surface treatment to the electrode materials to remove surface coatings and / or surface impurities from the electrode materials.

3. The method according to claim 2, wherein the surface treatment comprises applying a solvent to the electrode materials.

4. The method according to claim 3, wherein the solvent comprises at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, or chemical derivatives thereof.

5. The method according to claim 1, wherein The electrode materials include LiCoO2, LiMn2O4, LiFe t M 1-t PO4, or LiNi a Mn b Co c A d At least one of O2, a + b + c + d = 1; wherein 0 < t < 1; and wherein A = Al, Zr, or Mg.

6. The method according to claim 1, wherein the first heat treatment has a duration of about 1 hour to about 6 hours at a temperature of about 400 °C to about 600 °C, and wherein the second heat treatment has a duration of about 1 hour to about 5 hours and a temperature of about 450 °C to about 800 °C.

7. The method according to claim 1, wherein the first heat treatment has a duration of about 1 hour to about 6 hours at a temperature of about 400 °C to about 600 °C, and wherein the second heat treatment has a duration of about 3 hours to about 15 hours and a temperature of about 600 °C to about 900 °C.

8. The method according to claim 1, wherein the recycled electrode materials have a lithium concentration of at least about 99 wt%.

9. The method according to claim 1, further comprising: Washing the electrode materials to remove at least a portion of the binder.

10. The method according to claim 1, further comprising: Before the first heat treatment, removing oxidizable impurities from the electrode materials by treating with at least one of an acid having a pH not exceeding about 4 or a base having a pH of at least about 13.

11. The method according to claim 1, wherein the second heat treatment vaporizes all of the remaining binder in the electrode materials.

12. A method for recycling a certain amount of battery waste, the battery waste including electrode materials connected to current collectors, the electrode materials including active materials and binders, the method comprising: Washing the battery waste with a solvent such that the solvent dissolves a portion of the binder and at least a portion of the electrode materials separates from the current collectors; Vaporizing at least about 80 wt% of the binder via a first heat treatment; flotation of the electrode material in a polar solvent mixed with an enhancer, the enhancer promoting the hydrophobicity of impurities in the electrode material, the flotation forming a hydrophilic phase containing the electrode material and a hydrophobic phase containing the impurities; separating the hydrophobic phase from the hydrophilic phase; as well as A second heat treatment is applied to the electrode material to produce a regenerated electrode material, the second heat treatment vaporizing at least about 95 weight percent of the remaining binder in the electrode material.

13. The method according to claim 12, further comprising: Prior to the first thermal treatment, oxidizable impurities are removed from the electrode material via treatment with at least one of an acid having a pH not exceeding about 4 or a base having a pH of at least about 13.

14. The method according to claim 12, wherein The electrode materials include LiCoO2, LiMn2O4, LiFe t M 1-t PO4, or LiNi a Mn b Co c A d At least one of O2; wherein a+b+c+d=1; and A=Al, Zr, or Mg.

15. The method according to claim 12, further comprising: A liquid is applied to the electrode material to remove surface coatings and / or surface impurities from the electrode material.

16. The method according to claim 15, further comprising: After the surface treatment, the electrode material is filtered to produce wet electrodes and a waste stream.

17. The method according to claim 16, further comprising: The waste stream is at least one of purified, neutralized, or filtered.

18. The method of claim 12, further comprising: An ultrasonic frequency is applied to the current collector to remove residual electrode material from the current collector.

19. The method of claim 12, wherein the washing comprises sonicating the battery waste.

20. A method comprising: separating an electrode material from a current collector via at least one of rotary sieving, oscillatory and ultrasonic sieving, or air jet sieving, the electrode material comprising a hydrophobic binder; crushing and / or grinding the electrode material to form an electrode powder; applying a first heat treatment to the electrode powder at a temperature of about 100° C. to about 700° C. for a duration of about 1 hour to about 6 hours, the first heat treatment at least partially decomposing the hydrophobic binder; as well as A second heat treatment is applied to the electrode powder to produce a regenerated electrode material, the second heat treatment decomposing at least 98 weight percent of the hydrophobic binder present in the electrode material prior to the first heat treatment.

21. The method according to claim 20, further comprising: Dust from the exhaust gas originating from the separation is collected to produce purified air.

22. The method according to claim 21, further comprising: The dust is combined with the electrode powder.

23. The method according to claim 20, wherein The electrode materials include LiCoO2, LiMn2O4, LiFe t M 1-t PO4, or LiNi a Mn b Co c A d At least one of O2; wherein a+b+c+d=1; and A=Al, Zr, or Mg.

24. A method comprising: separating an electrode material from a current collector via at least one of tank stirring in water or sonication in water, the electrode material comprising a hydrophilic binder; filtering the electrode material to form a wet electrode material and a waste stream; drying the wet electrode material to form a dried electrode material; applying a first heat treatment to the dried electrode material, the first heat treatment vaporizing at least about 80 weight percent of the hydrophilic binder; and A second heat treatment is applied to the dried electrode material to produce a regenerated electrode material, the second heat treatment having a duration of about 1 hour to about 15 hours and a temperature of about 450°C to about 900°C.

25. The method of claim 24, further comprising: Ultrasonic frequencies are applied to the current collector to remove residual electrode material.

26. The method of claim 24, further comprising: The waste stream is at least one of purified, neutralized, or filtered.

27. The method of claim 26, further comprising: The waste stream was added to water.

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