CN115020854A - Method for accelerating separation of battery electrode material and current collector - Google Patents
Method for accelerating separation of battery electrode material and current collector Download PDFInfo
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- CN115020854A CN115020854A CN202210686753.7A CN202210686753A CN115020854A CN 115020854 A CN115020854 A CN 115020854A CN 202210686753 A CN202210686753 A CN 202210686753A CN 115020854 A CN115020854 A CN 115020854A
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- current collector
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- electrode material
- pole piece
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- 239000007772 electrode material Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 34
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 17
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- 235000002906 tartaric acid Nutrition 0.000 claims description 6
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
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- JKTORXLUQLQJCM-UHFFFAOYSA-N 4-phosphonobutylphosphonic acid Chemical compound OP(O)(=O)CCCCP(O)(O)=O JKTORXLUQLQJCM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
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- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011149 active material Substances 0.000 claims description 3
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- 229910052802 copper Inorganic materials 0.000 claims description 3
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052743 krypton Inorganic materials 0.000 claims description 3
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 3
- BDKWOJYFHXPPPT-UHFFFAOYSA-N lithium dioxido(dioxo)manganese nickel(2+) Chemical compound [Mn](=O)(=O)([O-])[O-].[Ni+2].[Li+] BDKWOJYFHXPPPT-UHFFFAOYSA-N 0.000 claims description 3
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
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- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/15—Electronic waste
- B09B2101/16—Batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the field of waste lithium battery recovery, and discloses a method for accelerating separation of a battery electrode material and a current collector, which comprises the following steps: (1) disassembling the retired battery: disassembling a positive pole piece or a negative pole piece from a retired lithium battery; the pole piece comprises a current collector and an electrode material layer closely attached to the current collector; (2) material treatment: soaking the pole piece in a specific solution, wherein the specific solution can separate the electrode material layer from the current collector; (3) material separation: and introducing gas into the solution to accelerate the separation of the electrode material layer and the current collector. According to the invention, on the basis of separation (liquid phase separation) by using the action of the pole piece and the solution, the separation of the electrode material and the current collector is accelerated by air flow disturbance, so that the separation efficiency is obviously improved. Moreover, the introduced gas can dilute the harmful gas generated in the separation process, so that the risk brought by the harmful gas is effectively avoided, and the safety of the operation process is improved.
Description
Technical Field
The invention belongs to the field of waste lithium battery recovery, and particularly relates to a method for accelerating separation of a battery electrode material layer and a current collector, which can accelerate separation of the battery electrode material layer and the current collector and improve the safety of an operation process.
Background
With the rapid popularization and development of electric vehicles, how to deal with a large number of retired batteries becomes an urgent problem. Therefore, the reasonable recycling and reusing of the retired battery have very important significance and value. At present, battery electrode material recovery mainly involves the steps of battery disassembly, separation of an electrode material layer and a current collector and regeneration of the electrode material, wherein the separation process of the electrode material layer and the current collector is of great importance, and the subsequent regeneration performance of the electrode material is influenced. The current separation methods mainly comprise two methods, namely high-temperature solid-phase calcination separation and liquid-phase separation.
The high-temperature solid-phase calcination separation separates the electrode material layer and the current collector through high-temperature calcination, but the energy consumption of the process is high, and the degradation of active substances can be caused. Meanwhile, the current collector is easy to break at high temperature, and impurities are introduced into the electrode material.
Thus, liquid phase separation techniques are highly desired. Patent application No. 201910421896.3 discloses a method of stripping an active substance by dissolving a binder with an organic solution and by ultrasound. However, the separation requires long time and is low in efficiency, and the current collector is easy to break due to the increase of the ultrasonic intensity or the time. Patent application No. 201710840613.X discloses a technology for directly leaching active substances on a current collector by inorganic acid, and patent application No. 201710503058.1 discloses a technology for directly leaching the active substances on the current collector by using sodium hydroxide (alkali) to dissolve aluminum foil, but the current collector reacts in acid or alkali to generate combustible gas such as hydrogen, so that explosion is easily caused, and the current collector is not suitable for industrial production and application.
Disclosure of Invention
In view of the above defects or improvement needs in the prior art, an object of the present invention is to provide a method for accelerating the separation of a battery electrode material and a current collector, which accelerates the separation of the electrode material and the current collector through air flow disturbance on the basis of the separation (liquid phase separation) by using the effect of a pole piece and a solution, thereby significantly improving the separation efficiency. Compared with other means, the gas flow disturbance means based on the method is milder, the current collector is not easy to crack, and the introduced gas can dilute the harmful gas generated in the separation process, so that the risk brought by the harmful gas is effectively avoided, and the safety of the operation process can be improved.
To achieve the above object, according to the present invention, there is provided a method for accelerating separation of a battery electrode material and a current collector, comprising the steps of:
(1) disassembling the retired battery: disassembling a positive pole piece or a negative pole piece from a retired lithium battery; the pole piece comprises a current collector and an electrode material layer closely attached to the current collector;
(2) material treatment: soaking the pole piece in a specific solution, wherein the specific solution can separate the electrode material layer from the current collector;
when the pole piece is a positive pole piece, the solution is N-methyl pyrrolidone (NMP), Dimethylacetamide (DMAC), N-Dimethylformamide (DMF), triethyl phosphate (TEP), dimethyl sulfoxide (DMSO), hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, oxalic acid, citric acid, malic acid, tartaric acid, oxalic acid, phytic acid, lactic acid, lithium hydroxide, sodium hydroxide or potassium hydroxide solution;
when the pole piece is a negative pole piece, the solution is water, polyamino polyether tetramethylene Phosphonic Acid (PAPEMP), hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, oxalic acid, citric acid, malic acid, tartaric acid, oxalic acid, phytic acid or lactic acid solution;
(3) material separation: and introducing gas into the solution to accelerate the separation of the electrode material layer and the current collector.
As a further preferred aspect of the present invention, in the step (3), the gas is introduced at a rate in the range of 0.125 to 30 liters of gas/(liter of solution.min), preferably 2.5 to 25 liters of gas/(liter of solution.min), more preferably 15 to 20 liters of gas/(liter of solution.min).
As a further preferred aspect of the present invention, in the step (3), the gas introduced is at least one of air, carbon dioxide, nitrogen, helium, neon, argon, krypton, xenon, and radon.
As a further preferred aspect of the present invention, in the step (1), the current collector is an aluminum current collector, a copper current collector, a nickel current collector, a titanium current collector or a stainless steel current collector;
the compacted density of the electrode material layer is 0.5-4.0g/cm 3 The conductive paste consists of an active substance, a binder and a conductive agent.
As a further preferable aspect of the present invention, the active material is specifically a ternary nickel cobalt manganese material, a ternary nickel cobalt aluminum material, a lithium iron phosphate material, a lithium cobaltate material, a cobalt-free high nickel layered material, a lithium-rich positive electrode material, a lithium manganate material, a lithium nickel manganate material, a lithium titanate material, a titanium niobate material, a silicon-based material, or graphite.
Through the technical scheme of the invention, compared with the existing separation technology/method, the separation of the electrode material layer and the current collector can be accelerated by introducing gas into the specific solution which can separate the electrode material layer and the current collector to cause disturbance. Compared with other separation means such as ultrasonic and mechanical stirring, the invention has the advantages that the acting force generated by gas disturbance solution is milder, the electrode material can be promoted to integrally fall off from the current collector in a massive sheet form, the separation is thorough, no residue is generated basically, and the recovery rate of the electrode material can be effectively improved. Meanwhile, the acting force generated by the airflow is relatively soft, so that the current collector is prevented from being broken to a great extent, and a pure electrode material can be obtained; in addition, the harmful/combustible gas generated in the separation process can be diluted by ventilating, the safety coefficient of the reaction is greatly improved, the safety of the operation process is improved, the operation is simple and convenient, the cost is extremely low, and the method is favorable for industrial large-scale production.
Based on the invention, the rate range of the gas introduced in the aeration treatment process can be controlled to be 0.125-30L of gas/(L of solution/min), especially 2.5-25L of gas/(L of solution/min) and 15-20L of gas/(L of solution/min), so that the separation efficiency can be improved, the amount of impurities such as current collector debris and the like caused by disturbance can be effectively controlled, the problems that the separation speed is slow and the separation efficiency is influenced due to too slow aeration rate and the impurity content in the electrode material is increased and the purity of the electrode material is influenced due to too fast aeration rate can be avoided.
Specifically, the invention can obtain the following beneficial effects:
1. the separation of the current collector and the electrode material layer is accelerated (stirring is not needed) by introducing air flow to generate acting force, and the current collector is not easy to break by the acting force of the air flow. The method directly introduces gas into the specific solution for soaking the pole pieces to be separated, the types of the gas can be various, and the amount of the introduced gas and the introduction rate of the gas can be controlled; in the method, the specific solution can separate the electrode material layer from the current collector, and the gas flow can promote the separation process, so that the separation efficiency is improved, and impurities in the active substances are less.
2. Compared with separation means such as ultrasonic separation and mechanical stirring, the invention has the advantages that the acting force generated by the invention is milder, the electrode material is promoted to integrally fall off from the current collector in a massive sheet form, the separation is more thorough, no residue is generated basically, and the recovery rate of the electrode material can be effectively improved.
3. Harmful/combustible gas generated by the reaction is diluted by introducing airflow, so that the concentration of the generated gas is greatly reduced, and the safety of the operation process is improved.
4. Simple and convenient operation, low cost and contribution to industrial large-scale production and application.
The method of the invention can lead gas to be introduced into the specific solution which can separate the electrode material layer from the current collector to cause disturbance, promote the liquid to flow and accelerate the separation of the electrode material layer from the current collector. Meanwhile, the introduced gas can dilute harmful/flammable gas generated by side reaction in the separation process of the electrode material and the current collector, and the risk brought by the harmful/flammable gas is reduced.
The method is suitable for all the existing liquid phase separation technologies, can greatly improve the separation efficiency, reduce the impurities of the current collector generated by separation and improve the safety of the separation process. In conclusion, the method disclosed by the invention promotes the efficient and rapid separation of the electrode material layer and the current collector, and reduces the potential safety hazard caused by harmful/inflammable gases.
Drawings
FIG. 1 is a schematic process flow diagram of the process of the present invention.
FIG. 2 is a graph showing a compacted density of 4.0g/cm in example 1 3 Is being decommissioned LiNi 0.5 Co 0.2 Mn 0.3 O 2 A separation effect diagram of the positive pole piece; this figure specifically corresponds to retired LiNi 0.5 Co 0.2 Mn 0.3 O 2 And introducing argon into the positive pole piece in 0.1mol/L NaOH aqueous solution at a rate of 30L/min to separate an effect graph.
FIG. 3 is a graph showing a compacted density of 2.2g/cm in example 3 3 Washing a dried real object image after separating the retired lithium titanate cathode; the figure specifically corresponds to a negative electrode material and a copper foil separated after nitrogen is introduced into an out-of-service lithium titanate negative electrode piece at the speed of 10L/min, the separation speed is high, and the stripping rate is high; in fig. 3, (a) corresponds to a gray negative electrode material, and (b) corresponds to a brown copper foil.
FIG. 4 is a graph showing a compacted density of 0.5g/cm in example 4 3 A physical separation diagram of the ex-service hard carbon negative pole piece; the figure specifically corresponds to that the hard carbon negative pole piece is soaked in an aqueous solution, and air is introduced at 2.5L/min to promote the separation of the negative pole material and the copper foil.
Fig. 5 is a comparison graph of the separation effect of three different separation modes in example 2 and comparative example 2, wherein (a) in fig. 5 corresponds to the current collector after 300W power ultrasonic separation in comparative example 2, (b) in fig. 5 corresponds to the current collector after mechanical stirring separation in comparative example 2 at 400r/min, and (c) in fig. 5 corresponds to the current collector after carbon dioxide gas separation in example 2 at 20L/min.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
Disassembling the retired battery, and separating out the electrode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 The current collector is aluminum foil, and the compaction density is 4.0g/cm 3 The positive electrode sheet of (1). 100g of positive plate is soaked in 1L of 0.1mol/L NaOH aqueous solution, then argon is respectively introduced into the four groups of solutions at the speed of 15L/min, 20L/min, 25L/min and 30L/min (the argon gas is introduced by connecting a reactor with an argon gas cylinder, as shown in figure 1; in the following embodiment, the gas cylinder of the corresponding gas is adopted according to the difference of the passing gas). And recording the reaction time and the gas production rate of the reaction when the positive electrode material is completely stripped, wherein the gas production rate is hydrogen. And testing by an inductively coupled plasma spectrum generator to measure the Al content in the electrode material. The final results are shown in the following table:
| rate of aeration | Reaction time | Amount of gas | Al content of electrode material | Volume ratio of hydrogen |
| 15L/min general purposeQi (Qi) | 25min 52s | 399.31L | 0.5471％ | 2.83％ |
| Aeration at 20L/min | 23min 16s | 476.61L | 0.5386％ | 2.36％ |
| Aeration at 25L/min | 21min 44s | 554.61L | 0.5642％ | 2.01％ |
| Aeration at 30L/min | 20min 25s | 624.01L | 0.7264％ | 1.81％ |
As can be seen from the above table, the separation can be accelerated well by introducing gas, and the higher the aeration rate is, the higher the separation speed is. At various aeration rates shown in the above table, the Al content in the electrode material was kept at a low level; considering that the reaction time is long and the ventilation rate is high, the Al content of the current collector in the electrode material is increased, and therefore, the ventilation rate is optimal at 15-20L/min.
Example 2
Disassembling the retired battery, and separating out the electrode material LiFePO 4 The current collector is aluminum foil, and the compaction density is 3.5g/cm 3 The positive electrode sheet of (1). 150g ofThe positive plate is soaked in 1L of 0.1mol/L citric acid solution, and then carbon dioxide gas is introduced into the same four groups of solutions at the speed of 10L/min, 15L/min, 20L/min and 25L/min respectively. And recording the reaction time and the gas production rate of the reaction when the positive electrode material is completely stripped, wherein the gas production rate is hydrogen. And testing by an inductively coupled plasma spectrum generator to measure the Al content in the electrode material. The final results are shown in the following table:
| rate of aeration | Reaction time | Amount of gas | Al content of electrode material | Volume ratio of hydrogen |
| Aeration at 10L/min | 24min 17s | 244.23L | 0.0446％ | 0.57％ |
| Aeration at 15L/min | 20min 23s | 307.14L | 0.0413％ | 0.45％ |
| Aeration at 20L/min | 17min 54s | 359.39L | 0.0394％ | 0.39％ |
| Aeration at 25L/min | 16min 21s | 410.13L | 0.0437％ | 0.34％ |
As can be seen from the above table, the separation can be accelerated well by introducing gas, and the higher the aeration rate is, the higher the separation speed is. At various aeration rates shown in the above table, the Al content in the electrode material was kept at a low level; considering the long reaction time and the high aeration rate, the Al content of the current collector in the electrode material is increased. Therefore, the aeration rate is best at 15-20L/min.
Example 3
Disassembling the retired battery, separating out an electrode material of lithium titanate, a current collector of copper foil and a compaction density of 2.2g/cm 3 The negative electrode plate is characterized in that 200g of the negative electrode plate is soaked in 2L of water/ethanol mixed solution (v/v is 1) with the content of polyamino polyether tetramethylene Phosphonic Acid (PAPEMP) being 10%, then the four same groups of solutions are respectively subjected to standing, 300W power ultrasound, magneton mechanical stirring at the speed of 400r/min and nitrogen introduction at the speed of 1L/min and 10L/min, the separation time is recorded when the negative electrode material is completely stripped, no gas is generated in the separation process, and the Cu content in the electrode material is measured through the test of an inductively coupled plasma spectrum generator. The nitrogen gas was introduced at a rate of 10L/min, and the obtained negative electrode material and copper foil are shown in FIG. 3, and the final results are shown in the following table:
| processing method | Reaction time | Cu content of electrode material |
| Standing still | 53min28s | 0.0168％ |
| Ultrasound | 24min 56s | 3.4103％ |
| Mechanical stirring | 29min 13s | 2.3677％ |
| Aeration at a rate of 1L/min | 23min 39s | 0.0102％ |
| Aeration at 10L/min | 16min 44s | 0.0136％ |
It can be obviously seen that compared with standing separation, ultrasonic, mechanical stirring and gas introduction can well accelerate separation, wherein the speed of accelerating separation by gas introduction is the fastest, the content of impurity Cu in the electrode material is the lowest, and no gas is generated in the separation reaction. As can be seen from fig. 3, the copper foil surface of the separation-promoting current collector is bright and clean, substantially no electrode material remains, and the recovery rate is high.
Example 4
Disassembling the retired battery, and separating out the battery with the compaction density of 0.5g/cm 3 The current collector is hard of copper foilAnd (2) soaking 100g of the negative electrode plate in 2L of aqueous solution, standing the four groups of solutions respectively, performing 300W power ultrasonic treatment, performing mechanical stirring on magnetons at a speed of 400r/min, introducing air at a speed of 0.25L/min and at a speed of 2.5L/min, recording separation time when the negative electrode material is completely stripped, and measuring the Cu content in the electrode material by testing through an inductively coupled plasma spectrum generator. As shown in fig. 4, air was introduced at a rate of 2.5L/min, and the negative electrode material was completely peeled off from the current collector after 10 minutes. The final results are shown in the following table:
compared with standing separation, ultrasonic separation, mechanical stirring and gas introduction can accelerate separation well, wherein the gas introduction accelerates the separation at the fastest speed, the impurity Cu content in the electrode material is the lowest, and no gas is generated in the separation reaction.
Comparative example 1
Disassembling the retired battery, and separating out the electrode material LiNi 0.5 Co 0.2 Mn 0.3 O 2 The current collector is aluminum foil, and the compaction density is 4.0g/cm 3 The positive electrode sheet of (1). 100g of positive plate is soaked in 1L of 0.1mol/L NaOH aqueous solution, and then the same three groups of solution are respectively stood, subjected to 300W power ultrasound and mechanically stirred at a magneton speed of 400 r/min. And recording the reaction time and the gas production rate of the reaction when the positive electrode material is completely stripped, wherein the gas production rate is hydrogen. And testing by an inductively coupled plasma spectrum generator to measure the Al content in the electrode material. The final results are shown in the following table:
| processing method | Reaction time | Amount of gas | Al content of electrode material | Volume ratio of hydrogen |
| Standing still | 7h 13min | 11.28L | 0.8329％ | 100％ |
| Ultrasound | 1h 14min | 11.24L | 3.5974％ | 100％ |
| Mechanical stirring | 1h 36min | 11.29L | 2.2864％ | 100％ |
Compared with the example 1, it is obvious that compared with the standing separation, the ultrasonic, mechanical stirring and gas introduction can accelerate the separation well, wherein the speed of the gas introduction accelerating the separation is the fastest, the content of the impurity Al in the electrode material is the lowest, the hydrogen content is greatly diluted to a safe level, and the explosion can not occur even if the electrode material is exposed in the air (and the 100% H shown in the table above) 2 If exposed to air by accident, an explosion may still occur).
Comparative example 2
Disassembling the retired battery, and separating out the electrode material LiFePO 4 The current collector is aluminum foil, and the compaction density is 3.5g/cm 3 The positive electrode sheet of (1). 150g of positive plate is soaked in 1L of 0.1mol/L citric acid solution, and the three groups of solutions are respectively subjected to standing, 300W power ultrasonic and magneton 400r/min speed mechanical stirring. And recording the reaction time and the gas production rate of the reaction when the positive electrode material is completely stripped, wherein the gas production rate is hydrogen. And testing by an inductively coupled plasma spectrum generator to measure the Al content in the electrode material. The final results are shown in the following table:
| processing method | Reaction time | Amount of gas | Al content of electrode material | Volume ratio of hydrogen |
| Standing still | 6h 52min | 16.13L | 0.7933％ | 100％ |
| Ultrasound | 1h 23min | 9.64L | 3.6327％ | 100％ |
| Mechanical stirring | 1h 47min | 10.71L | 2.3116％ | 100％ |
When the standing separation is adopted, the separation time is too long. By combining example 2 and comparative example 2, it can be seen that the three methods of ultrasound, mechanical agitation and aeration can effectively accelerate the separation. Wherein the aeration separation effect is best and the separation efficiency is highest. Fig. 5 is a graph of the separation effect of the three separation methods, and it can be clearly seen that electrode material remains on the current collectors after the separation by ultrasonic and mechanical agitation, and ventilation promotes the surface of the separated current collectors to be bright and clean, so that no electrode material remains basically, and the recovery rate is high.
The above embodiments are only examples, and the gas to be introduced may be a single-phase or multi-component gas mixture such as air, carbon dioxide, nitrogen, helium, neon, argon, krypton, xenon, and radon. The types of the retired batteries can be flexibly adjusted; the active material in the battery pole piece can be, for example, ternary nickel cobalt manganese material, ternary nickel cobalt aluminum material, lithium iron phosphate material, lithium cobaltate material, cobalt-free high nickel layered material (such as Li [ Ni ] 0.9 Mn 0.1 ]O 2 Etc.), lithium rich positive electrode materials (e.g., Li) 1.3 Nb 0.3 Mn 0.4 O 2 Etc.), a lithium manganate material, a lithium nickel manganate material, a lithium titanate material, a titanium niobate material, a silicon-based material, or graphite. The method of the present invention is suitable for liquid phase separation systems, for example, the solution system for soaking the positive electrode plate can be a liquid reagent (such as N-methylpyrrolidone NMP, dimethylacetamide DMAC), N-dimethylformamide DMF, triethyl phosphate TEP, dimethyl sulfoxide DMSO) capable of dissolving the binder between the electrode material and the current collector based on the similar phase dissolution principle, or can be a liquid reagent capable of reacting with the surface of the current collector to achieve electric connectionA liquid reagent (e.g., hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, oxalic acid, citric acid, malic acid, tartaric acid, oxalic acid, phytic acid, lactic acid, lithium hydroxide, sodium hydroxide, or potassium hydroxide solution) for the purpose of separating the electrode material from the current collector; the solution system for soaking the negative electrode plate can also be a liquid reagent (such as water and poly-amino poly-ether tetramethylene Phosphonic Acid (PAPEMP)) which is based on the similar compatibility principle and can dissolve the binder between the electrode material and the current collector, or can be a liquid reagent (such as hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, oxalic acid, citric acid, malic acid, tartaric acid, oxalic acid, phytic acid or lactic acid solution) which can react with the surface of the current collector to achieve the purpose of separating the electrode material from the current collector.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A method of accelerating the separation of a battery electrode material and a current collector, comprising the steps of:
(1) disassembling the retired battery: disassembling a positive pole piece or a negative pole piece from a retired lithium battery; the pole piece comprises a current collector and an electrode material layer closely attached to the current collector;
(2) material treatment: soaking the pole piece in a specific solution, wherein the specific solution can separate the electrode material layer from the current collector;
when the pole piece is a positive pole piece, the solution is N-methyl pyrrolidone (NMP), Dimethylacetamide (DMAC), N-Dimethylformamide (DMF), triethyl phosphate (TEP), dimethyl sulfoxide (DMSO), hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, oxalic acid, citric acid, malic acid, tartaric acid, oxalic acid, phytic acid, lactic acid, lithium hydroxide, sodium hydroxide or potassium hydroxide solution;
when the pole piece is a negative pole piece, the solution is water, polyamino polyether tetramethylene Phosphonic Acid (PAPEMP), hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, oxalic acid, citric acid, malic acid, tartaric acid, oxalic acid, phytic acid or lactic acid solution;
(3) material separation: and introducing gas into the solution to accelerate the separation of the electrode material layer and the current collector.
2. The method according to claim 1, wherein in step (3), the gas is introduced at a rate in the range of 0.125 to 30 liters of gas/(liter of solution per minute), preferably 2.5 to 25 liters of gas/(liter of solution per minute), and more preferably 15 to 20 liters of gas/(liter of solution per minute).
3. The method of claim 1, wherein in step (3), the gas is at least one of air, carbon dioxide, nitrogen, helium, neon, argon, krypton, xenon, and radon.
4. The method according to claim 1, wherein in the step (1), the current collector is an aluminum current collector, a copper current collector, a nickel current collector, a titanium current collector or a stainless steel current collector;
the compacted density of the electrode material layer is 0.5-4.0g/cm 3 The conductive paste consists of an active substance, a binder and a conductive agent.
5. The method of claim 4, wherein the active material is selected from the group consisting of a ternary nickel cobalt manganese material, a ternary nickel cobalt aluminum material, a lithium iron phosphate material, a lithium cobaltate material, a cobalt-free nickel layered material, a lithium rich positive electrode material, a lithium manganate material, a lithium nickel manganate material, a lithium titanate material, a titanium niobate material, a silicon based material, and graphite.
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