CN112939096A - Direct repairing method for ternary cathode material of waste lithium ion battery - Google Patents
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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Abstract
The invention discloses a direct repair method of a ternary cathode material of a waste lithium ion battery, and belongs to the technical field of solid phase regeneration of the cathode material of the waste lithium ion battery. The invention solves the problem of complicated separation and purification operations in the traditional pyrogenic process and wet process recovery process of the ternary cathode material of the lithium ion battery. The method for directly repairing the ternary cathode material by using the high-temperature solid-phase sintering method has the advantages of simplicity and high efficiency, improves the utilization rate of the material, reduces the recovery cost, successfully reduces Li-Ni mixed discharge caused by circulation, repairs the damaged layered crystal structure, and has the characteristics of high discharge specific capacity, good cycle performance and the like. In addition, the method provided by the invention has the advantages of simplicity, easiness in implementation, good repeatability, low cost and high yield, and has good large-scale application potential.
Description
Technical Field
The invention relates to a direct repair method of a ternary cathode material of a waste lithium ion battery, belonging to the technical field of solid phase regeneration of the cathode material of the waste lithium ion battery.
Background
The lithium ion battery is used as a preferred technology of a 21 st century battery system, and has the outstanding advantages of high energy density, long cycle life, environmental friendliness and the like. In addition, lithium ion batteries also show unlimited potential in electrochemical energy storage and conversion, driving a new revolution in portable electronic devices. With the rapid development of electric vehicles, lithium ion batteries are also becoming the most widely used power battery technology in electric vehicles. The service life of the ternary lithium ion battery is 8-10 years, and when the service life of the battery is over, if the battery cannot be used in a gradient manner and is not recycled, millions of tons of waste batteries are generated, so that the environment is seriously polluted and resources are greatly wasted.
At present, the main recycling method of the waste ternary lithium ion battery in industry is a pyrogenic process and a wet process. The pyrometallurgy is to recover battery materials by a heat treatment mode, and the technical process is simpler, but has the problems of low recovery rate, easy environmental pollution and the like; the wet method realizes the recycling of battery materials through low-temperature leaching, purification and separation, but the recycling process is complex. Therefore, it is necessary to provide a method for directly repairing a ternary cathode material of a waste lithium ion battery to solve the above technical problems.
Disclosure of Invention
The invention provides a direct repair method of a ternary cathode material of a waste lithium ion battery, aiming at solving the technical problems.
The technical scheme of the invention is as follows:
a direct repair method for a ternary positive electrode material of a waste lithium ion battery comprises the following steps:
disassembling a waste lithium ion battery under the protection of inert gas, and removing a shell, positive and negative terminals, a sealing ring and a cover plate;
separating the positive plate from the negative plate, soaking the positive plate by using dimethyl carbonate to remove electrolyte, soaking the positive plate by using an organic solvent for 2-4 hours at the temperature of 100 ℃, removing the binder, stripping out the positive material, centrifuging and drying to obtain a waste ternary positive material;
step three, fully washing the waste ternary positive electrode material obtained in the step two for 4-8 hours by using an organic solvent, then washing for 1-2 times by using ethanol, centrifuging and drying to obtain a ternary material to be repaired;
grinding the ternary material to be repaired obtained in the step three, and then screening and removing impurities by using 80-mesh, 200-mesh and 400-mesh sieves in sequence to obtain ternary powder to be repaired with uniform particle size;
analyzing the components of the ternary powder to be repaired after the treatment of the fourth step to determine the contents of nickel, cobalt, manganese and lithium elements;
supplementing elements missing from the ternary powder to be repaired according to a proportion, uniformly mixing, and then carrying out high-temperature calcination treatment under different atmosphere conditions;
and step seven, after the high-temperature calcination treatment is finished, cooling to room temperature, removing black solids, and grinding to obtain the repaired ternary cathode material.
Further, the anode ternary material of the waste lithium ion battery is a waste NCM523 or NCM622 material which is recycled for about 2000 times.
Further, the organic solvent in the second step and the third step is N-methyl pyrrolidone.
Further, in the sixth step, the ratio of lithium to the total molar amount of nickel, cobalt and manganese is 1.05: 1 ratio with LiOH.
Further, ball milling is adopted in the sixth step for 4-6 hours, so that the ternary powder to be repaired and the supplementary material are uniformly mixed.
Further, the high-temperature calcination conditions in the sixth step are as follows: the temperature is 500 ℃ and 800 ℃, and the time is 12-20 h.
Further, the high-temperature calcination process in the sixth step is as follows: keeping the temperature at 500 ℃ for 4h, and then heating to 800 ℃ and keeping the temperature for 16 h.
The invention has the following beneficial effects: the method for directly repairing the ternary cathode material by using the high-temperature solid-phase sintering method has the advantages of simplicity and high efficiency, avoids the complex separation and purification operations in the traditional pyrometallurgical and wet-process recovery processes, improves the utilization rate of the material, and reduces the recovery cost. The method provided by the invention successfully reduces Li-Ni mixed discharge caused by circulation, repairs the damaged layered crystal structure, and the repaired ternary cathode material has the characteristics of high specific discharge capacity, good circulation performance and the like. In addition, the method provided by the invention has the advantages of simplicity, easiness in implementation, good repeatability, low cost, high yield and the like, and has good large-scale application potential.
Drawings
FIG. 1 is an XRD pattern of the NCM523 material of example 1 before and after repair;
FIG. 2 is an XRD pattern of the NCM622 material before and after repair in example 2;
FIG. 3 is a Raman spectrum of the NCM523 material of example 1 before and after repair;
FIG. 4 is a Raman spectrum of the NCM622 material of example 2 before and after repair;
FIG. 5 is a scanning electron micrograph of the NCM523 material of example 1 after repair;
FIG. 6 is a scanning electron micrograph of the NCM622 material of example 2 after repair;
FIG. 7 is a graph of the discharge before and after repair of the NCM523 material of example 1;
FIG. 8 is a graph of the discharge before and after repair of the NCM622 material of example 2;
FIG. 9 is a graph of galvanostatic cycling performance before and after repair of the NCM523 material of example 1;
FIG. 10 is a plot of galvanostatic cycling performance before and after repair of the NCM622 material of example 2;
fig. 11 is a graph of the rate capability of the NCM523 repaired in example 1 and the NCM622 material repaired in example 2.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1: repairing waste NCM523 material lithium ion battery
Firstly, disassembling the waste NCM523 battery under the protection of inert gas, and removing a shell, a positive terminal, a negative terminal, a sealing ring and a cover plate;
separating the positive and negative plates, and soaking the positive and negative plates by using DMC to remove the electrolyte; soaking the positive plate for 2-4h at the temperature of 100 ℃ by using N-methyl pyrrolidone, removing the binder, stripping out the positive material, centrifuging and drying to obtain a waste NCM523 positive material;
thirdly, fully washing the waste NCM523 positive electrode material obtained in the second step for 5 hours by using N-methylpyrrolidone, then washing for 2 times by using ethanol, and drying after centrifugation to obtain an NCM523 material to be repaired;
grinding the NCM523 material to be repaired for 30min, and screening by using sieves of 80 meshes, 200 meshes and 400 meshes in sequence to remove impurities to obtain ternary powder to be repaired, wherein the ternary powder has uniform particle size;
dissolving the waste NCM523 material into aqua regia for component analysis to determine the content of nickel (Ni), cobalt (Co), manganese (Mn) and lithium (Li);
and sixthly, the ratio of lithium to the total molar amount of nickel, cobalt and manganese is 1.05: 1, supplementing LiOH, ball-milling for 6 hours, mixing, and then calcining at high temperature in an oxygen atmosphere under the reaction conditions that the temperature is 500 ℃, the temperature is kept for 4 hours, and the temperature is increased to 800 ℃, and the temperature is kept for 16 hours;
and seventhly, after the reaction is finished, cooling the tubular furnace to room temperature, removing black solids, grinding and screening to obtain the repaired NCM523 positive electrode material.
The NCM523 positive electrode materials before and after repair were characterized and compared, and the results are shown in fig. 1, 3, 5, 7, 9 and 11: fig. 1 is an XRD contrast before and after the NCM523 material repaired by the present example, fig. 3 is a raman spectrum before and after the NCM523 material is repaired, and fig. 1 and fig. 3 show that the layered crystal structure of the repaired NCM523 material is obviously restored and Li-Ni misclassification is obviously improved. Fig. 5 shows the morphology of the repaired material, and it can be seen from fig. 7 that the first-cycle specific discharge capacity of the lithium ion battery prepared from the repaired NCM523 material is increased from 126.704mAh/g to 170.964mAh/g at a current density of 0.1C, and the capacity of the lithium ion battery prepared from the repaired NCM523 material is maintained at 144.99mAh/g at a current density of 1C for 100 cycles. It can be seen from fig. 11 that the repaired NCM523 material exhibits good rate capability.
Example 2: repairing waste NCM622 material lithium ion battery
Firstly, disassembling the waste NCM622 battery under the protection of inert gas, and removing a shell, positive and negative terminals, a sealing ring and a cover plate
Separating the positive and negative plates, and soaking the positive and negative plates by using DMC to remove the electrolyte; soaking the positive plate for 2-4h at the temperature of 100 ℃ by using N-methyl pyrrolidone, removing the binder, stripping out the positive material, centrifuging and drying to obtain a waste NCM622 positive material;
thirdly, fully washing the waste NCM622 positive electrode material obtained in the second step for 5 hours by using an organic solvent, then washing for 2 times by using ethanol, centrifuging and drying to obtain an NCM622 material to be repaired;
grinding the NCM622 material to be repaired for 30min, and screening by using sieves of 80 meshes, 200 meshes and 400 meshes in sequence to remove impurities to obtain ternary powder to be repaired, wherein the ternary powder has uniform particle size;
dissolving the waste NCM622 material into aqua regia for component analysis, and determining the content of nickel (Ni), cobalt (Co), manganese (Mn) and lithium (Li);
and sixthly, the ratio of lithium to the total molar amount of nickel, cobalt and manganese is 1.05: 1, supplementing LiOH, ball-milling for 6 hours, mixing, and then calcining at high temperature in an oxygen atmosphere under the reaction conditions that the temperature is 500 ℃, the temperature is kept for 4 hours, and the temperature is increased to 800 ℃, and the temperature is kept for 16 hours;
and seventhly, after the reaction is finished, cooling the tubular furnace to room temperature, removing black solids, grinding and screening to obtain the repaired NCM622 positive electrode material.
The NCM622 positive electrode materials before and after repair were characterized and compared, and the results are shown in fig. 2, 4, 6, 8, 10 and 11: fig. 2 is an XRD contrast before and after the NCM622 material repaired by the present example, fig. 4 is a raman spectrum before and after the NCM622 material is repaired, and fig. 2 and fig. 4 show that the layered crystal structure of the repaired NCM622 material is significantly restored and Li-Ni misclassification is significantly improved. Figure 6 shows the morphology of the repaired material. FIG. 8 shows that the specific discharge capacity of the lithium ion battery prepared from the repaired NCM622 material at the first circle of the lithium ion battery at the current density of 0.1C is improved from 96.72mAh/g to 198.81 mAh/g. FIG. 10 shows that the capacity of the lithium ion battery made of the repaired NCM622 material is maintained at 128.58mAh/g after 100 cycles under the current density of 1C. It can be seen from fig. 11 that the repaired NCM622 material showed good rate capability.
Example 3:
this example differs from example 1 only in that: the method for mixing the lithium source and the material in the sixth step is manual grinding for 30min-60min, and the rest of the operation steps are the same as those in the example 1.
Example 4:
this example differs from example 2 only in that: the method for mixing the lithium source and the material in the sixth step is manual grinding for 30min-60min, and the rest of the operation steps are the same as those in the example 2.
Example 5:
this example differs from example 1 only in that: the atmosphere for calcination in the sixth step was air, and the remaining operation steps were the same as in example 1.
Example 6:
this example differs from example 2 only in that: the atmosphere for calcination in the sixth step was air, and the remaining operation steps were the same as in example 2.
Example 7:
this example differs from example 1 only in that: in the sixth step, according to the total molar weight ratio of lithium to nickel, cobalt and manganese, 1.05: 1 ratio of supplemental Li2CO3The rest of the operation steps and implementationExample 1 is the same.
Example 8:
this example differs from example 2 only in that: in the sixth step, according to the total molar weight ratio of lithium to nickel, cobalt and manganese, 1.05: 1 ratio of supplemental Li2CO3The remaining operation steps are the same as in example 2.
Claims (8)
1. A direct repair method for a ternary positive electrode material of a waste lithium ion battery is characterized by comprising the following steps:
disassembling a waste lithium ion battery under the protection of inert gas, and removing a shell, positive and negative terminals, a sealing ring and a cover plate;
separating the positive and negative plates, and soaking by using dimethyl carbonate to remove the electrolyte; then soaking the positive plate for 2-4h at 100 ℃ by using an organic solvent, removing the binder, stripping out the positive material, centrifuging and drying to obtain a waste ternary positive material;
step three, fully washing the waste ternary positive electrode material obtained in the step two for 4-8 hours by using an organic solvent, then washing for 1-2 times by using ethanol, centrifuging and drying to obtain a ternary material to be repaired;
grinding the ternary material to be repaired obtained in the step three, and then screening and removing impurities by using 80-mesh, 200-mesh and 400-mesh sieves in sequence to obtain ternary powder to be repaired with uniform particle size;
analyzing the components of the ternary powder to be repaired after the treatment of the fourth step to determine the contents of nickel, cobalt, manganese and lithium elements;
supplementing elements missing from the ternary powder to be repaired according to a proportion, uniformly mixing, and then carrying out high-temperature calcination treatment under different atmosphere conditions;
and step seven, after the high-temperature calcination treatment is finished, cooling to room temperature, removing black solids, and grinding to obtain the repaired ternary cathode material.
2. The direct repair method of the ternary positive electrode material of the waste lithium ion battery according to claim 1, wherein the ternary positive electrode material of the waste lithium ion battery is an NCM523 material or an NCM622 material.
3. The direct repair method of the ternary cathode material of the waste lithium ion battery according to claim 1, wherein the organic solvent in the second step and the third step is N-methylpyrrolidone.
4. The method for directly repairing the ternary cathode material of the waste lithium ion battery as claimed in claim 1, wherein the ratio of lithium to the total molar amount of nickel, cobalt and manganese in the sixth step is 1.05: 1 ratio with LiOH.
5. The direct repair method of the ternary cathode material of the waste lithium ion battery as claimed in claim 1, wherein in the sixth step, the ternary powder to be repaired and the supplementary material are uniformly mixed by ball milling for 4-6 hours.
6. The method for directly repairing the ternary cathode material of the waste lithium ion battery according to claim 1, wherein the atmosphere condition of the high-temperature calcination in the sixth step is an oxygen atmosphere.
7. The direct repair method of the ternary cathode material of the waste lithium ion battery according to claim 1, wherein the high-temperature calcination conditions in the sixth step are as follows: the temperature is 500 ℃ and 800 ℃, and the time is 12-20 h.
8. The direct repair method of the ternary cathode material of the waste lithium ion battery according to claim 1, wherein the high-temperature calcination process in the sixth step is as follows: keeping the temperature at 500 ℃ for 4h, and then heating to 800 ℃ and keeping the temperature for 16 h.
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| CN202110161218.5A CN112939096A (en) | 2021-02-05 | 2021-02-05 | Direct repairing method for ternary cathode material of waste lithium ion battery |
| PCT/CN2021/117439 WO2022166197A1 (en) | 2021-02-05 | 2021-09-09 | Direct repair method for waste lithium-ion battery ternary positive electrode material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636605A (en) * | 2021-07-07 | 2021-11-12 | 华中科技大学 | Physical repair method for completely-failed ternary positive electrode material under low-cost air condition |
| CN114204013A (en) * | 2021-12-15 | 2022-03-18 | 中南大学 | Direct repairing method for waste ternary lithium battery positive electrode material and ternary positive electrode material prepared by same |
| WO2022166197A1 (en) * | 2021-02-05 | 2022-08-11 | 哈尔滨工业大学 | Direct repair method for waste lithium-ion battery ternary positive electrode material |
| CN115432741A (en) * | 2022-09-23 | 2022-12-06 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Method for recycling waste lithium battery positive plate and battery |
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| CN115432699B (en) * | 2022-10-21 | 2023-07-11 | 湖南宸宇富基新能源科技有限公司 | Waste negative electrode-based regenerated graphite material and preparation and application thereof |
| CN115724474B (en) * | 2022-11-16 | 2023-12-08 | 清华大学深圳国际研究生院 | Repairing method of failed layered positive electrode material, positive electrode material and application of positive electrode material |
| CN117619859B (en) * | 2023-11-28 | 2024-05-24 | 吉奥环朋科技(扬州)有限公司 | Recycling recovery method of waste lithium ion power battery |
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| CN103915661A (en) * | 2013-01-09 | 2014-07-09 | 中国科学院过程工程研究所 | Method for direct recovery and restoration of lithium ion battery positive electrode material |
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| CN107706477A (en) * | 2017-08-31 | 2018-02-16 | 长沙佳纳锂业科技有限公司 | A kind of waste and old ternary anode material for lithium-ion batteries solid phase regeneration method |
| CN112054265A (en) * | 2020-09-30 | 2020-12-08 | 合肥国轩高科动力能源有限公司 | Method for recycling and reusing anode material of waste ternary lithium ion battery |
| CN112939096A (en) * | 2021-02-05 | 2021-06-11 | 哈尔滨工业大学 | Direct repairing method for ternary cathode material of waste lithium ion battery |
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- 2021-09-09 WO PCT/CN2021/117439 patent/WO2022166197A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103915661A (en) * | 2013-01-09 | 2014-07-09 | 中国科学院过程工程研究所 | Method for direct recovery and restoration of lithium ion battery positive electrode material |
| CN111977704A (en) * | 2020-07-27 | 2020-11-24 | 昆明理工大学 | Rapid regeneration method of waste ternary lithium ion battery anode material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022166197A1 (en) * | 2021-02-05 | 2022-08-11 | 哈尔滨工业大学 | Direct repair method for waste lithium-ion battery ternary positive electrode material |
| CN113636605A (en) * | 2021-07-07 | 2021-11-12 | 华中科技大学 | Physical repair method for completely-failed ternary positive electrode material under low-cost air condition |
| CN114204013A (en) * | 2021-12-15 | 2022-03-18 | 中南大学 | Direct repairing method for waste ternary lithium battery positive electrode material and ternary positive electrode material prepared by same |
| CN114204013B (en) * | 2021-12-15 | 2024-03-22 | 中南大学 | Direct repair method for waste ternary lithium battery positive electrode material and ternary positive electrode material prepared by same |
| CN115432741A (en) * | 2022-09-23 | 2022-12-06 | 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) | Method for recycling waste lithium battery positive plate and battery |
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| WO2022166197A1 (en) | 2022-08-11 |
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