CN116885327A - Recycling process of lithium ion battery anode material - Google Patents
Recycling process of lithium ion battery anode material Download PDFInfo
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- CN116885327A CN116885327A CN202311037672.5A CN202311037672A CN116885327A CN 116885327 A CN116885327 A CN 116885327A CN 202311037672 A CN202311037672 A CN 202311037672A CN 116885327 A CN116885327 A CN 116885327A
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- 238000000034 method Methods 0.000 title claims abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 23
- 238000004064 recycling Methods 0.000 title claims abstract description 15
- 239000010405 anode material Substances 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 40
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 29
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011888 foil Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000004804 winding Methods 0.000 claims abstract description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 9
- 238000012216 screening Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910001386 lithium phosphate Inorganic materials 0.000 claims description 4
- 230000001502 supplementing effect Effects 0.000 claims description 4
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 claims description 4
- ILYSAKHOYBPSPC-UHFFFAOYSA-N 2-phenylbenzoic acid Chemical compound OC(=O)C1=CC=CC=C1C1=CC=CC=C1 ILYSAKHOYBPSPC-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 3
- SNKMVYBWZDHJHE-UHFFFAOYSA-M lithium;dihydrogen phosphate Chemical compound [Li+].OP(O)([O-])=O SNKMVYBWZDHJHE-UHFFFAOYSA-M 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- SYBYTAAJFKOIEJ-UHFFFAOYSA-N 3-Methylbutan-2-one Chemical compound CC(C)C(C)=O SYBYTAAJFKOIEJ-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 2
- 239000010406 cathode material Substances 0.000 claims 6
- 239000000203 mixture Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
Landscapes
- Engineering & Computer Science (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)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a recycling process of a lithium ion battery anode material, which comprises the following steps: the method comprises the steps of disassembling a module battery into a single battery, discharging, then disassembling the battery, separating positive and negative pole pieces of a disassembled winding core, soaking the separated pole pieces in an organic solution respectively to realize preliminary separation of foil materials and the pole pieces, selecting a positive pole piece, cutting the positive pole piece into small pieces, crushing the small pieces into powder, sieving and removing impurities to obtain raw material powder, and treating the raw material powder of a lithium source by using a physical sintering method to obtain qualified lithium source reclaimed materials. According to the invention, impurities such as moisture, free carbon and the like are removed by high-temperature baking, the organic adhesive between the aluminum foil and the pole piece is evaporated at high temperature, so that the aluminum foil and the pole piece are dispersed, and then the lithium source plate material with large mass and smaller granularity is screened out by utilizing the vibrating screen, so that the lithium source plate material is separated from the aluminum foil with lighter weight and larger volume. The high-temperature baking also causes the surface of the aluminum foil to expand, the density is low, and the sieving is also facilitated.
Description
Technical Field
The invention relates to the technical field of battery recovery, in particular to a recovery process of a lithium ion battery anode material.
Background
Over the last decades, lithium ion batteries have been used in large numbers in the automotive propulsion field, as these batteries can provide reliable service for many years and are expected to be usable for about 10 years under normal driving conditions. These lithium ion batteries can then be used for utility energy storage until the end of their useful life.
Environmental problems caused by the disposal of lithium ion batteries have attracted public general attention. The need to extract raw materials from a limited supply in the earth is reduced if the available materials can be recovered from the used batteries. In addition, if the used lithium ion battery is recyclable, significant negative environmental impact caused by mining and processing of ore can be avoided.
In the year 2016, 12, the industrial information department issues a temporary method for recycling and managing the power storage battery of the new energy automobile, which makes sure that an automobile production enterprise bears the main responsibility of recycling the power storage battery, requires a producer to take responsibility in the whole life cycle of the product, connects production and recycling in series, and improves the recycling rate. The european union committee promulgates new european batteries for the year 2020, 12, aiming to ensure that batteries put into the european union market have sustainability and safety throughout the life cycle. Under a large environment, various battery manufacturers such as Ningde times, biedi, middle-navigation lithium batteries, guozhen high-power and ultra-power are actively distributing lithium batteries for recycling.
The methods for recycling lithium battery materials on the market generally comprise the following steps: physical methods (including crushing and sorting processes), chemical methods (including pyrometallurgical and wet recovery processes), biological metallurgical techniques, and the like. These methods are relatively effective for recovering lithium, cobalt, phosphorus, iron, etc. materials in lithium ion batteries, but they also have a common problem in that the purity of the recovered materials is insufficient. Because the pole piece of the lithium ion battery needs to be matched with the foil to realize good functions, and the aluminum foil is the current foil with highest neutral price ratio, most of pole pieces of the lithium ion battery are tightly adhered with the aluminum foil. The current recovery method is difficult to effectively separate the pole piece from the foil, so that the recovery material contains higher aluminum impurities, the purity of the lithium ion material is influenced, and the subsequent reutilization is prevented.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a recovery process of a lithium ion battery anode material, which solves the problem that the recovery method of the lithium ion battery anode material in the prior art is difficult to separate a pole piece from a foil material, so that aluminum impurities in the recovered material are higher.
According to an embodiment of the invention, the recovery process of the positive electrode material of the lithium ion battery comprises the following steps:
s1, disassembling a module battery into single batteries, and then screening the appearance to select the battery with serious obvious damage as the battery to be disassembled; grading the rest batteries after charge and discharge aging treatment, and carrying out degradation treatment on part of the batteries which can be degraded according to the battery grade, wherein part of the batteries which cannot be degraded are used as the batteries to be disassembled;
s2, discharging the battery to be disassembled to be less than or equal to 2.5V, disassembling the battery, separating positive and negative pole pieces of the disassembled winding core, soaking the separated pole pieces respectively by using an organic solution to realize preliminary separation of the foil and the pole pieces, and simultaneously partially eliminating electrolyte and adhesive;
s3, selecting positive pole pieces, classifying according to the types of positive pole materials, cutting each classified pole piece into small pieces, crushing the small pieces into powder, sieving and removing impurities to obtain raw material powder, and treating the raw material powder of a lithium source by using a physical sintering method to obtain qualified lithium source reclaimed materials.
Further, for the raw material powder obtained in the step S3, the Li content is detected first, and if the Li content is less than or equal to 4.0%, a lithium supplementing agent is added and mixed uniformly, so that the Li content is more than or equal to 4.0%.
Further, for the raw material powder with the Li content being detected, the Al content is detected, and if the Al content is less than or equal to 350ppm, a physical sintering method is directly adopted for treatment; if the Al content is 350-600 ppm, adding the lithium source material corresponding to the group of material types, wherein the ratio of the raw material powder to the added material is 8:2-3:7, and then performing physical sintering treatment.
Further, the processing steps of the physical sintering method are as follows: baking raw material powder by an atmosphere roller furnace, removing moisture, adhesive, free carbon and other impurities in the material, separating the pole piece foil and the powder by using a 50-mesh screen through vibration of high frequency in a dehumidifying environment, recovering and packaging aluminum foil, grading the powder by using a 100-mesh vibration screen, and refining and mixing after qualified products are separated.
Further, the baking temperature in the atmosphere roller hearth furnace is 400-800 ℃, the time is 3-10 h, and the final discharging temperature is less than or equal to 60 ℃.
Preferably, the organic solution comprises one or more of phenylbenzoic acid, N-methylpyrrolidone, acetone, ethanol, liquid ammonia, methyl butanone, isopropanol, phenol, propylene oxide.
Preferably, the lithium supplementing agent comprises one or more of lithium phosphate, lithium carbonate, lithium hydroxide, lithium dihydrogen phosphate or lithium sulfate and lithium oxide.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, impurities such as moisture, free carbon and the like are removed through high-temperature baking, organic adhesive between the aluminum foil and the pole piece is evaporated at high temperature, so that the aluminum foil and the pole piece are dispersed, and then a lithium source plate material with large mass and smaller granularity is screened out by utilizing a vibrating screen, so that the lithium source plate material is separated from the aluminum foil with lighter volume and larger size;
2. the high-temperature baking in the invention can also cause the surface of the aluminum foil with small particles to expand and crack, so that the surface morphology of the aluminum foil becomes more irregular, therefore, the aluminum foil can be more easily peeled off from the closely adhered pole pieces, and the density of the aluminum foil after expansion is low, thereby being more beneficial to screening.
Detailed Description
The technical scheme of the invention is further described below by referring to examples.
The waste lithium ion batteries used in the embodiment of the invention all adopt the Ningde 280Ah square aluminum shell battery cells.
Because the steps S1 and S2 are substantially identical in the process of the present invention, the following examples employ the following steps:
s1, disassembling a module battery into single batteries, and then screening the appearance to select the battery with serious obvious damage as the battery to be disassembled; grading the rest batteries after charge and discharge aging treatment, and carrying out degradation treatment on part of the batteries which can be degraded according to the battery grade, wherein part of the batteries which cannot be degraded are used as the batteries to be disassembled;
s2, discharging the battery to be disassembled to be less than or equal to 2.5V, disassembling the battery, separating positive and negative pole pieces of the disassembled winding core, and then soaking the separated pole pieces respectively through organic solutions, wherein the organic solutions are phenylbenzoic acid, so that the preliminary separation of foil and the pole pieces is realized, and meanwhile, the electrolyte and the adhesive are partially eliminated.
The positive pole piece separated through the steps is prepared into a final lithium source reclaimed material by adopting different S3 steps according to different embodiments.
Example 1:
and (3) taking 20kg of the positive electrode plate material obtained in the previous step, firstly cutting into small pieces, grinding and crushing into powder, and then passing through a 50-200-mesh multi-stage vibrating screen, wherein the difference between each vibrating screen and the other vibrating screen is 50 meshes, screening lithium source material powder with different fineness grades, and then screening powder materials with different grades to remove impurities to obtain raw material powder. And testing the content of Li and Al in the raw material powder, wherein the content of Li is detected to be 3.6 percent, and the content of Al is detected to be 278ppm, and then 1.0 percent of lithium phosphate is added for uniform mixing, so that the content of Li reaches 4.6 percent.
And (3) baking the raw material powder by an atmosphere roller hearth furnace, wherein the specific baking temperature is 500 ℃, the time is 10 hours, and the final discharging temperature is 52 ℃. Removing water, adhesive, free carbon and other impurities in the material, sieving with a 100-mesh sieve in a dehumidification environment, refining and mixing, testing the content of Li to be 4.0% and the content of Al to be 278ppm, and obtaining the required lithium source reclaimed material.
Example 2:
and (3) taking 20kg of the positive electrode plate material obtained in the previous step, firstly cutting into small pieces, grinding and crushing into powder, and then passing through a 50-200-mesh multi-stage vibrating screen, wherein the difference between each vibrating screen and the other vibrating screen is 50 meshes, screening lithium source material powder with different fineness grades, and then screening powder materials with different grades to remove impurities to obtain raw material powder. And testing the content of Li and Al in the raw material powder, firstly detecting that the content of Li is 4.0 percent, then detecting that the content of Al is 325ppm, adding 0.3 percent of lithium carbonate and 0.3 percent of lithium hydroxide, and uniformly mixing.
And (3) baking the raw material powder by an atmosphere roller hearth furnace, wherein the specific baking temperature is 800 ℃, the time is 3 hours, and the final discharging temperature is 60 ℃. Removing water, adhesive, free carbon and other impurities in the material, sieving with a 300-mesh sieve in a dehumidifying environment, refining and mixing, testing the content of Li to be 4.6% and the content of Al to be 325ppm, and obtaining the required lithium source reclaimed material.
Example 3:
taking 20kg of the positive electrode plate material obtained in the previous step, firstly cutting into small pieces, grinding and crushing the small pieces into powder, then sieving the powder by a multi-stage vibrating sieve with 50-200 meshes, wherein the difference between each vibrating sieve is 50 meshes, sieving lithium source material powder with different fineness grades, sieving powder materials with different grades respectively to remove impurities to obtain raw material powder, testing the Li content and the Al content of the raw material powder to be 3.5%, detecting the Al content to be 460ppm, and adding 0.4% of lithium phosphate, 0.4% of lithium dihydrogen phosphate and 0.4% of lithium oxide to be uniformly mixed.
And (3) baking the raw material powder by an atmosphere roller hearth furnace, wherein the specific baking temperature is 650 ℃, the time is 6 hours, and the final discharging temperature is 44 ℃. Removing water, adhesive, free carbon and other impurities in the material, sieving with a 200-mesh sieve in a dehumidifying environment, refining and mixing, testing the content of Li to be 4.3 percent and the content of Al to be 460ppm, and obtaining the required lithium source reclaimed material.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (7)
1. The recovery process of the lithium ion battery anode material is characterized by comprising the following steps of: the method comprises the following steps:
s1, disassembling a module battery into single batteries, and then screening the appearance to select the battery with serious obvious damage as the battery to be disassembled; grading the rest batteries after charge and discharge aging treatment, and carrying out degradation treatment on part of the batteries which can be degraded according to the battery grade, wherein part of the batteries which cannot be degraded are used as the batteries to be disassembled;
s2, discharging the battery to be disassembled to be less than or equal to 2.5V, disassembling the battery, separating positive and negative pole pieces of the disassembled winding core, soaking the separated pole pieces respectively by using an organic solution to realize preliminary separation of the foil and the pole pieces, and simultaneously partially eliminating electrolyte and adhesive;
s3, selecting positive pole pieces, classifying according to the types of positive pole materials, cutting each classified pole piece into small pieces, crushing the small pieces into powder, sieving and removing impurities to obtain raw material powder, and treating the raw material powder of a lithium source by using a physical sintering method to obtain qualified lithium source reclaimed materials.
2. The process for recycling lithium ion battery cathode material according to claim 1, wherein: and (3) detecting the Li content of the raw material powder obtained in the step S3, and adding a lithium supplementing agent to mix uniformly if the Li content is less than or equal to 4.0%, so that the Li content is more than or equal to 4.0%.
3. The process for recycling lithium ion battery cathode material according to claim 2, wherein: detecting the content of Al in the raw material powder after the content of Li is detected, and if the content of Al is less than or equal to 350ppm, directly adopting a physical sintering method for treatment; if the Al content is 350-600 ppm, adding the lithium source material corresponding to the group of material types, wherein the ratio of the raw material powder to the added material is 8:2-3:7, and then performing physical sintering treatment.
4. The process for recycling lithium ion battery cathode material according to claim 1, wherein the physical sintering method comprises the following processing steps: baking raw material powder by an atmosphere roller furnace, removing moisture, adhesive, free carbon and other impurities in the material, separating the pole piece foil and the powder by using a 50-mesh screen through vibration of high frequency in a dehumidifying environment, recovering and packaging aluminum foil, grading the powder by using a 100-mesh vibration screen, and refining and mixing after qualified products are separated.
5. The process for recycling lithium ion battery cathode material according to claim 4, wherein: the baking temperature in the atmosphere roller hearth furnace is 400-800 ℃, the time is 3-10 h, and the final discharging temperature is less than or equal to 60 ℃.
6. The process for recycling lithium ion battery cathode material according to claim 1, wherein: the organic solution comprises one or more of phenylbenzoic acid, N-methyl pyrrolidone, acetone, ethanol, liquid ammonia, methyl butanone, isopropanol, phenol and propylene oxide.
7. The process for recycling lithium ion battery cathode material according to claim 2, wherein: the lithium supplementing agent comprises one or a mixture of more of lithium phosphate, lithium carbonate, lithium hydroxide, lithium dihydrogen phosphate or lithium sulfate and lithium oxide.
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