GB2622974A - Method for efficiently recovering electrolyte of spent lithium-ion battery - Google Patents
Method for efficiently recovering electrolyte of spent lithium-ion battery Download PDFInfo
- Publication number
- GB2622974A GB2622974A GB2318911.1A GB202318911A GB2622974A GB 2622974 A GB2622974 A GB 2622974A GB 202318911 A GB202318911 A GB 202318911A GB 2622974 A GB2622974 A GB 2622974A
- Authority
- GB
- United Kingdom
- Prior art keywords
- electrolyte
- washing
- salt solution
- dimethyl carbonate
- ion battery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003792 electrolyte Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 25
- 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
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012266 salt solution Substances 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 19
- 239000012074 organic phase Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000008346 aqueous phase Substances 0.000 claims description 14
- 239000002699 waste material Substances 0.000 claims description 13
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 9
- 229910052744 lithium Inorganic materials 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 235000002639 sodium chloride Nutrition 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000013517 stratification Methods 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000047 product Substances 0.000 abstract description 10
- -1 carbonate ester Chemical class 0.000 abstract description 4
- 150000001768 cations Chemical class 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000005809 transesterification reaction Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 abstract 4
- 230000003197 catalytic effect Effects 0.000 abstract 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 9
- 239000012634 fragment Substances 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 5
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 4
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 4
- 239000012267 brine Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- 229910001290 LiPF6 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004064 recycling Methods 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Disclosed in the present invention is a method for efficiently recovering an electrolyte of a spent lithium-ion battery. The method comprises: crushing a spent lithium-ion battery to obtain a crushed material with an electrolyte; placing the crushed material in a salt solution and washing same; subjecting same to solid-liquid separation after washing to obtain a filtrate; leaving the filtrate to stand for layering to obtain a water phase and an organic phase; and mixing the organic phase with methanol, and distilling same under the conditions of a temperature of 60-100ºC and a vacuum degree of 10-80 kPa to obtain a crude dimethyl carbonate product. In the present invention, a salt solution is used for washing, and a solute which does not react with the electrolyte is dissolved in the salt solution, such that the density of the water phase is increased, the electrolyte and the water phase can be layered, and the electrolyte floats on the water phase, thereby realizing the layering of the electrolyte and water; and some metal cations in some salts enter the organic phase during the salt-solution washing process. A carbonate ester and methanol undergo a transesterification reaction under the catalytic action of the metal cations to generate dimethyl carbonate, the temperature is controlled to distil out a crude dimethyl carbonate product, and the carbonate ester product obtained after distillation has high purity and can be sold on the market.
Description
METHOD FOR EFFICIENTLY RECOVERING ELECTROLYTE OF SPENT
LITHIUM-ION BATTERY
TECHNICAL FIELD
The present disclosure relates to the field of recycling use of battery material, and in particular to a method for efficiently recovering waste lithium ion battery electrolyte.
BACKGROUND
The electrolyte in lithium-ion batteries accounts for about 17% of the battery, and is generally composed of carbonate organic solvents, such as ethylene carbonate (EC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), and propylene carbonate (PC), electrolyte lithium salt lithium hexafluorophosphate (LiPF6), additives, etc. During the use of lithium-ion batteries, some lithium ions would migrate into the electrolyte. The lithium content in the electrolyte of waste lithium-ion batteries can reach 7-14g/L, which is of high recovery value.
At present, the biggest problems for lithium ion electrolyte recovery are: 1. Electrolyte collection problem: the electrolyte in the lithium-ion battery is distributed among the positive electrode and negative electrode sheets and the diaphragm, and when the electrolyte is poured out of the battery, most of the electrolyte remains among the sheets and the diaphragm, and there is very little electrolyte that can be directly poured out of the battery; and there is no efficient or convenient collection method for the electrolyte in the current literature report. 2. Carbonate recovery problem: the carbonates reported in the current literature are all carbonate product that directly obtained by vacuum distillation, but the carbonate product obtained by vacuum distillation is not a single carbonate, but a mixture containing several carbonates, which is difficult to be reused or to be sold in the market.
SUMMARY
The present disclosure aims to solve at least one of the above-mentioned technical problems existing in the prior art. In view of this, the present disclosure provides a method for efficiently recovering waste lithium-ion battery electrolyte, which can collect the electrolyte economically and efficiently, and the distilled carbonate product is of high purity.
According to one aspect of the present disclosure, a method for efficiently recovering waste lithium-ion battery electrolyte is provided, comprising the following steps: Sl: Pulverizing a waste lithium ion battery to obtain a pulverized material with electrolyte, and washing the pulverized material in a salt solution, and performing solid-liquid separation after washing to obtain a filtrate; S2: Leaving the filtrate to stand for stratification to obtain an aqueous phase and an organic phase; and 53: Mixing the organic phase with methanol, and performing distillation under the conditions of a temperature of 60 °C to 100 °C and a vacuum degree of 10 kPa to 80 kPa, to obtain a crude product of dimethyl carbonate.
In some embodiments of the present disclosure, in step Si, the electrolyte comprises the 10 following components: lithium salt 1 mol/L to 2 mol/L, dimethyl carbonate 40 v% to 60 v%, ethyl methyl carbonate 5 v% to 25 v%, ethylene carbonate 10 v% to 25 v%, and propylene carbonate 0 to 10 v%. The lithium salt is lithium hexafluorophosphate.
In some embodiments of the present disclosure, in step S I, the salt solution is a neutral salt solution. Further, the salt in the salt solution is selected from one or more of sodium chloride, sodium sulfate, potassium chloride or potassium sulfate.
In some embodiments of the present disclosure, in step Si, the mass concentration of the salt solution is 5% to 25%, and the liquid-solid ratio of the salt solution to the pulverized material is (2-8): 1 L/kg.
In some embodiments of the present disclosure, in step S I, the washing is performed at a stirring speed of 60 r/min to 400 r/min.
In some embodiments of the present disclosure, in step Si, the duration of the washing is 5 min to 30 min. In some embodiments of the present disclosure, in step S2, the aqueous phase is returned to step S I for the washing.
In some embodiments of the present disclosure, in step S2, the duration of the standing for stratification is 0.5 h to 3 h In some embodiments of the present disclosure, in step S3, the volume ratio of the organic phase to methanol is 1: (0.2-1).
In some embodiments of the present disclosure, in step S3, the crude product of dimethyl carbonate is frozen crystallized, and then the obtained dimethyl carbonate crystal is heated and melted to obtain pure dimethyl carbonate. Further, the temperature of the frozen crystallization is -5 °C to 3 °C.
In some embodiments of the present disclosure, in step S3, before the distillation, the temperature is raised to 55 °C to 80 °C under a normal pressure to react for I to 3 hours.
In some embodiments of the present disclosure, in step S3, the distilled residual solution enters the next lithium extraction process. The distilled residual solution can also be separated and purified to obtain by-products, such as ethylene glycol and propylene glycol, by means of rectification.
According to a preferred embodiment of the present disclosure, it has at least the following beneficial effects: The main component of the electrolyte in the lithium-ion battery is carbonate. Several carbonates are insoluble in water and the density of carbonates is very close to that of water. When being mixed with water, the carbonate is neither soluble in water nor stratified with water, and forms small droplets in water and is difficult to separate from water. In the present disclosure, a certain concentration of salt solution is used for washing, and solutes that do not react with the electrolyte are dissolved in the salt solution, so that the density of the aqueous phase is increased, and the density of the electrolyte is lower than that of the aqueous phase, so that the electrolyte can be stratified with the aqueous phase and floated on the aqueous phase to achieve the stratification of the electrolyte and water. Moreover, some metal cations in some salts enter the organic phase during the washing process with the salt solution, and under the catalysis of the metal cations, the carbonate and methanol undergo transesterification to generate dimethyl carbonate. Part of the reaction formula is as follows: (CH20)2C0 (ethylene carbonate) + 2CH3OH (C1130)2C0 + HOCH2CH2OH, C4H603 (propylene carbonate) + 2CH3OH (CH30)2C0 + CH3CHOHCH2OH.
The boiling points of the resulting ethylene glycol, propylene glycol and other carbonates are all higher than 100 °C, while the boiling point of dimethyl carbonate is only 90°C, so the crude product of dimethyl carbonate can be distilled out under temperature control, and subsequently the dimethyl carbonate can be purified by frozen crystallization. The present disclosure can collect the electrolyte economically and efficiently, and the distilled carbonate product is of high purity and can be sold in the market.
BRIEF DESCRIPTION OF DRAWINGS
The present disclosure will be further described below in conjunction with the drawings and embodiments, wherein: Figure I is a process flow chart of the present disclosure. DETAILED DESCRIPTION The concept of the present disclosure and the technical effects produced by the present disclosure will be clearly and completely described below with reference to the embodiments, so as to make the purpose, characteristics and effects of the present disclosure fully understood. Obviously, the described embodiments are only a part of the embodiments of the present disclosure, rather than all the embodiments. Based on the embodiments of the present disclosure, other embodiments obtained by those skilled in the art without creative efforts are all within the protection scope of the
present disclosure.
Example 1
A method for efficiently recovering waste lithium-ion battery electrolyte, with reference to Figure 1, comprised the following specific process: 5kg of waste ternary lithium battery was taken, and pulverized with a pulverizer after discharging to release the electrolyte in the lithium-ion battery. Then the battery fragments with electrolyte after pulverizing was added into 20L of sodium sulfate brine with a concentration of 10%, stirred and washed at room temperature for 10 minutes. After the washing was completed, the thick battery fragments were removed and drained using a coarse mesh, and then the thin slag was removed by suction filtration. The filtered solution was left to stand for 0.5h in a separatory bucket to separate the aqueous phase and electrolyte. The aqueous phase was returned to the previous step to wash the battery fragments, and 600 mL of electrolyte was collected by liquid separation. The collected electrolyte was added with 200 mL of methanol, heated up to 60 °C in a rotary evaporator to react for 2 hours, and distilled for 1 h at a vacuum degree of 30 kPa and a distillation temperature of 80 °C to obtain 500 mL of distillate. The distilled residual solution entered the next lithium extraction process. The distillate was placed in a refrigerator and frozen at 0 CC for 1 h, and then centrifuged and filtered under a 0 °C frozen condition to obtain dimethyl carbonate crystals. The dimethyl carbonate crystals were melted at room temperature to obtain 400 mL of dimethyl carbonate product. The purity of dimethyl carbonate detected by GC-MS was 99%.
Example 2
A method for efficiently recovering waste lithium-ion battery electrolyte comprised the following specific process 5kg of waste ternary lithium battery was taken, and pulverized with a pulverizer after discharging to release the electrolyte in the lithium-ion battery. Then the battery fragments with electrolyte after pulverizing was added into I.5L of sodium chloride brine with a concentration of 15%, stirred and washed at room temperature for 20 minutes. After the washing was completed, the thick battery fragments were removed and drained using a coarse mesh, and then the thin slag was removed by suction filtration. The filtered solution was left to stand for lh in a separatory bucket to separate the aqueous phase and electrolyte. The aqueous phase was returned to the previous step to wash the battery fragments, and 540 nth of electrolyte was collected by liquid separation. The collected electrolyte was added with 150 mL of methanol, heated up to 60 °C in a rotary evaporator to react for 2 hours, and distilled for 1 h at a vacuum degree of 40 lcPa and a distillation temperature of 80 °C to obtain 420 mL of distillate. The distilled residual solution entered the next lithium extraction process. The distillate was placed in a refrigerator and frozen at 0 CC for 1 h, and then centrifuged and filtered under a 0 °C frozen condition to obtain dimethyl carbonate crystals. The dimethyl carbonate crystals were melted at room temperature to obtain 340 mL of dimethyl carbonate product. The purity of dimethyl carbonate detected by GC-MS was 99%.
Example 3
A method for efficiently recovering waste lithium-ion battery electrolyte comprised the following specific process: 5kg of waste ternary lithium battery was taken, and pulverized with a pulverizer after discharging to release the electrolyte in the lithium-ion battery. Then the battery fragments with electrolyte after pulverizing was added into 25L of potassium sulfate brine with a concentration of 20%, stirred and washed at room temperature for 20 minutes. After the washing was completed, the thick battery fragments were removed and drained using a coarse mesh, and then the thin slag was removed by suction filtration. The filtered solution was left to stand for 0.5h in a separatory bucket to separate the aqueous phase and electrolyte. The aqueous phase was returned to the previous step to wash the battery fragments, and 620 mL of electrolyte was collected by liquid separation. The collected electrolyte was added with 200 mL of methanol, and heated up to 60 °C in a rotary evaporator to react for 2 hours, and distilled for 1 h at a vacuum degree of 20 kPa and a distillation temperature of 80 °C to obtain 540 mL of distillate. The distilled residual solution entered the next lithium extraction process. The distillate was placed in a refrigerator and frozen at 0 °C for 1 h, and then centrifuged and filtered under a 0 °C frozen condition to obtain dimethyl carbonate crystals. The dimethyl carbonate crystals were melted at room temperature to obtain 420 mL of dimethyl carbonate product. The purity of dimethyl carbonate detected by GC-MS was 99%.
The embodiments of the present disclosure have been described in detail above in conjunction with the drawings, but the present disclosure is not limited to the above-mentioned embodiments. Within the scope of knowledge possessed by those of ordinary skill in the art, various changes can also be made without departing from the essence of the present disclosure. Furthermore, the embodiments and the features in the embodiments of the present disclosure may be combined with each other without conflict.
Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the present disclosure belongs. In case of conflict, the definitions in this specification shall prevail. When mass, concentration, temperature, time, or other value or parameter is expressed as a range, a preferred range or a range bounded by a series of upper preferred values and lower preferred values, it should be understood as specifically disclosing all ranges formed by any pairing of any upper limit or preferred value of any range with any lower limit or preferred value of any range, whether the range is individually disclosed or not For example, a range of 1-50 should be understood to include any number, combination of numbers, or subrange selected from 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, II, 12, 13, 14, Ii, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50, and all decimal values among the above integers, for example, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. With regard to subranges, specific consideration is given to "nested subrange" extending from any endpoint within the range. For example, the nested subranges of the exemplary range 1-50 may include 1-10, 1-20, 1-30, and 1-40 in one direction, or 50-40, 50-30, 50-20 and 50-10 in the other direction
Claims (10)
- CLAIMS1. A method for efficiently recovering waste lithium-ion battery electrolyte, comprising the following steps: S 1: pulverizing a waste lithium-ion battery to obtain a pulverized material with electrolyte, washing the pulverized material in a salt solution, and performing solid-liquid separation after washing to obtain a filtrate; 52: leaving the filtrate to stand for stratification to obtain an aqueous phase and an organic phase; and 53: mixing the organic phase with methanol, and performing distillation under the conditions of 10 a temperature of 60 °C to 100 °C and a vacuum degree of 10 kPa to 80 kPa, to obtain a crude product of dimethyl carbonate.
- 2. The method according to claim I, wherein in step Si, the salt solution is a neutral salt solution; and the salt in the salt solution is selected from one or more of sodium chloride, sodium sulfate, potassium chloride or potassium sulfate.
- 3. The method according to claim 1, wherein in step Si, the mass concentration of the salt solution is 5% to 25%, and the liquid-solid ratio of the salt solution to the pulverized material is (2-8): 1 L/kg.
- 4. The method according to claim I, wherein in step S I, the washing is performed at a stirring speed of 60 r/min to 400 r/min.
- 5. The method according to claim 1, wherein in step S I, the duration of the washing is 5 min to min.
- 6. The method according to claim 1, wherein in step S2, the aqueous phase is returned to step 51 for the washing.
- 7. The method according to claim 1, wherein in step S2, the duration of the standing for stratification is 0.5 h to 3 h.
- S. The method according to claim 1, wherein in step S3, the volume ratio of the organic phase to methanol is 1: (0.2-1).
- 9. The method according to claim 1, wherein in step S3, the crude product of dimethyl carbonate is frozen crystalized, then the obtained dimethyl carbonate crystal is heated up and melted to obtain pure dimethyl carbonate.
- 10. The method according to claim I, wherein in step S3, the distilled residual solution enters the next lithium extraction process.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210608686.7A CN114865134A (en) | 2022-05-31 | 2022-05-31 | Method for efficiently recycling electrolyte of waste lithium ion battery |
PCT/CN2023/081684 WO2023231508A1 (en) | 2022-05-31 | 2023-03-15 | Method for efficiently recovering electrolyte of spent lithium-ion battery |
Publications (3)
Publication Number | Publication Date |
---|---|
GB202318911D0 GB202318911D0 (en) | 2024-01-24 |
GB2622974A true GB2622974A (en) | 2024-04-03 |
GB2622974A8 GB2622974A8 (en) | 2024-05-15 |
Family
ID=82641320
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB2318911.1A Pending GB2622974A (en) | 2022-05-31 | 2023-03-15 | Method for efficiently recovering electrolyte of spent lithium-ion battery |
Country Status (4)
Country | Link |
---|---|
CN (1) | CN114865134A (en) |
DE (1) | DE112023000108T5 (en) |
GB (1) | GB2622974A (en) |
WO (1) | WO2023231508A1 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114865134A (en) * | 2022-05-31 | 2022-08-05 | 广东邦普循环科技有限公司 | Method for efficiently recycling electrolyte of waste lithium ion battery |
CN115528338A (en) * | 2022-09-16 | 2022-12-27 | 广东邦普循环科技有限公司 | Method for recovering lithium from lithium ion battery electrolyte |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4181676A (en) * | 1977-09-07 | 1980-01-01 | Bayer Aktiengesellschaft | Process for the preparation of dialkyl carbonates |
CN106659947A (en) * | 2014-06-18 | 2017-05-10 | 罗地亚经营管理公司 | Process for recovering an electrolyte salt |
CN108923092A (en) * | 2018-06-29 | 2018-11-30 | 惠州市宙邦化工有限公司 | A kind of waste and old lithium ionic cell electrolyte processing method |
CN111454152A (en) * | 2020-06-22 | 2020-07-28 | 东营市海科新源化工有限责任公司 | Preparation method and preparation device of electronic grade dimethyl carbonate |
CN112531227A (en) * | 2019-09-17 | 2021-03-19 | 天津理工大学 | Harmless recycling method for electrolyte in waste lithium ion battery |
CN114865134A (en) * | 2022-05-31 | 2022-08-05 | 广东邦普循环科技有限公司 | Method for efficiently recycling electrolyte of waste lithium ion battery |
-
2022
- 2022-05-31 CN CN202210608686.7A patent/CN114865134A/en active Pending
-
2023
- 2023-03-15 DE DE112023000108.1T patent/DE112023000108T5/en active Pending
- 2023-03-15 WO PCT/CN2023/081684 patent/WO2023231508A1/en active Application Filing
- 2023-03-15 GB GB2318911.1A patent/GB2622974A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4181676A (en) * | 1977-09-07 | 1980-01-01 | Bayer Aktiengesellschaft | Process for the preparation of dialkyl carbonates |
CN106659947A (en) * | 2014-06-18 | 2017-05-10 | 罗地亚经营管理公司 | Process for recovering an electrolyte salt |
CN108923092A (en) * | 2018-06-29 | 2018-11-30 | 惠州市宙邦化工有限公司 | A kind of waste and old lithium ionic cell electrolyte processing method |
CN112531227A (en) * | 2019-09-17 | 2021-03-19 | 天津理工大学 | Harmless recycling method for electrolyte in waste lithium ion battery |
CN111454152A (en) * | 2020-06-22 | 2020-07-28 | 东营市海科新源化工有限责任公司 | Preparation method and preparation device of electronic grade dimethyl carbonate |
CN114865134A (en) * | 2022-05-31 | 2022-08-05 | 广东邦普循环科技有限公司 | Method for efficiently recycling electrolyte of waste lithium ion battery |
Also Published As
Publication number | Publication date |
---|---|
CN114865134A (en) | 2022-08-05 |
GB2622974A8 (en) | 2024-05-15 |
DE112023000108T5 (en) | 2024-05-29 |
GB202318911D0 (en) | 2024-01-24 |
WO2023231508A1 (en) | 2023-12-07 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
GB2622974A (en) | Method for efficiently recovering electrolyte of spent lithium-ion battery | |
CN109336142B (en) | Method for extracting lithium from salt lake brine and preparing aluminum hydroxide simultaneously | |
CN108281729B (en) | Waste lithium ion battery electrolyte recovery process | |
CN106910889B (en) | A method of regenerating positive active material from waste lithium iron phosphate battery | |
CN102496752B (en) | Method for recycling electrolyte of waste lithium ion battery | |
EP2312686A1 (en) | Method for implementing full cycle regeneration of waste lead acid battery | |
CN104600392A (en) | Method for recovering electrolyte of waste lithium ion battery | |
CN101450815A (en) | Method for preparing nickel and cobalt doped lithium manganate by using waste and old lithium ionic cell as raw material | |
CN110013822A (en) | A kind of method of waste and old lithium ion battery recycling co-production lithium adsorbent | |
CN108288737B (en) | Method for recovering lithium hexafluorophosphate from waste lithium battery cathode material | |
CN102332581B (en) | Method for producing lithium ferrous phosphate by using lithium mine as lithium source | |
CN106929664A (en) | A kind of method that lithium is reclaimed from waste and old ternary lithium ion battery | |
CN105390765A (en) | Recovery method for electrolyte solution of lithium ion battery | |
CN109825708A (en) | Method for recovering positive and negative electrode substances in waste alkaline zinc-manganese dioxide battery | |
CN100482631C (en) | Method of preparing boron lithium dioxalate complex salt | |
CN111115665A (en) | Method for recycling lithium-potassium-rich aluminum electrolyte | |
CN109292746A (en) | The method of lithium hexafluoro phosphate is recycled in a kind of waste lithium cell | |
CN111924816A (en) | Method for recovering electrolyte of waste lithium ion battery | |
CN101654741B (en) | Method for separating and recovering lithium and cobalt from lithium ion cell | |
FR3139947A1 (en) | METHOD FOR RECYCLING LITHIUM FROM THE ELECTROLYTE OF A LITHIUM-ION BATTERY | |
CN115353088B (en) | Method for recycling lithium ion battery electrolyte | |
CN100359734C (en) | Recycling method of waste alkaline zinc-manganese dioxide battery | |
WO2023098167A1 (en) | Method for recovering waste lithium cobalt oxide battery | |
CN103137981B (en) | Preparation method for anhydrous lithium iodide | |
CN106435186A (en) | Cobalt waste acid hydrolysis method and application of cobalt waste acid hydrolysis method to preparation of high-purity cobalt liquid for cobaltosic oxide |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
789A | Request for publication of translation (sect. 89(a)/1977) |
Ref document number: 2023231508 Country of ref document: WO |