CN115332659A - Method for recovering electrolyte by underwater crushing waste lithium ion battery - Google Patents
Method for recovering electrolyte by underwater crushing waste lithium ion battery Download PDFInfo
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- CN115332659A CN115332659A CN202210898701.6A CN202210898701A CN115332659A CN 115332659 A CN115332659 A CN 115332659A CN 202210898701 A CN202210898701 A CN 202210898701A CN 115332659 A CN115332659 A CN 115332659A
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- calcium chloride
- crusher
- electrolyte
- mixed solution
- lithium ion
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- 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
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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
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- 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
Abstract
The invention discloses a method for recycling electrolyte by underwater crushing of waste lithium ion batteries, which comprises the steps of adding a calcium chloride mixed solution and the waste lithium ion batteries into a crusher for underwater crushing, distilling a crushed filtrate, layering the distilled filtrate to obtain an electrolyte and a water phase, extracting the water phase by using carbon tetrachloride, and separating raffinate by a nanofiltration membrane to obtain a lithium salt solution and a calcium chloride solution. According to the invention, the calcium chloride mixed solution can ensure that the temperature cannot be sharply increased, the potential safety hazard is reduced, the electrolyte can be completely dissolved, and the characteristics of different water solubility of the electrolyte are utilized to separate the water-insoluble and water-soluble electrolytes for respective treatment, so that the pressure of subsequent rectification is reduced.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery recovery, and particularly relates to a method for recovering electrolyte from waste lithium ion batteries by underwater crushing.
Background
The lithium ion battery has the advantages of high energy density, no memory effect, excellent electrical property and the like, and is widely applied to the fields of electronic products, new energy automobiles, energy storage and the like. The service life of the lithium ion battery is generally 3-8 years, the lithium ion battery gradually enters a large-scale retirement period at present, and the problem of recycling the lithium ion battery is urgent.
At present, the method for recycling the waste lithium ion battery in China mainly comprises the process flows of disassembling, crushing, sorting, element refining and the like, and realizes the recycling of valuable resources such as nickel, cobalt, manganese, lithium and the like. In these processes, the used lithium ion batteries are first subjected to charged safe crushing or safe discharge. The traditional brine discharge process can generate chlorine or gases such as hydrogen, oxygen and the like, is not environment-friendly and has certain safety; physical discharge, however, has problems of low discharge efficiency and safety during discharge. Both chemical and physical discharge have various problems, and therefore, in order to improve the battery processing efficiency, charged crushing is a rigid demand for the current mass processing of waste batteries.
However, the charged safe crushing is still in the research stage at present, in the charged crushing in the present process, the positive and negative pole pieces in the battery are short-circuited due to the physical processes of extrusion, shearing and the like of the battery, and the residual electric quantity in the battery can be rapidly released, so that the phenomena of heat release, fire, explosion and the like occur in the crushing process, and the safety of the crushing process is influenced.
If direct breakage, the electrolyte in the battery flows out, not only pollutes the environment, contacts skin after, still can cause the injury to skin, and under the incomplete condition of discharging, direct breakage is easy to catch fire, explode more, and the safety risk is great. In the prior art, although the danger coefficient in the crushing process can be reduced by the disclosed liquid nitrogen freezing crushing, the existence of lithium embedded in a negative electrode still causes the explosion risk of the crushed material; the injected inert gas can not cool or isolate the heated battery materials although isolating air, and can not completely realize safe crushing; although safe crushing can be realized by underwater crushing, the electrolyte is leaked into water, and the electrolyte has different properties to water, some of the electrolyte is insoluble in water, some of the electrolyte is soluble in water, effective separation is difficult, and a large amount of organic wastewater is generated to pollute the environment and is difficult to treat.
Therefore, a method for recycling and processing the electrolyte while underwater crushing is needed, which realizes safe crushing and efficient utilization of resources.
Disclosure of Invention
The present invention has been made to solve at least one of the above-mentioned problems occurring in the prior art. Therefore, the invention provides a method for recycling electrolyte by underwater crushing of waste lithium ion batteries.
According to one aspect of the invention, the method for recycling the electrolyte by underwater crushing of the waste lithium ion battery is provided, and comprises the following steps:
s1: adding the calcium chloride mixed solution and the waste lithium ion battery into a crusher for carrying out submerged crushing, and controlling the temperature in the crusher to be below 40 ℃ in the process; wherein the calcium chloride mixed solution is a mixed solution of a calcium chloride solution and an organic solvent;
s2: after the crushing in the step S1 is finished, carrying out solid-liquid separation on the obtained solid-liquid mixture to obtain a filtrate;
s3: distilling the filtrate to separate the organic solvent to obtain distilled liquid, and standing and layering the distilled liquid to obtain an upper electrolyte and a lower water phase;
s4: extracting the lower aqueous phase by using carbon tetrachloride, and separating to obtain an organic phase and raffinate;
s5: and extracting lithium from the raffinate through a nanofiltration membrane, and separating to obtain a lithium salt solution and a calcium chloride solution.
In some embodiments of the present invention, in step S1, the concentration of the calcium chloride solution is 0.1 to 1mol/L, and the volume ratio of the calcium chloride solution to the organic solvent is (1 to 1.5): 1.
in some embodiments of the invention, in step S1, the organic solvent is at least one of methanol, ethanol or acetone. The organic solvent is a water-soluble organic solvent.
In some embodiments of the invention, in step S1, the amount of the waste lithium ion battery added is 10-20% of the volume of the calcium chloride mixed solution.
In some embodiments of the invention, in step S1, the temperature within the crusher is controlled by: and (3) conveying the calcium chloride mixed solution into a condenser from the upper part of the crusher by using a circulating pump, and returning the calcium chloride mixed solution into the crusher from the lower part of the crusher.
In some embodiments of the invention, the temperature of the distillation in step S3 is 50 to 85 ℃.
In some embodiments of the invention, in step S3, the volume content of the organic solvent in the post-distillation liquid is less than 5%.
In some embodiments of the invention, the standing time in step S3 is 0.5 to 1 hour.
In some embodiments of the invention, in step S4, the volume ratio of carbon tetrachloride to lower aqueous phase is (0.5-2): 1.
in some embodiments of the invention, in step S4, the organic phase is refined in a rectification process.
In some embodiments of the present invention, in step S5, the separated calcium chloride solution is used for preparing the calcium chloride mixed solution in step S1.
According to a preferred embodiment of the present invention, at least the following advantages are provided:
1. according to the invention, the waste lithium ion battery is crushed under liquid by using the calcium chloride mixed solution, on one hand, the calcium chloride solution has a good refrigeration effect, can absorb more heat, ensures that the temperature in the crusher does not rise sharply, and avoids potential safety hazards; on the other hand, the electrolyte after the waste lithium ion battery is crushed is dissolved, the electrolyte salt lithium hexafluorophosphate in the electrolyte is reacted with calcium chloride to generate lithium salt, calcium phosphate and calcium fluoride, and the electrolyte solvent carbonate and the like can be completely dissolved under the mixing action of the organic solvent and water due to different water solubility, so that the subsequent recovery of the electrolyte is facilitated.
2. After the crushing is finished, carrying out solid-liquid separation, recovering valuable substances and elements in the electrolyte, extracting a low-boiling-point organic solvent from the electrolyte by distillation, separating out water-insoluble electrolyte (such as diethyl carbonate, ethyl methyl carbonate and the like), and layering the filtrate by utilizing the characteristic that the density of a calcium chloride solution is greater than that of the electrolyte, thereby separating the water-insoluble electrolyte; extracting the water-soluble electrolyte into a carbon tetrachloride solution through carbon tetrachloride extraction, and subsequently sending the solution to a rectification process for refining; the remained raffinate contains a large amount of calcium chloride and lithium chloride, the calcium and the lithium are separated by a nanofiltration membrane to obtain lithium salt, and the calcium chloride solution can be mixed with the organic solvent for recycling.
3. The method separates the water-insoluble electrolyte and the water-soluble electrolyte for respective treatment by utilizing the characteristic of different water solubility of the electrolyte solvent, reduces the pressure of subsequent unified rectification, has lower distillation temperature, reduces the hydrolysis of esters, and improves the yield of the electrolyte.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a process flow diagram of example 1 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
A method for recycling electrolyte from waste lithium ion batteries by underwater crushing refers to FIG. 1, and the specific process is as follows:
step 1, mixing 1mol/L calcium chloride solution and methanol according to a volume ratio of 1.5:1, mixing to obtain a calcium chloride mixed solution;
step 2, adding the calcium chloride mixed solution into a crusher, wherein the crusher is provided with a containing box, crushing rollers which run in opposite directions are arranged in the containing box, and the added amount of the calcium chloride mixed solution needs to flow over the crushing rollers and cannot flow out of the containing box;
step 3, starting a crusher and a circulating pump, and putting waste lithium ion batteries into the crusher, wherein the adding amount of the waste lithium ion batteries is 20% of the volume of the calcium chloride mixed solution in the containing box, the waste lithium ion batteries are crushed by a crushing roller of the crusher and then enter the bottom of the crusher, the circulating pump sends the calcium chloride mixed solution to a condenser from the upper part of the crusher and then returns from the lower part of the crusher, the temperature in the crusher is controlled to be below 40 ℃ all the time, and no gas escapes in the process;
step 4, after the crushing in the step 3 is finished, obtaining a solid-liquid mixture, discharging from the bottom of the crusher, performing filter pressing, feeding obtained solid slag into a pyrolysis system, and feeding filtrate into a distillation process;
step 5, stirring and distilling the filtrate at 70 ℃ until the volume content of the methanol is lower than 5%, and separating out the methanol;
step 6, stopping stirring, standing for 0.5h, separating filtrate into two layers, and separating to obtain an upper electrolyte and a lower water phase;
step 7, extracting the lower-layer water phase by using carbon tetrachloride according to the volume ratio of 1;
and 8, extracting lithium from the raffinate obtained in the step 7 through a nanofiltration membrane, separating to obtain a lithium salt solution and a calcium chloride solution, mixing the calcium chloride solution with the methanol obtained in the step 5, and then preparing a calcium chloride mixed solution again. The total recovery rate of the electrolyte in the embodiment reaches 91.2%.
Example 2
A method for recycling electrolyte from waste lithium ion batteries by underwater crushing comprises the following specific processes:
step 1, mixing 0.5mol/L calcium chloride solution and ethanol according to a volume ratio of 1.3:1, mixing to obtain a calcium chloride mixed solution;
step 2, adding the calcium chloride mixed solution into a crusher, wherein the crusher is provided with a containing box, crushing rollers which run in opposite directions are arranged in the containing box, and the added amount of the calcium chloride mixed solution needs to flow over the crushing rollers and cannot flow out of the containing box;
step 3, starting a crusher and a circulating pump, and putting waste lithium ion batteries into the crusher, wherein the adding amount of the waste lithium ion batteries is 15% of the volume of the calcium chloride mixed solution in the containing box, the waste lithium ion batteries are crushed by a crushing roller of the crusher and then enter the bottom of the crusher, the circulating pump sends the calcium chloride mixed solution to a condenser from the upper part of the crusher and then returns from the lower part of the crusher, the temperature in the crusher is controlled to be below 40 ℃ all the time, and no gas escapes in the process;
step 4, after the crushing in the step 3 is finished, obtaining a solid-liquid mixture, performing filter pressing on the solid mixture discharged from the bottom of the crusher, feeding the obtained solid slag into a pyrolysis system, and feeding the filtrate into a distillation process;
step 5, stirring and distilling the filtrate at 80 ℃ until the volume content of ethanol is lower than 5%, and separating out ethanol;
step 6, stopping stirring, standing for 0.8h, separating filtrate into two layers, and separating to obtain an upper electrolyte and a lower water phase;
step 7, extracting the lower-layer water phase by using carbon tetrachloride according to the volume ratio of 1;
and 8, extracting lithium from the raffinate obtained in the step 8 through a nanofiltration membrane, separating to obtain a lithium salt solution and a calcium chloride solution, mixing the calcium chloride solution with the organic solvent obtained in the step 5, and then preparing a calcium chloride mixed solution again. The total recovery rate of the electrolyte in the embodiment reaches 90.4%.
Example 3
A method for recycling electrolyte from waste lithium ion batteries by underwater crushing comprises the following specific processes:
step 1, mixing 0.1mol/L calcium chloride solution and acetone according to a volume ratio of 1:1, mixing to obtain a calcium chloride mixed solution;
step 2, adding the calcium chloride mixed solution into a crusher, wherein the crusher is provided with a containing box, crushing rollers which run in opposite directions are arranged in the containing box, and the added amount of the calcium chloride mixed solution needs to flow over the crushing rollers and cannot flow out of the containing box;
step 3, starting a crusher and a circulating pump, and putting waste lithium ion batteries into the crusher, wherein the adding amount of the waste lithium ion batteries is 10% of the volume of the calcium chloride mixed solution in the containing box, the waste lithium ion batteries are crushed by a crushing roller of the crusher and then enter the bottom of the crusher, the circulating pump sends the calcium chloride mixed solution to a condenser from the upper part of the crusher and then returns from the lower part of the crusher, the temperature in the crusher is controlled to be below 40 ℃ all the time, and no gas escapes in the process;
step 4, after the crushing in the step 3 is finished, obtaining a solid-liquid mixture, performing filter pressing on the solid mixture discharged from the bottom of the crusher, feeding the obtained solid slag into a pyrolysis system, and feeding the filtrate into a distillation process;
step 5, stirring and distilling the filtrate at 60 ℃ until the volume content of acetone is lower than 5%, and separating out the acetone;
step 6, stopping stirring, standing for 1h, separating the filtrate into two layers, and separating to obtain an upper electrolyte and a lower water phase;
step 7, extracting the lower-layer water phase by using carbon tetrachloride according to the volume ratio of 1;
and 8, extracting lithium from the raffinate obtained in the step 8 through a nanofiltration membrane, separating to obtain a lithium salt solution and a calcium chloride solution, mixing the calcium chloride solution with the organic solvent obtained in the step 5, and then preparing a calcium chloride mixed solution again. The total recovery of the electrolyte in the embodiment reaches 89.3%.
Comparative example 1
The method for recycling the electrolyte by underwater crushing of the waste lithium ion battery is different from the method in the embodiment 1 in that the liquid used for crushing is water, and the specific process is as follows:
step 1, adding water into a crusher, wherein the crusher is provided with an accommodating box, crushing rollers which run in opposite directions are arranged in the accommodating box, and the adding amount of the water needs to overflow the crushing rollers and cannot overflow the accommodating box;
step 2, starting the crusher and the circulating pump, and putting the waste lithium ion batteries into the crusher, wherein the adding amount of the waste lithium ion batteries is 20% of the volume of water in the containing tank, the waste lithium ion batteries are crushed by a crushing roller of the crusher and then enter the bottom of the crusher, the circulating pump sends water into a condenser from the upper part of the crusher and then returns from the lower part of the crusher, the temperature in the crusher is controlled to be below 40 ℃ all the time, and gas escapes in the process to form phosphorus pentafluoride;
step 3, after the crushing in the step 2 is finished, obtaining a solid-liquid mixture, performing filter pressing on the solid mixture discharged from the bottom of the crusher, feeding the obtained solid slag into a pyrolysis system, and feeding the filtrate into a distillation process;
and 4, standing the filtrate without layering, and directly sending the filtrate into a rectification process.
The liquid used for crushing in the comparative example is water, phosphorus pentafluoride with pungent foul smell can overflow in the crushing process, and the water and the electrolyte are strongly mixed in the crushing stage, and the density of the carbonic ester is close to that of the water, so that the filtrate cannot be layered, the filtrate cannot be subjected to grading treatment, only unified rectification can be performed, and the pressure of rectification is increased. The total recovery rate of the electrolyte of the comparative example is only 70.6%, and the main reasons for electrolyte loss are as follows: (1) During crushing, water is not sufficiently dissolved for some water-insoluble electrolyte, and a small amount of electrolyte still remains in the solid slag; (2) The filtrate directly enters a rectification process, and the electrolyte is easy to hydrolyze in the rectification process.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A method for recycling electrolyte from waste lithium ion batteries by underwater crushing is characterized by comprising the following steps:
s1: adding the calcium chloride mixed solution and the waste lithium ion battery into a crusher for carrying out submerged crushing, and controlling the temperature in the crusher to be below 40 ℃ in the process; wherein the calcium chloride mixed solution is a mixed solution of a calcium chloride solution and an organic solvent;
s2: after the crushing in the step S1 is finished, carrying out solid-liquid separation on the obtained solid-liquid mixture to obtain a filtrate;
s3: distilling the filtrate to separate the organic solvent to obtain distilled liquid, and standing and layering the distilled liquid to obtain an upper electrolyte and a lower water phase;
s4: extracting the lower aqueous phase by using carbon tetrachloride, and separating to obtain an organic phase and raffinate;
s5: and extracting lithium from the raffinate through a nanofiltration membrane, and separating to obtain a lithium salt solution and a calcium chloride solution.
2. The method according to claim 1, wherein in step S1, the concentration of the calcium chloride solution is 0.1-1mol/L, and the volume ratio of the calcium chloride solution to the organic solvent is (1-1.5): 1.
3. the method according to claim 1, wherein in step S1, the organic solvent is at least one of methanol, ethanol or acetone.
4. The method according to claim 1, wherein in step S1, the amount of the waste lithium ion battery added is 10-20% of the volume of the calcium chloride mixed solution.
5. The method according to claim 1, characterized in that in step S1 the temperature inside the crusher is controlled by: and (3) conveying the calcium chloride mixed solution into a condenser from the upper part of the crusher by using a circulating pump, and returning the calcium chloride mixed solution into the crusher from the lower part of the crusher.
6. The method according to claim 1, wherein in step S3, the temperature of the distillation is 50-85 ℃.
7. The method according to claim 1, wherein in step S3, the volume content of the organic solvent in the post-distillation liquid is less than 5%.
8. The method of claim 1, wherein in step S4, the volume ratio of the carbon tetrachloride to the lower aqueous phase is (0.5-2): 1.
9. the method of claim 1, wherein in step S4, the organic phase is refined in a rectification process.
10. The method according to claim 1, wherein in step S5, the separated calcium chloride solution is used for preparing the calcium chloride mixed solution in step S1.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210898701.6A CN115332659A (en) | 2022-07-28 | 2022-07-28 | Method for recovering electrolyte by underwater crushing waste lithium ion battery |
| PCT/CN2022/117481 WO2024021232A1 (en) | 2022-07-28 | 2022-09-07 | Method for underwater crushing and electrolyte solution recycling of waste lithium ion battery |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210898701.6A CN115332659A (en) | 2022-07-28 | 2022-07-28 | Method for recovering electrolyte by underwater crushing waste lithium ion battery |
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| WO (1) | WO2024021232A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116544546A (en) * | 2023-07-06 | 2023-08-04 | 深圳市杰成镍钴新能源科技有限公司 | Method for recycling waste lithium battery material |
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| CN106823816B (en) * | 2016-12-19 | 2020-04-17 | 天齐锂业股份有限公司 | Electrochemical recovery method of lithium in anode material of waste lithium battery |
| PL3535803T3 (en) * | 2017-05-30 | 2022-06-27 | Li-Cycle Corp. | A process, apparatus, and system for recovering materials from batteries |
| CN110289457A (en) * | 2019-06-24 | 2019-09-27 | 中国科学院过程工程研究所 | A kind of green waste and old lithium ionic cell electrolyte recovery system and method |
| CN111924816A (en) * | 2020-07-02 | 2020-11-13 | 曲靖市华祥科技有限公司 | Method for recovering electrolyte of waste lithium ion battery |
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- 2022-07-28 CN CN202210898701.6A patent/CN115332659A/en active Pending
- 2022-09-07 WO PCT/CN2022/117481 patent/WO2024021232A1/en unknown
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116544546A (en) * | 2023-07-06 | 2023-08-04 | 深圳市杰成镍钴新能源科技有限公司 | Method for recycling waste lithium battery material |
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