CN109292746A - The method of lithium hexafluoro phosphate is recycled in a kind of waste lithium cell - Google Patents
The method of lithium hexafluoro phosphate is recycled in a kind of waste lithium cell Download PDFInfo
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- CN109292746A CN109292746A CN201811079901.9A CN201811079901A CN109292746A CN 109292746 A CN109292746 A CN 109292746A CN 201811079901 A CN201811079901 A CN 201811079901A CN 109292746 A CN109292746 A CN 109292746A
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- organic solvent
- hexafluoro phosphate
- lithium
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- acetonitrile
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/308—Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
-
- 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
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Primary Cells (AREA)
Abstract
The invention belongs to lithium battery recovery technology fields, and in particular to the method for lithium hexafluoro phosphate is recycled in a kind of waste lithium cell.The present invention mixes waste lithium cell core with organic solvent, the positive and negative pole material and diaphragm that can make battery come into full contact with organic solvent, then under ultrasonication, the lithium hexafluoro phosphate being adhered in positive and negative pole material, diaphragm and electrolyte is transferred in organic solvent；And organic solvent uses the mixture of acetonitrile and carbonic ester, can improve the solvability to lithium hexafluoro phosphate, and then realizes the high efficiente callback of lithium hexafluoro phosphate.Embodiment the result shows that, the lithium hexafluoro phosphate in waste lithium cell is recycled using above scheme, the rate of recovery is up to 92% or more.
Description
Technical field
The invention belongs to lithium battery recovery technology fields, and in particular to lithium hexafluoro phosphate is recycled in a kind of waste lithium cell
Method.
Background technique
Lithium battery due to being used widely with excellent chemical property, although the chemical property of lithium battery compared with
Length of service for stabilization, but battery is still limited, this just inevitably generates a large amount of waste lithium cell.Waste and old lithium
Containing there are many resources with recovery value in battery, such as electrolyte, iron content, aluminium, the metal of copper and change containing cobalt, lithium, nickel
Close object.About the recycling of electrolyte, alkali absorption method, rectification under vacuum method and treatment by extraction, such as patent document are used substantially
A kind of 201410069599.4 " the waste and old lithium ionic cell electrolyte recovery and treatment methods " provided are just returned using the method for distillation
Receive electrolyte.About lithium-containing compound, " valuable metal in waste lithium ion that patent document 201310281792.X is announced
Extract technology and its device " provides a kind of method for leaching cobalt acid lithium using electrolysis auxiliary；But lithium-ion battery electrolytes one
As be lithium hexafluoro phosphate, there is larger harmfulness to human body and environment, can not be recycled with above-mentioned technique.Although patent
Document 201610654668.7 provides a kind of recovery method of lithium hexafluoro phosphate in waste lithium cell, but recovery efficiency and pays no attention to
Think.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention provides a kind of method that lithium hexafluoro phosphate is recycled in waste lithium cell,
Recovery method provided by the invention can carry out high efficiente callback to the lithium hexafluoro phosphate in old and useless battery, improve waste lithium cell
Resource recovery.
In order to achieve the above object, the invention provides the following technical scheme:
A kind of method that lithium hexafluoro phosphate is recycled in waste lithium cell, includes the following steps:
(1) it will include the mixture progress ultrasound of waste lithium cell core and organic solvent, obtain Solid-liquid mixture；It is described
Organic solvent includes acetonitrile and carbonic ester；
(2) in anhydrous conditions, the Solid-liquid mixture of the step (1) is separated by solid-liquid separation, obtains extracting solution；
(3) extracting solution of the step (2) is distilled, obtains lithium hexafluoro phosphate.
Preferably, the volume ratio of acetonitrile and carbonic ester is (2~50) in step (1) organic solvent: 100.
Preferably, the carbonic ester includes in ethylene carbonate, propene carbonate, dimethyl carbonate and diethyl carbonate
It is one or more of.
Preferably, the organic solvent replace with acetonitrile, ethylene carbonate and dimethyl carbonate mixture or acetonitrile,
The mixture of the mixture or acetonitrile of propene carbonate and dimethyl carbonate, ethylene carbonate and diethyl carbonate.
Preferably, the quality of core and the volume ratio of organic solvent are 1g: (20~80) mL in the step (1).
Preferably, frequency ultrasonic in the step (1) is 30~60kHz, and the ultrasonic time is 5~15min.
Preferably, in step (1) ultrasonic procedure, the temperature of core and organic solvent mixed system is 15~25 DEG C.
Preferably, the mode of the separation of solid and liquid of the step (2) includes filtering or centrifugation.
Preferably, before step (3) distillation, further includes: be filled with hydrogen fluoride gas into extracting solution.
Preferably, the mode distilled in the step (3) is vacuum distillation.
The present invention provides in a kind of waste lithium cell recycle lithium hexafluoro phosphate method, include the following steps: will include
The mixture of waste lithium cell core and organic solvent carries out ultrasound, obtains Solid-liquid mixture；The organic solvent includes acetonitrile
And carbonic ester；Then in anhydrous conditions, gained Solid-liquid mixture is separated by solid-liquid separation, obtains extracting solution；It finally will be described
Extracting solution is distilled, and lithium hexafluoro phosphate is obtained.The present invention mixes waste lithium cell core with organic solvent, can make battery
Positive and negative pole material and diaphragm come into full contact with organic solvent, then under ultrasonication, will be adhered to positive and negative pole material, diaphragm and
Lithium hexafluoro phosphate in electrolyte is transferred in organic solvent；And organic solvent uses the mixture of acetonitrile and carbonic ester, can mention
Height realizes the high efficiente callback of lithium hexafluoro phosphate to the solvability of lithium hexafluoro phosphate.Embodiment the result shows that, utilization is above-mentioned
Scheme recycles the lithium hexafluoro phosphate in waste lithium cell, and the rate of recovery is up to 92% or more.
Specific embodiment
The method that the present invention provides a kind of to recycle lithium hexafluoro phosphate from waste lithium cell, includes the following steps:
(1) it will include the mixture progress ultrasound of waste lithium cell core and organic solvent, obtain Solid-liquid mixture；It is described
Organic solvent includes acetonitrile and carbonic ester；
(2) in anhydrous conditions, the Solid-liquid mixture of the step (1) is separated by solid-liquid separation, obtains extracting solution；
(3) extracting solution of the step (2) is distilled, obtains lithium hexafluoro phosphate.
The mixture of waste lithium cell core and organic solvent is carried out ultrasound by the present invention, obtains Solid-liquid mixture.This hair
The bright old and useless battery core preferably passes through dismantling waste lithium cell and obtains, and the mode of the dismantling is that those skilled in the art are ripe
The mode known；The waste lithium cell includes electric vehicle waste lithium cell or mobile phone waste lithium cell.
In the present invention, the organic solvent includes acetonitrile and carbonic ester；The volume ratio of the acetonitrile and carbonic ester is preferred
For (2~50): 100, it is further preferably (5~40): 100, more preferably (10~35): 100.
In the present invention, the carbonic ester preferably includes ethylene carbonate, propene carbonate, dimethyl carbonate and carbonic acid two
Two in one or more of ethyl ester, more preferably ethylene carbonate, propene carbonate, dimethyl carbonate and diethyl carbonate
Kind.In the present invention, when the organic solvent is the mixture of several components, the mixture is preferably acetonitrile, ethylene carbonate
The mixture or acetonitrile, carbonic acid third of the mixture or acetonitrile of ester and dimethyl carbonate, propene carbonate and dimethyl carbonate
The mixture of the mixture or acetonitrile of enester and diethyl carbonate, ethylene carbonate and diethyl carbonate.
In the present invention, the quality of core and the volume ratio of organic solvent are preferably 1g in the mixture: (20~80)
ML is further preferably 1g: (25~75) mL, more preferably 1g: (40~70) mL.
In the present invention, the frequency of the ultrasound is preferably 30~60kHz, is further preferably 33~55kHz, and more preferably 37
~50kHz；The time of the ultrasound is preferably 5~15min, is further preferably 7~12min, more preferably 8~10min.Ultrasonic mistake
The temperature of the mixture of Cheng Zhong, the core and organic solvent is preferably 15~25 DEG C, is further preferably 18~24 DEG C, more preferably
20~23 DEG C.The present invention preferably carries out ultrasound under the above conditions, can drop on the basis of guaranteeing lithium hexafluoro phosphate recovery rate
Low energy consumption, save the cost.
After obtaining Solid-liquid mixture, the present invention in anhydrous conditions, the Solid-liquid mixture is separated by solid-liquid separation, is obtained
Extracting solution.The present invention separates solidliquid mixture in anhydrous conditions, and the lithium hexafluoro phosphate that can be avoided in solidliquid mixture meets water
It decomposes, improves the rate of recovery of lithium hexafluoro phosphate；It also can be reduced lithium hexafluoro phosphate simultaneously and decompose the hydrogen fluoride gas generated to environment
Pollution.The present invention does not have particular/special requirement to the presentation mode of the anhydrous condition, using side well known to those skilled in the art
Formula.
In the present invention, the mode of the separation of solid and liquid is preferably included to filter or is centrifuged, the mode of the filtering or centrifugation
Using mode well known to those skilled in the art.
The present invention is removed large granular impurity therein, and then obtain dissolved with lithium hexafluoro phosphate by being separated by solid-liquid separation
Extracting solution.
After obtaining extracting solution, the present invention distills the extracting solution, obtains lithium hexafluoro phosphate.In the present invention, institute
Distillation to be stated preferably to be evaporated under reduced pressure, the pressure of the vacuum distillation is preferably 2050~2800Pa, further preferably for 2100~
2700Pa, more preferably 2300~2600Pa；The temperature of the vacuum distillation is preferably 80~100 DEG C, is further preferably 85~95
DEG C, more preferably 87~90 DEG C.The present invention does not have particular/special requirement to the time of the vacuum distillation, can will be organic in extracting solution
Solvent removal.
It in the present invention, further preferably include that hydrogen fluoride gas is filled with into extracting solution, so that in extracting solution before the distillation
Lithium salts be converted into lithium hexafluoro phosphate, and then improve the purity of lithium hexafluoro phosphate.The present invention is passed through mode to hydrogen fluoride gas
There is no particular/special requirement, is passed through mode using well known to those skilled in the art.
When distilling to extracting solution, fraction is also obtained, the fraction is organic solvent, and the present invention preferably will be described organic
Solvent returns to the extraction for being used for lithium hexafluoro phosphate, to improve the utilization rate of organic solvent.
The above method provided by the invention can be realized the high efficiente callback to lithium hexafluoro phosphate, and it is higher to obtain purity
Lithium hexafluoro phosphate.In the present invention, the rate of recovery >=92% of the lithium hexafluoro phosphate；The purity of the lithium hexafluoro phosphate >=
95.0%.
In the above specific embodiment, do not refer to that place uses mode well known to those skilled in the art；Agents useful for same
For commercial product well known to those skilled in the art.
In order to further illustrate the present invention, one kind provided by the invention is returned from waste lithium cell below with reference to embodiment
The method for receiving lithium hexafluoro phosphate is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
After waste lithium cell is substantially discharged, battery is adequately dried, moisture removal is removed, then dismantling is rolled up
Core mixes core with organic solvent according to dosage shown in table 1, carries out ultrasound, filtering according to technological parameter shown in table 2
Afterwards, filtrate is evaporated under reduced pressure, obtains lithium hexafluoro phosphate.
Embodiment 2~5
The lithium hexafluoro phosphate in waste lithium cell is recycled according to the method for embodiment 1, the difference is that dosage and technique
Parameter is different, before wherein embodiment 2 is evaporated under reduced pressure, is passed through hydrogen fluoride gas into gained extracting solution.Specifically it is listed in table 1~2.
1 Examples 1 to 5 dosage of each component of table
Each process parameter of 2 Examples 1 to 5 of table
As a result it characterizes
Examples 1 to 5 products obtained therefrom is analyzed using elemental analyser, the results showed that products obtained therefrom is hexafluorophosphoric acid
Lithium, characterization result are shown in Table 3.
The quality of gained lithium hexafluoro phosphate is weighed, is processing sample with the waste lithium cell of same brand and same model,
On the basis of the mass ratio of the lithium hexafluoro phosphate routinely added in model lithium battery preparation, hexafluoro phosphorus in Examples 1 to 5 is calculated
The rate of recovery of sour lithium, the results are shown in Table 3.
The characterization result of 3 Examples 1 to 5 of table
As shown in Table 3, recovery method provided by the invention can obtain the higher lithium hexafluoro phosphate of purity, and return
Yield is higher, reduces the waste of lithium resource.
As seen from the above embodiment, recovery method provided by the invention can carry out high efficiente callback to waste lithium cell, return
Receiving gained lithium hexafluoro phosphate can be used for the preparation of lithium battery, realize recycling for lithium resource；In addition, side provided by the invention
Gained organic solvent can also be used for the extraction of lithium hexafluoro phosphate after being evaporated under reduced pressure in case.
Although above-described embodiment is made that detailed description to the present invention, it is only a part of the embodiment of the present invention,
Rather than whole embodiments, people can also obtain other embodiments under the premise of without creativeness according to the present embodiment, these
Embodiment belongs to the scope of the present invention.
Claims (10)
1. a kind of method for recycling lithium hexafluoro phosphate in waste lithium cell, includes the following steps:
(1) it will include the mixture progress ultrasound of waste lithium cell core and organic solvent, obtain Solid-liquid mixture；It is described organic
Solvent includes acetonitrile and carbonic ester；
(2) in anhydrous conditions, the Solid-liquid mixture of the step (1) is separated by solid-liquid separation, obtains extracting solution；
(3) extracting solution of the step (2) is distilled, obtains lithium hexafluoro phosphate.
2. the method as described in claim 1, which is characterized in that the body of acetonitrile and carbonic ester in step (1) organic solvent
Product is than being (2~50): 100.
3. method according to claim 1 or 2, which is characterized in that the carbonic ester includes ethylene carbonate, propylene carbonate
One or more of ester, dimethyl carbonate and diethyl carbonate.
4. method according to claim 1 or 2, which is characterized in that the organic solvent replace with acetonitrile, ethylene carbonate and
The mixture or acetonitrile of dimethyl carbonate, the mixture of propene carbonate and dimethyl carbonate or acetonitrile, ethylene carbonate
With the mixture of diethyl carbonate.
5. method according to claim 1 or 2, which is characterized in that the quality of core and organic solvent in the step (1)
Volume ratio is 1g: (20~80) mL.
6. the method as described in claim 1, which is characterized in that ultrasonic frequency is 30~60kHz in the step (1), is surpassed
The time of sound is 5~15min.
7. method as described in claim 1 or 6, which is characterized in that in step (1) ultrasonic procedure, core with it is organic molten
The temperature of agent composition is 15~25 DEG C.
8. the method as described in claim 1, which is characterized in that the mode of the separation of solid and liquid of the step (2) include filtering or
Centrifugation.
9. the method as described in claim 1, which is characterized in that before step (3) distillation, further includes: to the extracting solution
In be filled with hydrogen fluoride gas.
10. the method as described in claim 1 or 9, which is characterized in that the mode distilled in the step (3) is vacuum distillation.
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| CN201811079901.9A CN109292746A (en) | 2018-09-17 | 2018-09-17 | The method of lithium hexafluoro phosphate is recycled in a kind of waste lithium cell |
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| CN201811079901.9A CN109292746A (en) | 2018-09-17 | 2018-09-17 | The method of lithium hexafluoro phosphate is recycled in a kind of waste lithium cell |
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Cited By (4)
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| CN110649344A (en) * | 2019-09-12 | 2020-01-03 | 金川集团股份有限公司 | Method for separating and recycling electrolyte in waste power lithium battery by using ultrasonic enhanced extraction method |
| CN113072584A (en) * | 2021-03-29 | 2021-07-06 | 兰州理工大学 | Method for preparing fluoro-oxalic acid phosphate by recycling electrolyte from waste lithium ion battery |
| WO2021258128A1 (en) | 2020-06-24 | 2021-12-30 | Commonwealth Scientific And Industrial Research Organisation | Electrolyte recovery |
| WO2024040906A1 (en) * | 2022-08-24 | 2024-02-29 | 广东邦普循环科技有限公司 | Method for recycling lithium-ion battery electrolyte |
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