CN110148801A - A kind of vacuum separation method of waste lithium iron phosphate battery positive plate - Google Patents
A kind of vacuum separation method of waste lithium iron phosphate battery positive plate Download PDFInfo
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- CN110148801A CN110148801A CN201910377619.7A CN201910377619A CN110148801A CN 110148801 A CN110148801 A CN 110148801A CN 201910377619 A CN201910377619 A CN 201910377619A CN 110148801 A CN110148801 A CN 110148801A
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- positive plate
- iron phosphate
- vacuum
- lithium iron
- waste lithium
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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
- 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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- Manufacturing & Machinery (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
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Abstract
A kind of vacuum separation method of waste lithium iron phosphate battery positive plate, waste lithium iron phosphate battery positive plate is cut into fluffy, fluffy useless pole piece is put into vacuum drying oven again and carries out vacuum baking, 1-6 hours are kept the temperature when temperature is 350-450 DEG C, then calcined useless pole piece is put into vibrating screen in batches, while the steel ball of different-grain diameter is added, carries out rapping screening, aluminium foil is obtained above in vibrating screen, is below the useless powder of LiFePO4.Enter in the useless powder of LiFePO4 The present invention reduces aluminium foil fragmentation in rapping screening process, while activate lithium, directly repairs recycling for LiFePO4 pyrogenic process and lay the foundation.
Description
Technical field
The present invention relates to ferric phosphate lithium cell waste positive recycling field, in particular to a kind of waste lithium iron phosphate
The vacuum separation method of battery anode slice.
Background technique
Polyanionic material LiFePO4 (LiFePO4, often it is abbreviated as LFP) and with safe and environment-friendly, stability is good, specific volume
Large size needed for the advantages that amount is high, cheap, the especially performance of its stable structure and safety are suitable for electric car etc.
Power source, it is considered to be important candidate positive electrode in power battery, electric tool and energy-storage battery has obtained widely answering
With.Therefore, the market potential of ferric phosphate lithium cell is very huge.
With skyrocketing for power battery preparation process middle and upper reaches material price, industry by sight turn to waste and old power battery this
On seat " invisible mine ".It was predicted that 2,500,000,000 will be generated to the year two thousand twenty China, about 520,000 tons of waste and old new energy resource power batteries,
Waste and old power battery by can at least provide 50% raw material supply.Meanwhile new energy resource power battery as waste electric products
Dangerous waste is set to by each country, battery various pieces have potential hazard, if dealt with improperly, it can be to environment and the mankind
Health causes serial injury.Therefore, either economically or for environmental protection above, it is necessary to carry out new energy resource power battery money
Source comprehensively utilizes work.Therefore, to using LiFePO4 as lithium ion battery (the hereinafter referred to as LiFePO4 electricity of positive electrode
Pond) carry out recycling will become particularly important.
CN201510372381.0, which is disclosed, to be recycled battery-grade iron phosphate and utilizes waste and old phosphorus in a kind of ferric phosphate lithium cell
The method that sour lithium iron battery prepares lithium iron phosphate positive material, by lithium iron phosphate positive material crush be heat-treated, acid adding leach and
Alkali is added to adjust the recycling that pH carries out ferric phosphate, then plus alkali, sodium carbonate prepare lithium carbonate, last ferric phosphate, sodium carbonate and carbon dust
Also calcining obtains lithium iron phosphate positive material.
103280610 A of CN discloses the comprehensive recovering process and process of a kind of lithium iron phosphate positive material, LiFePO4
Anode is first dissolved aluminium foil with excessive lye, and filtered filtration residue is soak 12 hours realization lithium, iron in 50 DEG C of acid in temperature
It separates, precipitating obtains lithium carbonate after sodium carbonate is added after filtrate adjusting pH, and addition is big after excess acid dissolution is added in the insoluble slag of iron
Amount lye adjusts pH and generates iron hydroxide.
105244564 A of CN discloses a kind of recoverying and utilizing method of lithium iron phosphate dynamic battery, comprising: by ferric phosphate
Positive/negative plate, diaphragm and shell are isolated after lithium dynamical battery electric discharge, dismantling, directly recycling diaphragm and shell；Negative electrode tab crushes
By ultrasound, stir process, copper sheet is recycled after filtering.Positive plate uses organic acid solution to carry out Leach reaction, mistake after pulverizing and sieving
It realizes after filter and is separated containing lithium, aluminum solutions with filter residues such as organic acid molysite, carbon black, binders；Lye is added into filtrate, obtains Al
(OH)3It precipitates and is separated with lithium-containing solution；Lithium will can be recycled after the processing of gained lithium-containing solution；Solution after sinker passes through crystallization step
Suddenly organic acid sodium salt product is obtained.
Patent CN200710076890.4 (a kind of comprehensive recovering process of positive pole waste tablet from ferric phosphate lithium cell), patent
A kind of regeneration method of iron phosphate lithium positive pole waste material of CN200710077245.4(), a kind of LiFePO4 of patent CN10138441A(
The comprehensive recovering process of anode waste paper) a kind of regeneration method of iron phosphate lithium positive pole waste material of patent CN10394015A(), specially
A kind of sharp recovery method of lithium iron phosphate anode material from lithium ionic cell waste of 200710129898.2(), patent CN
A kind of recovery method of lithium iron phosphate anode material from lithium ionic cell waste of 101359756A() will produce in be collected into
Positive waste paper or useless powder etc. are crushed, subsequently heat-treated to remove the simple process such as most conductive agent and binder, are obtained
The ground obtained iron phosphate lithium positive pole reclaimed materials of positive electrode.Above-mentioned 6 patents are recovered as full pyrogenic process recycling.
Currently, the most of method of ferric phosphate lithium cell recovery technology research delivered be pyrometallurgy calcination and regeneration and
Hydrometallurgical recovery valuable metal.Wherein the positive electrode of pyrogenic process calcination and regeneration is since it contains other impurities element such as Al content
It is excessively high, so that regenerated performance of lithium ion battery is bad.Therefore the hydrometallurgical processing method in later period was used in selection
Amount strong acid is when leaching the ion in battery completely, to increase it is a set of remove aluminium process, and Al is difficult to eliminate completely, although the leaching of its Li
Extracting rate is higher, but the later period needs a large amount of lye to go to neutralize excessive acid solution early period so causing process route complexity, and
Increase cost；But for renovation technique direct for pyrogenic process, because Al content is excessively high, the LiFePO4 product after reparation reaches completely
Less than the requirement of the national standard of LiFePO4 product.
Therefore, how to find it is a kind of so that LiFePO4 is given up the adhesive failure on pole piece, thus reach aluminium foil and
The method that the useless powder of LiFePO4 is separated realizes that Al content is below 0.05% in LiFePO4 and aluminium recycles entirely respectively, thus
Reaching the later period, directly to repair the ingredient requirement of high quality LiFePO4 using wet process synthetical recovery or pyrogenic process be to need further to be visited
The problem of rope.
Summary of the invention
It is an object of the invention to for the deficiencies of the prior art, provide a kind of the true of waste lithium iron phosphate battery positive plate
Empty separation method, this method is environmentally friendly, pollution-free, simple and easy it is not necessary that remaining medicament is added, and has maximally utilized on useless pole piece
Useful resources, the rate of recovery of aluminium are more than 99.5%, and the rate of recovery of LiFePO4 is more than 99%, and process is simple, and LiFePO4 gives up in powder
The new impurity including Al is not introduced, is reduced the process except Al for later period hydrometallurgic recovery LiFePO4, is particularly useful for phosphorus
The pyrogenic process of sour iron lithium, which is directly repaired, to be obtained the LiFePO4 product of high quality and lays the foundation.
The present invention is achieved by the following technical programs:
A kind of vacuum separation method of waste lithium iron phosphate battery positive plate, which comprises the following steps:
Step A, it shears: waste lithium iron phosphate battery positive plate cut into the fragment or strip of 30-40 centimeter length, simultaneously
The positive plate sheared is separated into fluffy.
Step B, it pre-processes: the resulting fluffy useless pole piece of step A being put into vacuum drying oven, vacuum drying oven is evacuated
State is shown in the vacuum degree on the vacuum meter in vacuum drying oven between 0.5-0.9, and burner hearth is at negative pressure.
Step C, vacuum baking: heating up to the resulting vacuum drying oven of step B, the heat preservation when temperature reaches 350-450 DEG C
1-6 hours, the useless pole piece after being roasted.
Step D, rapping separates: the resulting calcined useless pole piece of step C being put into vibrating screen in batches, while 1-3 is added
The steel ball of kilogram diameter different-grain diameter between 5-15 millimeters respectively, carries out rapping screening, and aluminium foil is obtained above in vibrating screen, under
Face is the useless powder of LiFePO4.
As a further refinement of the present invention, the waste lithium iron phosphate battery positive plate in the step A wraps respectively
It includes the useless pole piece generated in the preparation process of positive plate, in cell manufacturing process and is removed from waste lithium iron phosphate battery
Positive plate.
As a further refinement of the present invention, the vacuum degree in the step B refers to gas molecule in a space
(an atmospheric pressure 101325pa, i.e. 0.1MPa, vacuum meter are shown as " 0 ") is few under several density ratio standard state, and vacuum degree is
0.5-0.9 indicates that actual pressure is 0.05-0.01MPa.
As a further refinement of the present invention, the heating rate in the step C is to rise 12-24 DEG C per minute,
Heating-up time is 15-30 minutes.
As a further refinement of the present invention, the sieve of the vibrating screen in the step D is respectively 5-100 mesh, vibration
Beating frequency is under 60-120 per minute, and the content of Al is below 0.05% in the useless powder of gained LiFePO4.
Preferably, the optional 20-50 mesh of the sieve of vibrating screen, and the steel ball of rapping uses zirconia ball, the diameter of zirconium ball
The ball of different-grain diameter between 5-15 millimeters.
Compared with prior art, the beneficial effects of the present invention are:
1, recycle object of the invention is iron phosphate lithium positive pole piece, to the source of positive plate (including in preparation, processing or battery
Disassemble) etc. without particular/special requirement, therefore to the recycling of iron phosphate lithium positive pole piece without dead angle, yield is big, has saved resource, shuts out
Pollution of the iron phosphate lithium positive pole piece to environment absolutely.
2, it is roasted under the protective effect that the present invention passes through vacuum state anaerobic situation, binder is more volatile and fails, and reaches
To the purpose of removing；It ensure that the active metal aluminium in positive plate is not oxidized, original toughness of aluminium is retained, to reach
The LiFePO4 powder that gives up is removed to greatest extent from aluminium foil, and aluminium and LiFePO4 have respectively obtained recycling, the rate of recovery surpasses respectively
99.5% and 99% are crossed, while ensure that the pyrogenic process of later period LiFePO4 is directly repaired or hydrometallurgic recovery.
3, the separation of waste lithium iron phosphate positive plate and recycling has that rational technology, processing cost be low, pollution-free, nonhazardous
The advantages that, while without adding remaining chemical agent, prevent the generation of the three wastes, Al contains in the useless powder of isolated LiFePO4
Amount is below 0.05%；And by-product aluminium foil is free of LiFePO4 powder, can be used as product take-away, therefore application prospect is boundless.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, invention is further described in detail.It should be appreciated that specific embodiment described herein is used only for explaining this
Invention, is not intended to limit the present invention, and the present invention includes other embodiment and and its deformation within the scope of its technical idea.
In the present invention, sometimes according to power battery it is the difference of the materials such as LiMn2O4, ternary or cobalt acid lithium, or reduces and cut
It cuts, or increases the LiFePO4 after separation and give up the destruction step of powder, but as long as typical process flow is constant, then this hair
It is bright also to apply.
The embodiment of the invention provides a kind of vacuum separation methods of waste lithium iron phosphate battery positive plate, please refer to Fig. 1.
Below by specific embodiment, invention is further explained.
Embodiment 1
Step A, it shears: waste lithium iron phosphate battery positive plate being cut into the fragment or strip of 30 centimeter lengths, and is separated into pine
Bulk obtains fluffy useless pole piece.
Step B, it pre-processes: being first put into fluffy useless pole piece into vacuum drying oven, then vacuum drying oven vacuum state, make
The vacuum degree of vacuum drying oven is 0.5.
Step C, vacuum baking: heating up to vacuum drying oven, and heating rate is to rise 12 DEG C per minute, the heating-up time 30
Minute, 6 hours are kept the temperature when temperature reaches 350 DEG C, the useless pole piece after being roasted.
Step D, rapping separates: calcined useless pole piece being put into batches in the vibrating screen that sieve is 5 mesh, and it is public to be added 1
The steel ball of the jin diameter different-grain diameter between 5-15 millimeter respectively, progress rapping screening, has respectively obtained aluminium foil and ferric phosphate
Lithium gives up powder.
By the separation and recovery of waste lithium iron phosphate positive plate, the rate of recovery of LiFePO4 and aluminium foil is respectively 99.7% He
99.6%, gained LiFePO4 give up powder in Al content be 0.012%.
Embodiment 2
Step A, it shears: waste lithium iron phosphate battery positive plate being cut into the fragment or strip of 35 centimeter lengths, and be separated into pine
Bulk.
Step B, it pre-processes: being first put into fluffy useless pole piece into vacuum drying oven, then vacuum drying oven vacuum state, make
The vacuum degree of vacuum drying oven is 0.7.
Step C, vacuum baking: heating up to vacuum drying oven, and heating rate is to rise 20 DEG C per minute, the heating-up time 21
Minute, 1 hour is kept the temperature when temperature reaches 420 DEG C, the useless pole piece after being roasted.
Step D, rapping separates: calcined useless pole piece being put into batches in the vibrating screen that sieve is 60 mesh, and it is public to be added 2
The steel ball of the jin diameter different-grain diameter between 5-15 millimeter respectively, progress rapping screening, has respectively obtained aluminium foil and ferric phosphate
Lithium gives up powder.
By the separation and recovery of waste lithium iron phosphate positive plate, the rate of recovery of LiFePO4 and aluminium foil is respectively 99.3% He
99.9%, gained LiFePO4 give up powder in Al content be 0.008%.
Embodiment 3
Step A, it shears: waste lithium iron phosphate battery positive plate being cut into 40 centimeter lengths, and is separated into fluffy.
Step B, it pre-processes: being first put into fluffy useless pole piece into vacuum drying oven, then vacuum drying oven vacuum state, make
The vacuum degree of vacuum drying oven is 0.9.
Step C, vacuum baking: heating up to vacuum drying oven, and heating rate is to rise 24 DEG C per minute, the heating-up time 15
Minute, 4 hours are kept the temperature when temperature reaches 380 DEG C, the useless pole piece after being roasted.
Step D, rapping separates: calcined useless pole piece being put into the vibrating screen that sieve is 100 mesh in batches, and is added 3
The steel ball of kilogram diameter different-grain diameter between 5-15 millimeters respectively, carries out rapping screening, has respectively obtained aluminium foil and phosphoric acid
Iron lithium gives up powder.
By the separation and recovery of waste lithium iron phosphate positive plate, the rate of recovery of LiFePO4 and aluminium foil is respectively 99.7% He
99.6%, gained LiFePO4 give up powder in Al content be 0.007%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (5)
1. a kind of vacuum separation method of waste lithium iron phosphate battery positive plate, which comprises the following steps:
A, it shears: waste lithium iron phosphate battery positive plate being cut into 30-40 centimetres of length, while the positive plate sheared
It is separated into fluffy；
B, it pre-processes: the resulting fluffy useless pole piece of step A being put into vacuum drying oven, vacuum drying oven vacuum state makes
Vacuum degree in vacuum drying oven is between 0.5-0.9, and the burner hearth of vacuum drying oven is at negative pressure；
C, vacuum baking: heating up to the resulting vacuum drying oven of step B, keeps the temperature 1-6 hours when temperature reaches 350-450 DEG C,
Useless pole piece after being roasted；
D, rapping separates: the useless pole piece after the resulting roasting of step C being put into vibrating screen in batches, while 1-3 kilograms of diameter is added
The steel ball of different-grain diameter between 5-15 millimeters respectively carries out rapping screening, and aluminium foil is obtained above in vibrating screen, is below phosphoric acid
Iron lithium gives up powder.
2. a kind of vacuum separation method of waste lithium iron phosphate battery positive plate according to claim 1, it is characterised in that:
Waste lithium iron phosphate battery positive plate in the step A is the useless pole piece produced during the preparation process of positive plate, battery system
One of the standby useless pole piece generated in the process, the positive plate removed from waste lithium iron phosphate battery are a variety of.
3. a kind of vacuum separation method of waste lithium iron phosphate battery positive plate according to claim 1, it is characterised in that:
Vacuum degree in the step B refers to that the density in a space under the density ratio standard state of gas molecula number is small, vacuum
Degree is that 0.5-0.9 indicates that actual pressure is 0.05-0.01MPa.
4. a kind of vacuum separation method of waste lithium iron phosphate battery positive plate according to claim 1, it is characterised in that:
In the step C, the heating rate of vacuum drying oven is to rise 12-24 DEG C per minute, and the heating-up time is 15-30 minutes.
5. a kind of vacuum separation method of waste lithium iron phosphate battery positive plate according to claim 1, it is characterised in that:
The sieve of vibrating screen in the step D is respectively 5-100 mesh, and rapping frequency is gained ferric phosphate under 60-120 per minute
The content of Al is below 0.05% in the useless powder of lithium.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111411233A (en) * | 2020-03-30 | 2020-07-14 | 安徽元琛环保科技股份有限公司 | Method for separating waste lithium battery positive electrode material and current collector by vacuum aluminum evaporation |
| CN112234272A (en) * | 2020-09-22 | 2021-01-15 | 华中科技大学 | Low-energy-consumption and low-Al-content recovery method for lithium iron phosphate positive plate |
| CN112225191A (en) * | 2020-10-09 | 2021-01-15 | 武汉瑞科美新能源有限责任公司 | Method for degrading PVDF in positive electrode of waste lithium iron phosphate battery |
| CN112599766A (en) * | 2020-12-14 | 2021-04-02 | 台州市宸明新能源科技有限公司 | Regeneration process of waste lithium iron phosphate battery positive electrode material |
| CN112713328A (en) * | 2020-12-25 | 2021-04-27 | 华南理工大学 | Method for separating and recycling aluminum foil and positive active material in retired lithium ion power battery |
| CN113247875A (en) * | 2021-05-24 | 2021-08-13 | 中国恩菲工程技术有限公司 | Method for extracting phosphorus and iron from iron phosphate slag |
| CN114361637A (en) * | 2022-01-14 | 2022-04-15 | 中南大学 | Method for separating electrode material and foil of lithium battery |
| CN116715213A (en) * | 2023-08-10 | 2023-09-08 | 河北顺境环保科技有限公司 | Recycling treatment method of non-injected lithium iron phosphate waste sheet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111411233A (en) * | 2020-03-30 | 2020-07-14 | 安徽元琛环保科技股份有限公司 | Method for separating waste lithium battery positive electrode material and current collector by vacuum aluminum evaporation |
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| CN112234272A (en) * | 2020-09-22 | 2021-01-15 | 华中科技大学 | Low-energy-consumption and low-Al-content recovery method for lithium iron phosphate positive plate |
| CN112234272B (en) * | 2020-09-22 | 2022-02-18 | 华中科技大学 | Low-energy-consumption and low-Al-content recovery method for lithium iron phosphate positive plate |
| CN112225191A (en) * | 2020-10-09 | 2021-01-15 | 武汉瑞科美新能源有限责任公司 | Method for degrading PVDF in positive electrode of waste lithium iron phosphate battery |
| CN112599766A (en) * | 2020-12-14 | 2021-04-02 | 台州市宸明新能源科技有限公司 | Regeneration process of waste lithium iron phosphate battery positive electrode material |
| CN112713328A (en) * | 2020-12-25 | 2021-04-27 | 华南理工大学 | Method for separating and recycling aluminum foil and positive active material in retired lithium ion power battery |
| CN113247875A (en) * | 2021-05-24 | 2021-08-13 | 中国恩菲工程技术有限公司 | Method for extracting phosphorus and iron from iron phosphate slag |
| CN113247875B (en) * | 2021-05-24 | 2022-11-25 | 中国恩菲工程技术有限公司 | Method for extracting phosphorus and iron from iron phosphate slag |
| CN114361637A (en) * | 2022-01-14 | 2022-04-15 | 中南大学 | Method for separating electrode material and foil of lithium battery |
| CN116715213A (en) * | 2023-08-10 | 2023-09-08 | 河北顺境环保科技有限公司 | Recycling treatment method of non-injected lithium iron phosphate waste sheet |
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