CN106636649A - Method for recovering lithium iron phosphate cathode material from waste lithium batteries - Google Patents
Method for recovering lithium iron phosphate cathode material from waste lithium batteries Download PDFInfo
- Publication number
- CN106636649A CN106636649A CN201611064237.1A CN201611064237A CN106636649A CN 106636649 A CN106636649 A CN 106636649A CN 201611064237 A CN201611064237 A CN 201611064237A CN 106636649 A CN106636649 A CN 106636649A
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- sample
- iron phosphate
- lithium iron
- reclaimed
- waste
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
-
- 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
-
- 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
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- 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)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Secondary Cells (AREA)
- Primary Cells (AREA)
Abstract
A method for recovering a lithium iron phosphate cathode material from waste lithium batteries comprises the following steps that step 1, high-temperature baking is conducted under inert gas, an adhesive is decomposed, and foil is separated from an active material; step 2, through ultrasonic or mechanical friction, washing is conducted through deionized water or ethanol, all the residual cathode material on a pole piece is desorbed, all the cathode material is filtered and collected, a sample is dried, and the sample is ground and transferred to the next process; step 3, a carbon source is added to the sample obtained in the second step, and ball-milling is conducted till the material reaches the required grain size; step 4, under the inert gas, the sample ball-milled in the third step is re-baked at the high temperature; and step 5, in the fourth step, the re-baked sample obtained in the fourth step can be directly used as a new battery pole piece manufacturing material.
Description
【Technical field】
The present invention relates to batteries of electric automobile technical field, more particularly to a kind of iron phosphate lithium positive pole material of waste lithium cell
The method that material is reclaimed.
【Background technology】
At this stage, developing rapidly with lithium battery industry, the recycling technology of lithium battery also become everybody and extremely close
How the hot issue of note, currently reclaiming the valuable metal element in battery to the recovery principal focal point of old and useless battery.It is existing
The recovery method of waste lithium cell be to metallic element mainly using burning or acid dissolving by the way of, such method technological process
Long, equipment cost is higher, produces a large amount of waste water, serious secondary pollution is caused to environment.
In view of the above, it is necessary what the lithium iron phosphate positive material for providing a kind of new waste lithium cell was reclaimed in fact
Method overcomes disadvantages described above.
【The content of the invention】
It is an object of the invention to provide the method that a kind of lithium iron phosphate positive material of waste lithium cell is reclaimed, on the one hand,
Environmental pollution is not resulted in removal process, process is simple is with low cost, on the other hand, the recovery that the embodiment of the present invention is obtained
Sample, will not produce impurity, and organic efficiency is high and quality is good.
To achieve these goals, the present invention provides the side that a kind of lithium iron phosphate positive material of waste lithium cell is reclaimed
Method, comprises the steps：
Step one：Waste pole piece is carried out into high-temperature baking under an inert gas, is decomposed adhesive, is made foil and active substance
Separate；
Step 2：Using ultrasound or mechanical friction, using deionized water or alcohol flushing, the positive pole remained on pole piece is made
Material is all desorbed, and collects whole positive electrodes, and drying sample, sample is ground and is transferred to next work after filtration
Sequence；
Step 3：In the sample that addition carbon source is obtained in step 2, ball milling is carried out, makes material reach desired particle size big
It is little；
Step 4：Under an inert gas, by the good sample of step 3 ball milling again high-temperature baking；
Step 5：Again the sample after toasting in step 4 can be directly used for new battery pole piece making material.
Specifically, the adhesive in step one is：PVDF, baking temperature is：350 DEG C -480 DEG C, baking time is：2h-
4h。
Specifically, the carbon source in step 3 is one or more in carbon black, acetylene black, graphite and carbohydrate, institute
The adding proportion for stating carbon source is：3%-10%.
Specifically, the baking temperature in step 4 is：600 DEG C -800 DEG C, baking time is：4h-24h.
Specifically, in step one and step 4, the noble gases be nitrogen, helium, neon and argon in one kind or
It is several.
Compared with prior art, the side that a kind of lithium iron phosphate positive material of waste lithium cell that the present invention is provided is reclaimed
Method, on the one hand, environmental pollution is not resulted in removal process, process is simple is with low cost, on the other hand, the embodiment of the present invention
The recovery sample for obtaining, will not produce impurity, and organic efficiency is high and quality is good.
【Description of the drawings】
The process chart of the method that Fig. 1 is reclaimed for the lithium iron phosphate positive material that the present invention provides waste lithium cell.
Fig. 2 is recovery sample and production raw material electrical property comparison diagram.
Fig. 3 is the SEM figures that sample is recycled using the embodiment of the present invention.
Fig. 4 is comparison diagram of the XRD spectrum with standard drawing peak position that sample is recycled using the embodiment of the present invention.
【Specific embodiment】
In order that the purpose of the present invention, technical scheme and Advantageous Effects become apparent from understanding, below in conjunction with accompanying drawing and
Specific embodiment, the present invention will be described in further detail.It should be appreciated that being embodied as described in this specification
Mode is not intended to limit the present invention just for the sake of explaining the present invention.
The present invention provides a kind of method that lithium iron phosphate positive material of waste lithium cell is reclaimed, and comprises the steps：
Step one：Waste pole piece is carried out into high-temperature baking under an inert gas, is decomposed adhesive, is made foil and active substance
Separate；
Step 2：Using ultrasound or mechanical friction, using deionized water or alcohol flushing, the positive pole remained on pole piece is made
Material is all desorbed, and collects whole positive electrodes, and drying sample, sample is ground and is transferred to next work after filtration
Sequence；
Step 3：In the sample that addition carbon source is obtained in step 2, ball milling is carried out, makes material reach desired particle size big
It is little；
Step 4：Under an inert gas, the good sample of step 3 ball milling is re-started into high-temperature baking；
Step 5：Again the sample after toasting in step 4 can be directly used for new battery pole piece making material.
In a preferred embodiment, the adhesive in step one is：PVDF, baking temperature is：350 DEG C -480 DEG C,
Baking time is：2h-4h.
In a preferred embodiment, during the carbon source in step 3 is carbon black, acetylene black, graphite and carbohydrate
One or more, the adding proportion of the carbon source is：3%-10%.
In a preferred embodiment, the baking temperature in step 4 is：600 DEG C -800 DEG C, baking time is：4h-
24h。
In a preferred embodiment, in step one and step 4, the noble gases be nitrogen, helium, neon and
One or more in argon.
Embodiment：
(1) waste pole piece is toasted under nitrogen gas, decomposed P VDF (Kynoar) makes foil and active matter
Matter is separated, and baking temperature is：480 DEG C, baking time is：4h.
(2) mechanical friction is adopted, using alcohol flushing, the positive electrode remained on pole piece is all desorbed, is filtered
Whole positive electrodes, and drying sample are collected afterwards, sample is ground and is transferred to subsequent processing.
(3) add acetylene black in sample, carry out ball milling, make material reach desired particle size size, the addition ratio of acetylene black
Example be：3%.
(4) under nitrogen gas, the good sample of ball milling is re-started into baking, baking temperature is：700 DEG C, baking time
For：12h.
(5) sample after toasting again can be directly used for new battery pole piece making material.
Using key property such as Fig. 2 of the lithium iron phosphate positive material of the lithium battery obtained by the inventive method, wherein：Should
The lithium iron phosphate positive material of the lithium battery obtained with the inventive method is that (left side is recovery sample：Recovery sample, right side is：
Production raw material).
The process chart of the method that Fig. 1 is reclaimed for the lithium iron phosphate positive material that the present invention provides waste lithium cell；Fig. 2
For recovery sample and production raw material electrical property comparison diagram；Fig. 3 is the SEM figures that sample is recycled using the embodiment of the present invention；
Fig. 4 is comparison diagram of the XRD spectrum with standard drawing peak position that sample is recycled using the embodiment of the present invention.
The lithium iron phosphate positive material of the lithium battery obtained using the present embodiment can be seen that to reclaim sample by Fig. 2 to Fig. 4
Product.The recovery sample granule is more uniform, and, at 1.2 μm or so, without obvious bonding situation between granule, nothing is substantially miscellaneous for mean diameter
Mass peak, degree of crystallinity are preferable；The recovery sample is 148mAh/g as the gram volume of the lithium iron phosphate positive material of lithium battery, first
Secondary efficiency for charge-discharge is：94.62%, electrical property is showed slightly poorer to original production raw material, but meets existing commercial
LiFePO4 unit for electrical property parameters basic demand.
In sum, the method that a kind of lithium iron phosphate positive material of waste lithium cell that the present invention is provided is reclaimed, a side
Face, does not result in environmental pollution in removal process, process is simple is with low cost, and on the other hand, what the embodiment of the present invention was obtained returns
Sample is received, impurity will not be produced, organic efficiency is high and quality is good.
The present invention is not restricted to described in description and embodiment, therefore for the personnel of familiar field
Additional advantage and modification are easily achieved, therefore in the essence of the general concept limited without departing substantially from claim and equivalency range
In the case of god and scope, the present invention is not limited to specific details, representational equipment and shown here as the diagram with description
Example.
Claims (5)
1. the method that a kind of lithium iron phosphate positive material of waste lithium cell is reclaimed, it is characterised in that：Comprise the steps：
Step one：Waste pole piece is carried out into high-temperature baking under an inert gas, decomposes adhesive, foil is made with active substance point
From；
Step 2：Using ultrasound or mechanical friction, using deionized water or alcohol flushing, the positive electrode remained on pole piece is made
All it is desorbed, whole positive electrodes, and drying sample is collected after filtration, sample is ground and is transferred to subsequent processing；
Step 3：In the sample that addition carbon source is obtained in step 2, ball milling is carried out, makes material reach desired particle size size；
Step 4：Under an inert gas, the good sample of step 3 ball milling is re-started into high-temperature baking；
Step 5：Again the sample after toasting in step 4 can be directly used for new battery pole piece making material.
2. the method that the lithium iron phosphate positive material of waste lithium cell according to claim 1 is reclaimed, it is characterised in that：Step
Adhesive in rapid one is：PVDF, baking temperature is：350 DEG C -480 DEG C, baking time is：2h-4h.
3. the method that the lithium iron phosphate positive material of waste lithium cell according to claim 1 is reclaimed, it is characterised in that：Step
Carbon source in rapid three is one or more in carbon black, acetylene black, graphite and carbohydrate, the adding proportion of the carbon source
For：3%-10%.
4. the method that the lithium iron phosphate positive material of waste lithium cell according to claim 1 is reclaimed, it is characterised in that：Step
Baking temperature in rapid four is：600 DEG C -800 DEG C, baking time is：4h-24h.
5. the method that the lithium iron phosphate positive material of waste lithium cell according to claim 1 is reclaimed, it is characterised in that：Step
Rapid one and step 4 in, the noble gases be nitrogen, helium, neon and argon in one or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064237.1A CN106636649A (en) | 2016-11-25 | 2016-11-25 | Method for recovering lithium iron phosphate cathode material from waste lithium batteries |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064237.1A CN106636649A (en) | 2016-11-25 | 2016-11-25 | Method for recovering lithium iron phosphate cathode material from waste lithium batteries |
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| CN106636649A true CN106636649A (en) | 2017-05-10 |
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ID=58811666
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611064237.1A Pending CN106636649A (en) | 2016-11-25 | 2016-11-25 | Method for recovering lithium iron phosphate cathode material from waste lithium batteries |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109473748A (en) * | 2018-10-24 | 2019-03-15 | 北京工业大学 | A kind of stripping means of waste and old ternary dynamic lithium battery positive electrode and collector |
| CN110265659A (en) * | 2019-06-05 | 2019-09-20 | 山东理工大学 | The method that waste battery reclaiming prepares lithium battery tertiary cathode material |
| CN111816861A (en) * | 2020-07-29 | 2020-10-23 | 湖北融通高科先进材料有限公司 | Method for preparing lithium iron phosphate positive electrode material by using waste lithium iron phosphate pole pieces |
| CN112768799A (en) * | 2021-01-25 | 2021-05-07 | 湖北融通高科先进材料有限公司 | Method for recycling waste lithium iron phosphate positive pole piece by dry method |
| CN113707893A (en) * | 2021-08-16 | 2021-11-26 | 广西师范大学 | Carbon-based electrocatalyst prepared from waste lithium iron phosphate battery positive electrode material and preparation method and application thereof |
| CN114006065A (en) * | 2020-12-22 | 2022-02-01 | 深圳清研装备科技有限公司 | Method for recovering ceramic diaphragm of waste lithium battery |
| CN114345539A (en) * | 2021-12-31 | 2022-04-15 | 湖南江冶新能源科技股份有限公司 | Method for separating anode powder and cathode powder of waste lithium battery |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109473748A (en) * | 2018-10-24 | 2019-03-15 | 北京工业大学 | A kind of stripping means of waste and old ternary dynamic lithium battery positive electrode and collector |
| CN110265659A (en) * | 2019-06-05 | 2019-09-20 | 山东理工大学 | The method that waste battery reclaiming prepares lithium battery tertiary cathode material |
| CN111816861A (en) * | 2020-07-29 | 2020-10-23 | 湖北融通高科先进材料有限公司 | Method for preparing lithium iron phosphate positive electrode material by using waste lithium iron phosphate pole pieces |
| CN114006065A (en) * | 2020-12-22 | 2022-02-01 | 深圳清研装备科技有限公司 | Method for recovering ceramic diaphragm of waste lithium battery |
| CN114006065B (en) * | 2020-12-22 | 2024-01-26 | 深圳清研锂业科技有限公司 | Method for recycling ceramic diaphragm of waste lithium battery |
| CN112768799A (en) * | 2021-01-25 | 2021-05-07 | 湖北融通高科先进材料有限公司 | Method for recycling waste lithium iron phosphate positive pole piece by dry method |
| CN112768799B (en) * | 2021-01-25 | 2022-04-29 | 湖北融通高科先进材料有限公司 | Method for recycling waste lithium iron phosphate positive pole piece by dry method |
| CN113707893A (en) * | 2021-08-16 | 2021-11-26 | 广西师范大学 | Carbon-based electrocatalyst prepared from waste lithium iron phosphate battery positive electrode material and preparation method and application thereof |
| CN113707893B (en) * | 2021-08-16 | 2022-08-12 | 广西师范大学 | Carbon-based electrocatalyst prepared from waste lithium iron phosphate battery positive electrode material and preparation method and application thereof |
| CN114345539A (en) * | 2021-12-31 | 2022-04-15 | 湖南江冶新能源科技股份有限公司 | Method for separating anode powder and cathode powder of waste lithium battery |
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Application publication date: 20170510 |