CN106241769A - A kind of method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet - Google Patents
A kind of method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet Download PDFInfo
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- CN106241769A CN106241769A CN201610583274.7A CN201610583274A CN106241769A CN 106241769 A CN106241769 A CN 106241769A CN 201610583274 A CN201610583274 A CN 201610583274A CN 106241769 A CN106241769 A CN 106241769A
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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
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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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Abstract
The present invention discloses a kind of method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet, comprises the steps: to pulverize after waste and old ferrous phosphate lithium battery anode sheet roasting, and positive pole aluminium flake is reclaimed in screening, obtains LiFePO 4 waste slurry；Being soaked in deionized water by LiFePO 4 waste slurry, conductive agent is removed in flotation, obtains the mixture of LiFePO 4 and binding agent；Add mixture in the mixed liquor of N methyl pyrrolidone and hydrochloric acid, extract binding agent, obtain the thick product of LiFePO 4；Add heat extraction N methyl pyrrolidone NMP and hydrochloric acid；Filter, wash, be dried to obtain LiFePO 4.The present invention progressively removes or separates conductive agent, binding agent, thus obtains the thick product of LiFePO 4；The operation simple, easy of this method not only step, low cost, and both avoided the energy consumption problem of high-temperature roasting, the impurity that turn avoid sour molten precipitation is difficult to except clean problem, thus is advantageously implemented industrialization.
Description
Technical field
The invention belongs to waste and old lithium ion battery recovery and utilization technology field, relate to a kind of from waste and old ferrous phosphate lithium battery
Positive plate reclaims the method for ferrousphosphate lithium material.
Background technology
Lithium ion battery is the green battery with a series of premium properties, since coming out, has been widely used.Phosphoric acid
Ferrous lithium material, owing to having the advantages such as high safety, high-environmental, high-energy-density, low price, long-life, becomes generally acknowledged lithium ion
The preferred material of electrokinetic cell, and the lithium ion battery with LiFePO 4 as positive electrode has been widely used in electronic work
The electrokinetic cell fields such as tool, electric bicycle, vehicle using motor, golf hurdle, ship model toy, mine lamp.Along with LiFePO 4
For the application of the lithium rechargeable battery of positive electrode, the yield of battery is quickly increasing, and meeting during preparing battery
Produce a large amount of waste slurry and useless pole piece.Therefore, for recycling material, cost-effective and protect environment, reclaim in waste material
LiFePO 4 become the most necessary.The common technology reclaiming LiFePO 4 mainly includes roasting direct, sour molten precipitation
Deng.
At present, the mode of roasting direct is used to reclaim LiFePO 4.Such as, Chinese patent application
200710129898.2, the recovery method of lithium iron phosphate cathode material in a kind of lithium ion battery waste material, it is by described waste material
Toasting 2-5h under the atmosphere of noble gas at 450-600 DEG C, the powdered product then baking obtained adds soluble iron
In the ethanol solution of salt mix, be dried, finally under the atmosphere of noble gas at 300-500 DEG C roasting 2-5h, recovery obtains
Lithium iron phosphate cathode material.Although the method is simple, but energy consumption is slightly higher, and reclaims the purity of the LiFePO 4 obtained relatively
Low, directly can not use as cell positive material.
The mode using sour molten precipitation reclaims LiFePO 4.Such as, Chinese patent application 201010253859.5, a kind of
The method that LiFePO 4 is prepared in water-system waste lithium-ion-power cell recovery, it specifically comprises the following steps that 1) by water-system waste lithium
After ion battery shearing-crushing, deionized water processing, sieve dried recovery electrode material and conductive agent mixture；2) will be dry
Electrode material and conductive agent mixture after dry add mineral acid and process, and are filtrated to get Li+、Fe2+、PO4 3-Acidity molten
Liquid；3) to containing Li+、Fe2+、PO4 3-Acid solution in add lithium salts or iron salt, add ascorbic acid stirring, control ph 3-
7；Filter, be precipitated；4) by step 3) LiFePO that obtains4Thick product joins and carries out ball milling in aqueous sucrose solution, is dried
Calcining obtains the LiFePO of regeneration4Material.The method does not produce secondary pollution, but impurity is difficult to except clean so that the product of raw material
Qualitative changeization is very big, causes homogeneity of product to hardly result in guarantee, it is impossible to meets industrialized great production and reclaims the need of LiFePO 4
Want.
Therefore, research to the recycling of waste lithium ion cell anode material at present remains society's common concern
Hot issue.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of and reclaims phosphoric acid Asia from waste and old ferrous phosphate lithium battery anode sheet
The method of ferrum lithium material.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet, it is characterised in that the method
Comprise the steps:
(1) pretreatment: will pulverize after waste and old ferrous phosphate lithium battery anode sheet roasting, positive pole aluminium flake is reclaimed in screening, obtains phosphoric acid sub-
Ferrum lithium waste slurry；
(2) flotation: LiFePO 4 waste slurry is soaked in deionized water, under certain condition stirring or sonic oscillation one
Fixing time, conductive agent is removed in flotation, obtains the mixture of LiFePO 4 and binding agent；
(3) extraction: LiFePO 4 step (2) obtained and the mixture of binding agent join N-Methyl pyrrolidone and salt
In the mixed liquor of acid, stirring or sonic oscillation 1-3h, static 2h under room temperature, extract binding agent, obtain LiFePO 4 and slightly produce
Product；
(4) remove impurity: LiFePO 4 thick product reacting by heating step (3) obtained, removes N-Methyl pyrrolidone NMP and salt
Acid；
(5) LiFePO 4 is reclaimed: filter, wash, be dried to obtain LiFePO 4.
Described step (1) sintering temperature is 300-400 DEG C, and roasting time is 1-4h.
Described step (2) stirring or the ultrasonic temperature swung are 20-100 DEG C, and the time is 1-3h.
The mixed liquor of the mixture of described step (3) LiFePO 4 and binding agent and N-Methyl pyrrolidone and hydrochloric acid
Mass ratio be the volume ratio of 10:6-7, N-Methyl pyrrolidone and hydrochloric acid be 1:1.
In described step (4), heating-up temperature is 100-220 DEG C, reacts 1-2h.
Described step (5) washing is deionized water wash 2-3 time, and baking temperature is 80 DEG C.
The composition of LiFePO 4 waste slurry comprises: LiFePO 4, conductive agent, binding agent；In extraction process, phosphoric acid is sub-
Ferrum lithium is dissolved in dilute hydrochloric acid, and binding agent is dissolved in N-Methyl pyrrolidone, thus realizes the separation of LiFePO 4 and binding agent,
Thick product to LiFePO 4；In dedoping step, the thick product of LiFePO 4 is heated to 100-220 DEG C, N-methyl pyrrole
Pyrrolidone and hydrochloric acid vapor away, remaining LiFePO 4.
Beneficial effects of the present invention: the present invention constitutes angle from this composition of LiFePO 4 waste slurry and considers, uses
Conductive agent, binding agent are progressively removed or separated to suitable method, thus obtains the thick product of LiFePO 4；This method not only walks
Rapid operation simple, easy, low cost, and both avoided the energy consumption problem of high-temperature roasting, the impurity that turn avoid sour molten precipitation is difficult
With except clean problem, thus it is advantageously implemented industrialization.
Accompanying drawing explanation
Fig. 1 is the flow chart of the detailed description of the invention of recovery process of the present invention.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the design of the present invention, technology path etc. are carried out clear, complete description, to fill
The sub-argument solution purpose of the present invention, feature and effect.Based on embodiments of the invention, others skilled in the art are not paying creative labor
Other embodiments obtained on the premise of Dong, belong to the scope of protection of the invention.Each technology in the invention is special
Levy, can be with combination of interactions on the premise of the most conflicting conflict.
The object of the present invention is the ferrous lithium phosphate cathode waste slurry produced in lithium ion battery manufacture process and phosphoric acid Asia
Ferrum lithium gives up positive plate and waste and old ferrous phosphate lithium battery.
Embodiment 1
As it is shown in figure 1, a kind of method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet, including as follows
Step:
1, pretreatment: pulverized after 400 DEG C of roasting temperature 4h by waste and old ferrous phosphate lithium battery anode sheet, positive pole is reclaimed in screening
Aluminium flake, obtains LiFePO 4 waste slurry.
2, flotation: process positive pole waste slurry with deionized water, stirring or sonic oscillation 1h at 100 DEG C, flotation is removed
Conductive agent, obtains the mixture of LiFePO 4 and binding agent.
3, extraction: the mixture of LiFePO 4 obtained above and binding agent is joined N-Methyl pyrrolidone and salt
In the mixed liquor of acid, the mixture of LiFePO 4 and binding agent with the mass ratio of N-Methyl pyrrolidone and hydrochloric acid mixed solution is
10:6, N-Methyl pyrrolidone is 1:1 with the volume ratio of hydrochloric acid, and stirring or sonic oscillation 1h, static 2h under room temperature, by extraction
The existing LiFePO 4 for the treatment of excess syndrome and the separation of binding agent, obtain the thick product of LiFePO 4.
4, remove impurity: the thick product of LiFePO 4 obtained above is heated to 220 DEG C, reacts 1h, removes N-methyl pyrrole
Pyrrolidone and hydrochloric acid.
5, LiFePO 4 is reclaimed: above-mentioned gained liquid is filtered, deionized water wash three times, is dried under the conditions of 80 DEG C
To LiFePO 4.
Waste and old ferrous phosphate lithium battery anode sheet first carries out the process of following steps:
Waste and old ferrous phosphate lithium battery remaining capacity is discharged, then disassembles battery, take out positive plate so that old and useless battery negative pole
In reversible lithium ion be transferred to positive plate, now positive plate forms the higher LiFePO 4 of lithium content.
Embodiment 2
1, pretreatment: pulverized after 300 DEG C of roasting temperature 4h by waste and old ferrous phosphate lithium battery anode sheet, positive pole is reclaimed in screening
Aluminium flake, obtains LiFePO 4 waste slurry.
2, flotation: process positive pole waste slurry with deionized water, stirring or sonic oscillation 3h at 20 DEG C, flotation is removed and is led
Electricity agent, obtains the mixture of LiFePO 4 and binding agent.
3, extraction: the LiFePO 4 that step 1 is obtained and the mixture of binding agent join N-Methyl pyrrolidone and
In the mixed liquor of hydrochloric acid, the mixture of LiFePO 4 and binding agent and N-Methyl pyrrolidone and the mass ratio of hydrochloric acid mixed solution
For 10:7, N-Methyl pyrrolidone is 1:1 with the volume ratio of hydrochloric acid, and under room temperature, stirring or sonic oscillation 3h, static 2h, pass through
Extraction realizes the separation of LiFePO 4 and binding agent, obtains the thick product of LiFePO 4.
4, remove impurity: the thick product of LiFePO 4 step 3 obtained is heated to 100 DEG C, reacts 2h, removes N-methyl pyrrole
Pyrrolidone and hydrochloric acid.
5, reclaim LiFePO 4: to filtrations of step 4 gained liquid, deionized water wash secondary, under the conditions of 80 DEG C dry
Obtain LiFePO 4.
The above is only the detailed description of the invention of the application, it is noted that for the ordinary skill people of the art
For Yuan, on the premise of without departing from the application principle, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as the protection domain of the application.
Claims (6)
1. the method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet, it is characterised in that the party
Method comprises the steps:
(1) pretreatment: will pulverize after waste and old ferrous phosphate lithium battery anode sheet roasting, positive pole aluminium flake is reclaimed in screening, obtains phosphoric acid sub-
Ferrum lithium waste slurry；
(2) flotation: LiFePO 4 waste slurry is soaked in deionized water, under certain condition stirring or sonic oscillation one
Fixing time, conductive agent is removed in flotation, obtains the mixture of LiFePO 4 and binding agent；
(3) extraction: LiFePO 4 step (2) obtained and the mixture of binding agent join N-Methyl pyrrolidone and salt
In the mixed liquor of acid, stirring or sonic oscillation 1-3h, static 2h under room temperature, extract binding agent, obtain LiFePO 4 and slightly produce
Product；
(4) remove impurity: LiFePO 4 thick product reacting by heating step (3) obtained, removes N-Methyl pyrrolidone NMP and salt
Acid；
(5) LiFePO 4 is reclaimed: filter, wash, be dried to obtain LiFePO 4.
The method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet the most according to claim 1,
It is characterized in that, described step (1) sintering temperature is 300-400 DEG C, and roasting time is 1-4h.
The method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet the most according to claim 1,
It is characterized in that, described step (2) stirring or the ultrasonic temperature swung are 20-100 DEG C, and the time is 1-3h.
The method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet the most according to claim 1,
It is characterized in that, the mixture of described step (3) LiFePO 4 and binding agent and N-Methyl pyrrolidone and the mixing of hydrochloric acid
The mass ratio of liquid be the volume ratio of 10:6-7, N-Methyl pyrrolidone and hydrochloric acid be 1:1.
The method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet the most according to claim 1,
It is characterized in that, in described step (4), heating-up temperature is 100-220 DEG C, reacts 1-2h.
The method reclaiming ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet the most according to claim 1,
It is characterized in that, described step (5) washing is deionized water wash 2-3 time, and baking temperature is 80 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394302A (en) * | 2017-07-27 | 2017-11-24 | 合肥国轩高科动力能源有限公司 | A kind of separation method of waste and old nickle cobalt lithium manganate battery battery core roasting material |
| CN107464963A (en) * | 2017-07-27 | 2017-12-12 | 合肥国轩高科动力能源有限公司 | A kind of method that valuable material is efficiently separated from waste lithium cell |
| CN109004305A (en) * | 2017-06-06 | 2018-12-14 | 湖南省正源储能材料与器件研究所 | The method of LiFePO 4 and free carbon is separated in a kind of cathode mixture |
| CN110635191A (en) * | 2019-09-12 | 2019-12-31 | 金川集团股份有限公司 | Method for cleanly recovering all components of waste power lithium battery |
| 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 |
| CN111088430A (en) * | 2019-12-26 | 2020-05-01 | 甘肃睿思科新材料有限公司 | Recovery processing method of waste slurry of lithium battery positive electrode |
| CN113991204A (en) * | 2021-10-22 | 2022-01-28 | 国网黑龙江省电力有限公司电力科学研究院 | Short-process recovery method of waste lithium iron phosphate anode material |
| WO2022252602A1 (en) * | 2021-05-31 | 2022-12-08 | 广东邦普循环科技有限公司 | Method for safely leaching waste battery and application |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109004305A (en) * | 2017-06-06 | 2018-12-14 | 湖南省正源储能材料与器件研究所 | The method of LiFePO 4 and free carbon is separated in a kind of cathode mixture |
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| CN107394302A (en) * | 2017-07-27 | 2017-11-24 | 合肥国轩高科动力能源有限公司 | A kind of separation method of waste and old nickle cobalt lithium manganate battery battery core roasting material |
| CN107464963A (en) * | 2017-07-27 | 2017-12-12 | 合肥国轩高科动力能源有限公司 | A kind of method that valuable material is efficiently separated from waste lithium cell |
| CN107464963B (en) * | 2017-07-27 | 2019-08-09 | 合肥国轩高科动力能源有限公司 | A method of efficiently separating valuable material from waste lithium cell |
| CN107394302B (en) * | 2017-07-27 | 2019-09-27 | 合肥国轩高科动力能源有限公司 | A kind of separation method of waste and old nickle cobalt lithium manganate battery battery core roasting material |
| CN110635191A (en) * | 2019-09-12 | 2019-12-31 | 金川集团股份有限公司 | Method for cleanly recovering all components of waste power lithium battery |
| 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 |
| CN111088430A (en) * | 2019-12-26 | 2020-05-01 | 甘肃睿思科新材料有限公司 | Recovery processing method of waste slurry of lithium battery positive electrode |
| WO2022252602A1 (en) * | 2021-05-31 | 2022-12-08 | 广东邦普循环科技有限公司 | Method for safely leaching waste battery and application |
| CN113991204A (en) * | 2021-10-22 | 2022-01-28 | 国网黑龙江省电力有限公司电力科学研究院 | Short-process recovery method of waste lithium iron phosphate anode material |
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