CN111977628A - Method for recovering and preparing lithium iron phosphate from lithium ion battery - Google Patents
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- CN111977628A CN111977628A CN202010922773.0A CN202010922773A CN111977628A CN 111977628 A CN111977628 A CN 111977628A CN 202010922773 A CN202010922773 A CN 202010922773A CN 111977628 A CN111977628 A CN 111977628A
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention provides a method for recovering and preparing lithium iron phosphate from a lithium ion battery, which comprises the following steps: s1: discharging the retired lithium iron phosphate battery, disassembling the discharged lithium iron phosphate battery to obtain a battery anode, crushing and screening the battery anode, and then performing air flow sorting to obtain lighter powder; s2: carrying out oxidation leaching on the powder obtained in the step S1 to obtain filtrate and filter residue containing metal ions, phosphate ions and acid radical ions; s3: adding phosphoric acid into the filtrate obtained in the step S2 to obtain an iron phosphate precipitate containing an aluminum element, wherein the iron phosphate precipitate is used as a precursor for preparing the lithium iron phosphate material; s4: mixing the precursor obtained in the step S3 with a lithium source to obtain a mixture; s5: and grinding the mixture obtained in the step S4 and a carbon source uniformly, and then sintering at a high temperature in an inert atmosphere to obtain the aluminum-doped lithium iron phosphate cathode material. The preparation method has the advantages of short preparation flow, low cost and strong operability, and the prepared lithium iron phosphate anode material has excellent performance and higher application value.
Description
Technical Field
The invention relates to the technical field of energy storage materials, in particular to a method for recycling and preparing lithium iron phosphate from a lithium ion battery.
Background
Since 1991, the commercialization of lithium ion batteries was first achieved by the japan sony corporation, lithium ion batteries have the advantages of high discharge voltage, large specific energy, small self-discharge, long cycle life, no memory effect, etc., and have gradually replaced the conventional secondary power source, and are widely used in the fields of portable electronic devices, electric vehicles, space technology, defense industry, etc. The lithium iron phosphate battery has the advantages of good safety, low cost, no toxicity and the like, and gradually occupies a leading position in the lithium ion battery market.
With the popularization of electric vehicles, the number of retired batteries is rapidly increased, environmental pollution and resource waste are caused by direct discarding, and how to properly recycle the retired batteries becomes a key point of attention of people. Patent CN111370800A discloses that after processing a lithium iron phosphate positive plate, iron phosphate, iron hydroxide and lithium carbonate are obtained, and the obtained iron phosphate is not doped with elements, and if used as a lithium iron phosphate precursor, it cannot play a role in modifying the doping of lithium iron phosphate. The patent CN102664294A smashes the battery core into fragments, soaks with sodium hydroxide solution and stirs, filters, washes, sieves to separate the current collector from the positive and negative electrode powder, then adjusts the proportion of each element in the powder, sinters to obtain the lithium iron phosphate positive electrode material, ignores the dissolution of the sodium hydroxide solution to the positive electrode current collector aluminum foil, has a certain amount of aluminum dissolved in the solution during the soakage process, with Al3+And the preparation of the lithium iron phosphate anode is influenced. The patent CN111135939A separates the electrode material by mechanical crushing and vibration screening, and the electrode material is passed through hydrometallurgyThe lithium resource is reasonably recovered, other valuable elements are not recovered, and the mechanical separation process of the current collector and the powder material in the patent is complex and has higher cost. According to the content, the defects of complicated steps, high cost, low practical application value and the like of the conventional recovery process can be found, and the development of a simple and efficient process for recycling the lithium iron phosphate retired battery is imperative.
Disclosure of Invention
The invention provides a method for recycling and preparing lithium iron phosphate from a lithium ion battery, and aims to provide a simple and efficient lithium battery recycling process, wherein lithium iron phosphate is recycled and prepared from a lithium iron phosphate retired battery, a lithium iron phosphate precursor is conveniently and quickly obtained, and a lithium iron phosphate anode material with excellent performance is prepared again.
In order to achieve the purpose, the invention provides a method for recovering and preparing lithium iron phosphate from a lithium ion battery, which comprises the following steps:
s1: discharging the retired lithium iron phosphate battery, disassembling to obtain a battery anode, crushing, screening, airflow sorting and collecting to obtain powder;
s2: carrying out oxidation leaching on the powder obtained in the step S1 under an acidic condition to obtain filtrate and filter residue;
s3: adjusting the pH of the filtrate obtained in the step S2 to 1-3 by using an alkali solution, and adding phosphoric acid into the filtrate to obtain an iron phosphate precipitate containing a small amount of aluminum elements, wherein the iron phosphate precipitate is used as a precursor for preparing a lithium iron phosphate material;
s4: mixing the precursor obtained in the step S3 with a lithium source to obtain a mixture;
s5: and grinding the mixture obtained in the step S4 and a carbon source uniformly, and sintering in an inert atmosphere to obtain the aluminum-doped lithium iron phosphate cathode material.
Preferably, in S1, a sieve with the diameter of the mesh of 0.5-2 mm is used for screening, the airflow separation equipment is a cyclone separator, and powder which does not meet the requirement returns to the crusher for continuous crushing.
Preferably, in the S2, the acid used for leaching is one or more of hydrochloric acid, sulfuric acid, acetic acid, oxalic acid, methanesulfonic acid and benzenesulfonic acid, and the concentration of the acid is 0.1-5 mol/L.
Preferably, in the step S2, hydrogen peroxide is added for oxidation leaching, and the concentration of the hydrogen peroxide is 5-20%.
Preferably, in S2, the filtrate contains metal ions, phosphate ions, and acid ions, and the metal ions are Fe3+And Al3+And the filter residue is a mixture of a binder and positive conductive carbon.
Preferably, in S3, the alkali solution is one or more of NaOH solution, KOH solution and ammonia water, the alkali concentration in the alkali solution is 0.1-5 mol/L, the phosphoric acid concentration is 1-3 mol/L,
preferably, in S3, the molar ratio of aluminum element to iron element in the iron phosphate precipitate is 0.1-10: 100.
Preferably, in S4, the lithium source is one or more of lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium phosphate, and lithium dihydrogen phosphate.
Preferably, in S4, the mass ratio of lithium in the lithium source to iron in the precursor is 1.05-1.15: 1.
Preferably, in the step S5, the carbon source is one or more of graphite, conductive carbon, acetylene black, conductive carbon black, carbon fibers, carbon nanotubes, carbon nanospheres, glucose, cellulose, sucrose, fructose and phenolic resin, and the mass ratio of the carbon source to the mixture is 0.005: 1-0.2: 1.
Preferably, in the step S5, the sintering temperature is 600-850 ℃, the sintering time is 8-12 hours, the inert gas is argon gas or a hydrogen-argon mixed gas, and hydrogen in the hydrogen-argon mixed gas accounts for 1% -10% of the total volume of the hydrogen-argon mixed gas.
The scheme of the invention has the following beneficial effects:
1. the recovery process is simple and convenient, the battery anode is directly crushed and sieved, air flow separation is carried out by utilizing the difference of the physical and chemical properties of the anode current collector aluminum foil and the anode material, chemical reagents are not required to be added for separating the pole piece from the anode material, and the energy consumption and the cost are lower.
2. A small amount of aluminum elements contained in the powder obtained by air flow separation do not need to be subjected to ion impurity removal, a part of aluminum enters into the iron phosphate precursor together when ferric ions are precipitated by using phosphoric acid, and the aluminum-doped lithium iron phosphate anode material can be directly obtained in the subsequent material preparation process.
3. The lithium iron phosphate anode material prepared by recycling the retired lithium iron phosphate battery has the advantages of short process, low cost and strong operability.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
Example 1
A method for recovering and preparing lithium iron phosphate from a lithium ion battery comprises the following steps:
(1) disassembling the retired lithium iron phosphate battery after discharging to obtain a battery anode, crushing and screening the battery anode by using a crusher, sieving by using a 1mm sieve, performing air flow separation on the screened materials, and collecting to obtain lighter powder;
(2) carrying out oxidation leaching on the powder obtained in the step (1) by using 1mol/L hydrochloric acid and 10% hydrogen peroxide to obtain filtrate and filter residue containing metal ions, phosphate ions and acid radical ions, wherein the metal ions in the filtrate are Fe3+、Al3+The anion is PO4 3-And Cl-The filter residue is a mixture of a binder and positive conductive carbon;
(3) adjusting the pH value of the filtrate obtained in the step (2) to 2 by using 0.5mol/L NaOH solution, and adding 3mol/L phosphoric acid into the filtrate to obtain iron phosphate precipitate containing a small amount of aluminum element, wherein the molar ratio of the aluminum element to the iron element in the precipitate is 8: 100;
(4) mixing the precursor obtained in the step (3) with lithium carbonate, and controlling the ratio of lithium to iron to be 1.15: 1;
(5) and (3) mixing the mixture obtained in the step (4) with glucose according to the mass ratio of 1: grinding and mixing 0.2, and reacting in hydrogen-argon mixed gas containing 5% hydrogen at 700 ℃ for 10h to obtain the aluminum-doped lithium iron phosphate cathode material.
Through tests, the aluminum-doped lithium iron phosphate anode material obtained by sintering is charged and discharged at 0.1C within 2-3.75V, and the first charging specific capacity is 159mAh g-1The first discharge specific capacity is 154mAh g-1The first charge-discharge efficiency is 96.8 percent, and the reversible capacity is still 122mAh g after 1C circulation for 100 circles-1。
Example 2
A method for recovering and preparing lithium iron phosphate from a lithium ion battery comprises the following steps:
(1) disassembling the retired lithium iron phosphate battery after discharging to obtain a battery anode, crushing and screening the battery anode by using a crusher, screening by using a 1.5mm screen, performing air flow separation on the screened materials, and collecting to obtain lighter powder;
(2) carrying out oxidation leaching on the powder obtained in the step (1) by using 2mol/L sulfuric acid and 15% hydrogen peroxide to obtain filtrate and filter residue containing metal ions, phosphate ions and acid radical ions, wherein the metal ions in the filtrate are Fe3+、Al3+The anion is PO4 3-And SO4 2-The filter residue is a mixture of a binder and positive conductive carbon;
(3) adjusting the pH value of the filtrate obtained in the step (2) to 1.5 by using 1mol/L ammonia water solution, and adding 2mol/L phosphoric acid into the filtrate to obtain iron phosphate precipitate containing a small amount of aluminum element, wherein the molar ratio of the aluminum element to the iron element in the precipitate is 10: 100;
(4) mixing the precursor obtained in the step (3) with lithium phosphate, and controlling the ratio of lithium to iron to be 1.1: 1;
(5) and (3) mixing the mixture obtained in the step (4) with acetylene black according to the mass ratio of 1: grinding and mixing 0.02 percent, and reacting for 12 hours at 600 ℃ in a hydrogen-argon mixed gas containing 10 percent of hydrogen to obtain the aluminum-doped lithium iron phosphate cathode material.
Through tests, the aluminum-doped lithium iron phosphate anode material obtained by sintering is charged and discharged at 0.1C within 2-3.75V, and the first charging specific capacity is 158mAh g-1The first discharge specific capacity is 152mAh g-1The first charge-discharge efficiency is 96.2 percent, and after 100 cycles of 1C circulation, the reversible capacity is still 119mAh g-1。
Example 3
A method for recovering and preparing lithium iron phosphate from a lithium ion battery comprises the following steps:
(1) disassembling the retired lithium iron phosphate battery after discharging to obtain a battery anode, crushing and screening the battery anode by using a crusher, screening by using a screen with the thickness of 0.5mm, then carrying out air flow separation on the screened materials, and collecting to obtain lighter powder;
(2) carrying out oxidation leaching on the powder obtained in the step (1) by using 5mol/L hydrochloric acid and 5% hydrogen peroxide to obtain filtrate and filter residue containing metal ions, phosphate ions and acid radical ions, wherein the metal ions in the filtrate are Fe3+、Al3+The anion is PO4 3-And Cl-The filter residue is a mixture of a binder and positive conductive carbon;
(3) adjusting the pH value of the filtrate obtained in the step (2) to 2.5 by using 0.5mol/L KOH solution, and adding 5mol/L phosphoric acid into the filtrate to obtain iron phosphate precipitate containing a small amount of aluminum element, wherein the molar ratio of the aluminum element to the iron element in the precipitate is 0.5: 100;
(4) mixing the precursor obtained in the step (3) with lithium acetate, and controlling the ratio of lithium to iron to be 1.05: 1;
(5) and (3) mixing the mixture obtained in the step (4) with the carbon nano tube according to the mass ratio of 1: 0.005 grinding and mixing. The reaction is carried out for 15h at 800 ℃ under the argon atmosphere. And obtaining the aluminum-doped lithium iron phosphate cathode material.
Through tests, the aluminum-doped lithium iron phosphate anode material obtained by sintering is charged and discharged at 0.1C within 2-3.75V, and the first charging specific capacity is 155mAh g-1The first discharge specific capacity is 151mAh g-1The first charge-discharge efficiency is 97.4 percent, and the reversible capacity is still 127mAh g after 1C circulation for 100 circles-1。
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for recovering and preparing lithium iron phosphate from a lithium ion battery is characterized by comprising the following steps:
s1: the method comprises the following steps of (1) discharging the retired lithium iron phosphate battery, disassembling to obtain a battery anode, crushing, screening and airflow sorting the obtained battery anode, and collecting to obtain powder;
s2: carrying out oxidation leaching on the powder obtained in the step S1 under an acidic condition to obtain filtrate and filter residue;
s3: adjusting the pH of the filtrate obtained in the step S2 to 1-3 by using an alkali solution, and adding phosphoric acid into the filtrate to obtain an iron phosphate precipitate containing an aluminum element, wherein the iron phosphate precipitate is used as a precursor for preparing a lithium iron phosphate material;
s4: mixing the precursor obtained in the step S3 with a lithium source to obtain a mixture;
s5: and grinding the mixture obtained in the step S4 and a carbon source uniformly, and sintering in an inert atmosphere to obtain the aluminum-doped lithium iron phosphate cathode material.
2. The method for recycling and preparing lithium iron phosphate from a lithium ion battery according to claim 1, wherein in the step S1, a screen with the mesh diameter of 0.5-2 mm is used for screening, and the airflow separation equipment is a cyclone separator.
3. The method for recovering and preparing lithium iron phosphate from a lithium ion battery according to claim 1, wherein in the step S2, the acid used for leaching is one or more of hydrochloric acid, sulfuric acid, acetic acid, oxalic acid, methanesulfonic acid and benzenesulfonic acid, and the concentration of the acid is 0.1-5 mol/L.
4. The method for recovering and preparing lithium iron phosphate from the lithium ion battery according to claim 1, wherein hydrogen peroxide is added to S2 for oxidation leaching, and the concentration of the hydrogen peroxide is 5-20%.
5. The method for recovering and preparing lithium iron phosphate from a lithium ion battery according to claim 1, wherein in the step S3, the alkali solution is one or more of a NaOH solution, a KOH solution and ammonia water, the alkali concentration in the alkali solution is 0.1-5 mol/L, and the phosphoric acid concentration is 1-3 mol/L.
6. The method for recovering and preparing lithium iron phosphate from a lithium ion battery according to claim 1, wherein in the step S3, the molar ratio of aluminum element to iron element in the ferric phosphate precipitate is 0.1-10: 100.
7. The method of claim 1, wherein in S4, the lithium source is one or more of lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate, lithium phosphate, and lithium dihydrogen phosphate.
8. The method for recovering and preparing lithium iron phosphate from a lithium ion battery according to claim 1, wherein in the step S4, the mass ratio of lithium in the lithium source to iron in the precursor is 1.05-1.15: 1.
9. The method for recovering and preparing lithium iron phosphate from the lithium ion battery according to claim 1, wherein in S5, the carbon source is one or more of graphite, conductive carbon, acetylene black, conductive carbon black, carbon fibers, carbon nanotubes, carbon nanospheres, glucose, cellulose, sucrose, fructose and phenolic resin, and the mass ratio of the carbon source to the mixture is 0.005: 1-0.2: 1.
10. The method for recovering and preparing lithium iron phosphate from a lithium ion battery according to claim 1, wherein in the step S5, the sintering temperature is 600-850 ℃, the sintering time is 8-12 h, the inert gas is argon or a hydrogen-argon mixture, and hydrogen in the hydrogen-argon mixture accounts for 1-10% of the total volume of the hydrogen-argon mixture.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104831A (en) * | 2021-04-07 | 2021-07-13 | 贵州唯特高新能源科技有限公司 | Lithium iron phosphate anode material, preparation method thereof, battery anode and lithium ion battery |
| CN114335786A (en) * | 2022-01-06 | 2022-04-12 | 巩义市瑞赛克机械设备有限公司 | Method and device for regenerating lithium iron phosphate anode material |
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| CN104332628A (en) * | 2014-09-04 | 2015-02-04 | 北汽福田汽车股份有限公司 | Preparation method and lithium ion battery of lithium ion battery positive material |
| CN108996484A (en) * | 2018-07-24 | 2018-12-14 | 深圳市德方纳米科技股份有限公司 | The preparation method of the recoverying and utilizing method of waste lithium iron phosphate battery, iron manganese phosphate for lithium and lithium iron phosphate positive material |
| CN109179358A (en) * | 2018-11-08 | 2019-01-11 | 广东省稀有金属研究所 | A method of preparing battery-grade iron phosphate from waste lithium iron phosphate battery |
| CN110422831A (en) * | 2019-08-02 | 2019-11-08 | 湖北昊瑞新能源有限公司 | A method of recycling ferric phosphate from ferric phosphate lithium cell |
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2020
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104332628A (en) * | 2014-09-04 | 2015-02-04 | 北汽福田汽车股份有限公司 | Preparation method and lithium ion battery of lithium ion battery positive material |
| CN108996484A (en) * | 2018-07-24 | 2018-12-14 | 深圳市德方纳米科技股份有限公司 | The preparation method of the recoverying and utilizing method of waste lithium iron phosphate battery, iron manganese phosphate for lithium and lithium iron phosphate positive material |
| CN109179358A (en) * | 2018-11-08 | 2019-01-11 | 广东省稀有金属研究所 | A method of preparing battery-grade iron phosphate from waste lithium iron phosphate battery |
| CN110422831A (en) * | 2019-08-02 | 2019-11-08 | 湖北昊瑞新能源有限公司 | A method of recycling ferric phosphate from ferric phosphate lithium cell |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104831A (en) * | 2021-04-07 | 2021-07-13 | 贵州唯特高新能源科技有限公司 | Lithium iron phosphate anode material, preparation method thereof, battery anode and lithium ion battery |
| CN114335786A (en) * | 2022-01-06 | 2022-04-12 | 巩义市瑞赛克机械设备有限公司 | Method and device for regenerating lithium iron phosphate anode material |
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Application publication date: 20201124 |