CN112142077A - Method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste - Google Patents
Method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste Download PDFInfo
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- CN112142077A CN112142077A CN202010936508.8A CN202010936508A CN112142077A CN 112142077 A CN112142077 A CN 112142077A CN 202010936508 A CN202010936508 A CN 202010936508A CN 112142077 A CN112142077 A CN 112142077A
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- iron phosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
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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
- 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
Abstract
The invention relates to a method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate cathode waste, belonging to the field of recycling treatment and resource utilization of electronic waste. According to the method, air is used as an oxidant to oxidize the lithium iron phosphate into the iron phosphate, so that lithium is extracted and enters a solution, and other impurity elements are rarely leached. Removing impurities from the lithium solution through neutralization and precipitation, and adding saturated sodium carbonate to obtain a lithium carbonate product; mixing the water leaching residue with iron powder and a small amount of phosphoric acid, performing ball milling activation reduction, stirring and dissolving a solid product obtained after activation by using a phosphoric acid solution, and filtering to obtain an iron and phosphorus solution. The method comprises the steps of utilizing the characteristic that the iron phosphate is low in solubility at high temperature, obtaining iron phosphate precipitate by adopting a high-temperature evaporation crystallization method, and obtaining the iron phosphate for the battery after aging, washing and calcining. The method has the advantages of low reagent cost, low acid consumption, high recovery rate of valuable elements, environmental friendliness and the like.
Description
Technical Field
The invention relates to a method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate cathode waste, belonging to the field of recycling treatment and resource utilization of electronic waste.
Background
The lithium ion battery is used as an energy storage device for mutual conversion of chemical energy and electric energy, and is a driving core of a new energy vehicle. The lithium iron phosphate battery has the advantages of good safety, good cycle performance, stable voltage, good rate performance and the like, so that the application of the lithium iron phosphate battery in the fields of power automobiles, energy storage and the like is rapidly developed. This means that a large number of discarded lithium iron phosphate batteries will be produced in the future. Harmful substances such as electrolytes contained in the waste batteries cause environmental pollution, and valuable metals such as lithium and iron contained in the waste batteries cannot be recycled, so that resource waste is caused. Therefore, the recovery of the waste batteries becomes an effective way for relieving the environmental pressure and bringing economic benefits.
The mature and largely applied method for recovering the lithium iron phosphate anode waste is an acid leaching method, namely, inorganic acid is used for leaching Li, Fe and P in the anode material, then the pH is adjusted back by alkali to precipitate Fe in the form of iron phosphate, and then sodium carbonate is added to recover Li in the form of lithium carbonate. The method comprises the steps of treating lithium iron phosphate waste materials by using an acid leaching process in Chinese patent CN107352524A, adjusting the pH value of a leachate to 1.5-2.5 with sodium hydroxide or ammonia water to precipitate iron phosphate, filtering to obtain crude iron phosphate and filtrate, refining the crude iron phosphate to obtain a battery-grade iron phosphate product, adding saturated sodium carbonate into the filtrate, and filtering and washing to obtain lithium carbonate. In the method, the recovery rates of lithium and iron phosphate respectively reach 90% and 95%. The Chinese patent CN106684485A adopts hydrogen peroxide to oxidize acid and leach the lithium iron phosphate anode waste, then adjusts the pH of the leachate to 1.5-4 to precipitate to obtain iron phosphate, and obtains lithium-containing filtrate and the iron phosphate through filtering and washing. However, the above methods all have the disadvantages of high acid and alkali consumption, generation of a large amount of salt-containing wastewater, and entrainment of a certain amount of lithium during iron phosphate precipitation, which results in a decrease in lithium recovery rate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a more economical and environment-friendly method for comprehensively recovering waste lithium iron phosphate. Under the condition of not damaging the structure of the lithium iron phosphate, air is blown into the aqueous solution to directly oxidize the lithium iron phosphate into the iron phosphate, so that lithium is released into the solution, the selective leaching of the lithium is realized, a lithium-containing solution and iron-phosphorus slag are obtained, and the recovery rate of the lithium can reach more than 98 percent. The iron-phosphorus slag adopts iron powder as a reducing agent to carry out mechanical activation reduction, and phosphoric acid is innovatively adopted as a leaching medium, so that the influence caused by the addition of other acid radical ions is avoided.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste is characterized by comprising the following steps:
(1) adding the lithium iron phosphate waste into water, blowing air into the water, and stirring and leaching the mixture to obtain a lithium-containing solution; adjusting the pH value of a lithium solution to 10-11, precipitating and removing impurities, heating the solution to 90-95 ℃, simultaneously adding a saturated sodium carbonate solution to precipitate lithium carbonate, and washing and drying a filtered solid product to obtain a lithium carbonate product;
(2) mixing the slag obtained after water leaching, iron powder and a small amount of phosphoric acid, and putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.55-0.6 times of that of iron in the water leaching slag, and the ball milling time is 0.5-3 hours;
(3) stirring and dissolving out the activated product by using a phosphoric acid solution, controlling the solid-to-liquid ratio to be 250-500 g/L, reacting for 0.5-3 hours at the temperature of 20-50 ℃, and filtering after the reaction is finished to obtain an iron and phosphorus solution; and synchronously adding the solution and hydrogen peroxide into a reaction container containing iron phosphate crystal seeds, controlling the temperature to be 90-95 ℃, stirring, crystallizing and separating out iron phosphate, aging, filtering, and washing and calcining a solid product to obtain the iron phosphate for the battery.
Further, the pH value of the water leaching reaction of the lithium iron phosphate waste material in the step (1) is controlled to be 3.5-5.0, and the adopted pH regulator is one or more of oxalic acid, citric acid, acetic acid and malic acid. The leaching reaction time is 1-5 hours, the reaction temperature is 20-90 ℃, and the solid-to-liquid ratio is 100-500 g/L.
Further, the lithium iron phosphate waste processed by the method comprises anode and cathode mixed powder obtained after disassembling, crushing and screening the invalid lithium iron phosphate battery, anode powder obtained after sorting, waste generated in the production process of battery materials, leftover materials and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method has the advantages that the cheap air is used as an oxidant to selectively recover lithium from the lithium iron phosphate waste, the lithium-containing solution is simply purified to obtain a high-quality lithium product, and the recovery rate of lithium is more than 98%;
(2) part of impurities in the iron-phosphorus slag can be taken away in the lithium leaching process, and a small amount of organic acid brought in can be decomposed at high temperature. In the process of leaching the iron and phosphorus slag, selective phosphoric acid is adopted as a leaching agent without introducing other impurity anions, so that the obtained iron phosphate product has good quality.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which however falls within the scope of protection of the present invention.
Example 1
Adding the lithium iron phosphate anode waste powder into water for size mixing, blowing air and stirring, controlling the solid-liquid ratio of the oxidation leaching condition to be 500g/L, the reaction time to be 1 hour, the reaction temperature to be 25 ℃, and slowly adding oxalic acid to maintain the pH value to be 5.0 in the process. And after the reaction is finished, filtering and separating, adjusting the pH of the filtrate to 11, precipitating and removing impurities, heating the solution to 95 ℃, simultaneously adding a saturated sodium carbonate solution to precipitate lithium carbonate, and washing and drying the filtered solid product to obtain a lithium carbonate product. Adding iron powder into the water leaching slag, adding a small amount of phosphoric acid, putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.55 times of that of iron in the water leaching slag, and the ball milling time is 1 hour; leaching the ball-milled and activated product by using a phosphoric acid solution, controlling the solid-to-liquid ratio of stirring and dissolving to be 250g/L, controlling the temperature to be 25 ℃, and filtering to obtain iron and phosphorus solutions, wherein the leaching rates of iron and phosphorus are analyzed to be 97.1% and 96.6% respectively. And synchronously adding the solution and hydrogen peroxide into a reaction container containing iron phosphate crystal seeds, controlling the temperature to be 95 ℃, stirring, crystallizing and separating out iron phosphate, aging, filtering, washing and calcining a solid product to obtain the iron phosphate for the battery.
Example 2
Adding the lithium iron phosphate anode waste powder into water for size mixing, blowing air and stirring, controlling the solid-liquid ratio of the oxidation leaching condition to be 350g/L, the reaction time to be 3 hours, the reaction temperature to be 50 ℃, and slowly adding acetic acid to maintain the pH value to be about 3.5 in the process. And (3) after the reaction is finished, carrying out solid-liquid separation to obtain a lithium-containing solution and leaching residues, wherein the leaching rate of lithium is 98.9%. And adjusting the pH value of the filtrate to 11, precipitating and removing impurities, then heating the solution to 95 ℃, simultaneously adding a saturated sodium carbonate solution to precipitate lithium carbonate, and washing and drying the filtered solid product to obtain a lithium carbonate product. Adding iron powder into the water leaching slag, adding a small amount of phosphoric acid, putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.575 times of that of iron in the water leaching slag, and the ball milling time is 2 hours; dissolving out the product after ball milling activation by using phosphoric acid, controlling the solid-to-liquid ratio of stirring dissolution to be 370g/L, controlling the temperature to be 30 ℃, and filtering to obtain iron and phosphorus solutions, wherein the leaching rates of iron and phosphorus are analyzed to be respectively 96.8% and 96.1%. And synchronously adding the solution and hydrogen peroxide into a reaction container containing iron phosphate crystal seeds, controlling the temperature to be 95 ℃, stirring, crystallizing and separating out iron phosphate, aging, filtering, washing and calcining a solid product to obtain the iron phosphate for the battery.
Example 3
Adding the lithium iron phosphate anode waste powder into water for size mixing, blowing air and stirring, controlling the solid-liquid ratio of the oxidation leaching condition to be 200g/L, the reaction time to be 5 hours, the reaction temperature to be 90 ℃, and slowly adding citric acid to maintain the pH value to be about 4.0 in the process. And after the reaction is finished, carrying out solid-liquid separation to obtain a lithium-containing solution and leaching residues, wherein the leaching rate of lithium is 99.2%. And adjusting the pH value of the filtrate to 11, precipitating and removing impurities, then heating the solution to 95 ℃, simultaneously adding a saturated sodium carbonate solution to precipitate lithium carbonate, and washing and drying the filtered solid product to obtain a lithium carbonate product. Adding iron powder into the water leaching slag, adding a small amount of phosphoric acid, putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.6 times of that of iron in the water leaching slag, and the ball milling time is 3 hours; dissolving out the product after ball milling activation by using phosphoric acid, controlling the solid-to-liquid ratio of stirring dissolution to be 500g/L, controlling the temperature to be 50 ℃, and filtering to obtain iron and phosphorus solutions, wherein the leaching rates of iron and phosphorus are analyzed to be respectively 96.2% and 95.3%. And synchronously adding the solution and hydrogen peroxide into a reaction container containing iron phosphate crystal seeds, controlling the temperature to be 95 ℃, stirring, crystallizing and separating out iron phosphate, aging, filtering, washing and calcining a solid product to obtain the iron phosphate for the battery.
Claims (3)
1. A method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste is characterized by comprising the following steps:
(1) adding the lithium iron phosphate waste into water, blowing air into the water, and stirring and leaching the mixture to obtain a lithium-containing solution; adjusting the pH value of a lithium solution to 10-11, precipitating and removing impurities, heating the solution to 90-95 ℃, simultaneously adding a saturated sodium carbonate solution to precipitate lithium carbonate, and washing and drying a filtered solid product to obtain a lithium carbonate product;
(2) mixing the slag obtained after water leaching, iron powder and a small amount of phosphoric acid, and putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.55-0.6 times of that of iron in the water leaching slag, and the ball milling time is 0.5-3 hours;
(3) stirring and dissolving out the activated product by using a phosphoric acid solution, controlling the solid-to-liquid ratio to be 250-500 g/L, reacting for 0.5-3 hours at the temperature of 20-50 ℃, and filtering after the reaction is finished to obtain an iron and phosphorus solution; and synchronously adding the solution and hydrogen peroxide into a reaction container containing iron phosphate crystal seeds, controlling the temperature to be 90-95 ℃, stirring, crystallizing and separating out iron phosphate, aging, filtering, and washing and calcining a solid product to obtain the iron phosphate for the battery.
2. The method for recycling lithium iron phosphate positive electrode waste to prepare battery-grade lithium carbonate and iron phosphate according to claim 1, wherein the pH of the water leaching reaction of the lithium iron phosphate waste in the step (1) is controlled to be 3.5-5.0, and the pH regulator is one or more of oxalic acid, citric acid, acetic acid and malic acid. The leaching reaction time is 1-5 hours, the reaction temperature is 20-90 ℃, and the solid-to-liquid ratio is 100-500 g/L.
3. The method for recycling lithium iron phosphate positive electrode waste materials to prepare battery-grade lithium carbonate and iron phosphate according to claim 1, wherein the lithium iron phosphate waste materials comprise anode and cathode mixed powder obtained after disassembling, crushing and screening of failed lithium iron phosphate batteries, anode powder obtained after sorting, waste materials and leftover materials generated in the production process of battery materials.
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Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624161A (en) * | 2020-12-31 | 2021-04-09 | 江西南氏锂电新材料有限公司 | Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite |
| CN113184822A (en) * | 2021-05-12 | 2021-07-30 | 福建富仕新材料有限责任公司 | Method for synthesizing battery-grade iron phosphate by using ilmenite |
| CN113285135A (en) * | 2021-05-07 | 2021-08-20 | 宁夏百川新材料有限公司 | Method for recycling multiple components of waste lithium iron phosphate battery |
| CN113279048A (en) * | 2021-05-10 | 2021-08-20 | 北京科技大学 | Method for preparing high-purity iron phosphate from iron-containing slag |
| CN113415793A (en) * | 2021-05-10 | 2021-09-21 | 北京科技大学 | Method for preparing high-purity iron phosphate from lithium iron phosphate battery waste |
| CN113501510A (en) * | 2021-07-13 | 2021-10-15 | 郑州中科新兴产业技术研究院 | Method for recycling and regenerating anode material of waste lithium iron phosphate battery |
| CN113753873A (en) * | 2021-10-19 | 2021-12-07 | 湖北虹润高科新材料有限公司 | Method for preparing low-aluminum impurity petaloid iron phosphate from waste iron phosphorus slag |
| CN113800488A (en) * | 2021-10-13 | 2021-12-17 | 中南大学 | Resource recovery method of lithium iron phosphate waste |
| CN113880064A (en) * | 2021-11-09 | 2022-01-04 | 株洲冶炼集团股份有限公司 | Method for treating high-impurity lithium iron phosphate waste powder by using low-consumption phosphoric acid |
| 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 |
| CN114421044A (en) * | 2022-01-29 | 2022-04-29 | 湖南裕能新能源电池材料股份有限公司 | Purification treatment method and system for phosphorus-iron slag mixture containing Al and Cu impurities |
| CN114655969A (en) * | 2022-03-28 | 2022-06-24 | 北京科技大学 | Method for preparing lithium carbonate and iron phosphate by recycling high-impurity lithium iron phosphate positive electrode waste |
| CN115043383A (en) * | 2022-08-16 | 2022-09-13 | 矿冶科技集团有限公司 | High-tap-density battery-grade iron phosphate and preparation method thereof |
| CN115057425A (en) * | 2022-08-18 | 2022-09-16 | 矿冶科技集团有限公司 | Method for preparing iron phosphate from waste lithium iron phosphate battery |
| CN115072905A (en) * | 2022-07-14 | 2022-09-20 | 国环电池科技(苏州)有限公司 | Treatment method of battery wastewater and method for recycling high-purity iron phosphate from battery wastewater |
| CN115367721A (en) * | 2021-05-19 | 2022-11-22 | 中国科学院过程工程研究所 | Method for preparing iron phosphate from iron-containing waste acid liquor |
| CN115385314A (en) * | 2022-09-29 | 2022-11-25 | 南昌航空大学 | Method for recovering iron and phosphorus elements in ferrophosphorus slag |
| CN115583640A (en) * | 2022-10-08 | 2023-01-10 | 中南大学 | Method for recycling waste lithium iron phosphate black powder with multiple impurities |
| CN115806280A (en) * | 2022-12-12 | 2023-03-17 | 中南大学 | Method for preparing iron phosphate by taking phosphorus iron powder as byproduct of phosphorus chemical industry as raw material |
| CN116062723A (en) * | 2023-02-06 | 2023-05-05 | 广东邦普循环科技有限公司 | Method for preparing battery-grade ferric phosphate by utilizing nickel-iron alloy |
| CN116177512A (en) * | 2023-04-23 | 2023-05-30 | 赣州市力道新能源有限公司 | Method for preparing iron phosphate material from scrapped lithium battery iron phosphate slag |
| WO2023169022A1 (en) * | 2022-03-07 | 2023-09-14 | 华中科技大学 | Method for processing and recycling ultrathin lithium foil, and product |
| CN116864851A (en) * | 2023-09-05 | 2023-10-10 | 赣州市力道新能源有限公司 | Process for deeply removing phosphorus from retired battery recovery feed liquid |
| WO2024021237A1 (en) * | 2022-07-25 | 2024-02-01 | 广东邦普循环科技有限公司 | Recovery method for lithium iron phosphate |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012072619A1 (en) * | 2010-11-29 | 2012-06-07 | Umicore | Process for the recovery of lithium and iron from lfp batteries |
| KR20160069769A (en) * | 2014-12-09 | 2016-06-17 | 한국교통대학교산학협력단 | FABRICATION METHOD OF LiFePO4, ACTIVE MATERIAL FABRICATED BY THE METHOD, MANUFACTURING METHOD OF LITHIUM ION SECONDARY BATTERY AND LITHIUM ION SECONDARY BATTERY HAVING THE ACTIVE MATERIAL |
| CN106450547A (en) * | 2016-10-19 | 2017-02-22 | 荆门市格林美新材料有限公司 | Method for recycling iron phosphate and lithium carbonate from lithium iron phosphate waste |
| CN106910959A (en) * | 2017-05-04 | 2017-06-30 | 北京科技大学 | A kind of method of selective recovery lithium in waste material from LiFePO4 |
| CN106915734A (en) * | 2017-03-03 | 2017-07-04 | 沧州凯盛达新能源科技有限公司 | The preparation method of ferric lithium phosphate precursor |
| CN110331288A (en) * | 2019-06-28 | 2019-10-15 | 湖南邦普循环科技有限公司 | A kind of method that waste lithium iron phosphate material selectivity mentions lithium |
| CN111187913A (en) * | 2020-02-20 | 2020-05-22 | 广东省稀有金属研究所 | Method for selectively recovering lithium and copper in waste lithium iron phosphate batteries |
| CN111370800A (en) * | 2020-03-03 | 2020-07-03 | 湖南雅城新材料有限公司 | Method for recovering waste lithium iron phosphate anode material |
-
2020
- 2020-09-08 CN CN202010936508.8A patent/CN112142077B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012072619A1 (en) * | 2010-11-29 | 2012-06-07 | Umicore | Process for the recovery of lithium and iron from lfp batteries |
| KR20160069769A (en) * | 2014-12-09 | 2016-06-17 | 한국교통대학교산학협력단 | FABRICATION METHOD OF LiFePO4, ACTIVE MATERIAL FABRICATED BY THE METHOD, MANUFACTURING METHOD OF LITHIUM ION SECONDARY BATTERY AND LITHIUM ION SECONDARY BATTERY HAVING THE ACTIVE MATERIAL |
| CN106450547A (en) * | 2016-10-19 | 2017-02-22 | 荆门市格林美新材料有限公司 | Method for recycling iron phosphate and lithium carbonate from lithium iron phosphate waste |
| CN106915734A (en) * | 2017-03-03 | 2017-07-04 | 沧州凯盛达新能源科技有限公司 | The preparation method of ferric lithium phosphate precursor |
| CN106910959A (en) * | 2017-05-04 | 2017-06-30 | 北京科技大学 | A kind of method of selective recovery lithium in waste material from LiFePO4 |
| CN110331288A (en) * | 2019-06-28 | 2019-10-15 | 湖南邦普循环科技有限公司 | A kind of method that waste lithium iron phosphate material selectivity mentions lithium |
| CN111187913A (en) * | 2020-02-20 | 2020-05-22 | 广东省稀有金属研究所 | Method for selectively recovering lithium and copper in waste lithium iron phosphate batteries |
| CN111370800A (en) * | 2020-03-03 | 2020-07-03 | 湖南雅城新材料有限公司 | Method for recovering waste lithium iron phosphate anode material |
Non-Patent Citations (3)
| Title |
|---|
| WEI WANG ET AL.: "An overview of recycling and treatment of spent LiFePO4 batteries in China", 《RESOURCES, CONSERVATION & RECYCLING》 * |
| YONGXIA YANG ET AL.: "A Closed-Loop Process for Selective Metal Recovery from Spent Lithium Iron Phosphate Batteries through Mechanochemical Activation", 《ACS SUSTAINABLE CHEM. EN》 * |
| 陈永珍等: "废旧磷酸铁锂电池回收技术研究进展", 《储能科学与技术》 * |
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| CN112624161A (en) * | 2020-12-31 | 2021-04-09 | 江西南氏锂电新材料有限公司 | Method for preparing lithium carbonate by extracting lithium from mechanically activated lepidolite |
| CN113285135A (en) * | 2021-05-07 | 2021-08-20 | 宁夏百川新材料有限公司 | Method for recycling multiple components of waste lithium iron phosphate battery |
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