CN110331288B - Method for selectively extracting lithium from waste lithium iron phosphate material - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- C22B7/006—Wet processes
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- H—ELECTRICITY
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- 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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- Y02P10/20—Recycling
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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
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Abstract
The invention discloses a method for selectively extracting lithium from a waste lithium iron phosphate material, which comprises the following steps: immersing the waste lithium iron phosphate material into a sodium hydroxide solution, carrying out alkaline leaching to remove aluminum, filtering, drying the material after aluminum removal obtained by filtering to obtain lithium iron phosphate powder, and recovering the filtered sodium aluminate filtrate; putting the lithium iron phosphate powder into a heating furnace, introducing selective lithium extraction gas, and roasting to obtain a compound of iron phosphate and lithium; adding a compound of ferric phosphate and lithium into a ball mill, carrying out wet ball milling, and filtering to respectively obtain a ferric phosphate solid and a lithium-containing solution; adjusting the pH value of the lithium-containing solution to 9.0-11.0, and removing impurities to obtain a pure lithium solution; and adding a sodium carbonate solution into the pure lithium solution for reaction, filtering, and washing and drying the solid obtained by filtering to obtain the lithium carbonate. The method provided by the invention is used for recovering lithium in the waste lithium iron phosphate material, and the recovery rate of lithium is up to more than 95%.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of lithium ion battery electrode materials, and particularly relates to a method for selectively extracting lithium from a waste lithium iron phosphate material.
Background
Lithium iron phosphate is a lithium ion battery material with the largest usage amount at present, and is regarded as the development direction of future lithium batteries by people in many industries. Since the 21 st century, with the blowout type development of the lithium battery new energy market, the treatment problem of the waste lithium iron phosphate batteries is increasingly prominent.
The LiFePO reported most at present4The waste material treatment process is mainly referred to from the waste material recovery processes of lithium cobaltate, lithium nickel cobalt manganese oxide and the like. In patent CN104953200A (a method for recovering battery-grade iron phosphate from lithium iron phosphate batteries and preparing lithium iron phosphate cathode materials by using waste lithium iron phosphate batteries), a heat treatment-acid leaching-iron phosphate precipitation-lithium carbonate precipitation-lithium iron phosphate synthesis process is adopted for lithium iron phosphate waste, and the lithium iron phosphate waste is prepared into a lithium iron phosphate material again. The invention patent CN106450547A (a method for recovering iron phosphate and lithium carbonate from lithium iron phosphate waste) adopts the processes of oxidizing roasting, phosphoric acid leaching, liquid-solid separation and lithium carbonate precipitation, realizes the high-efficiency separation of lithium and ferrophosphorus, and has good effect but complex process.
Therefore, a method for selectively extracting lithium from waste lithium iron phosphate materials, which has the advantages of simple process, low production cost, low energy consumption and obvious economic benefit and is beneficial to promoting the recovery and development of lithium iron phosphate batteries, is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a method for selectively extracting lithium from a waste lithium iron phosphate material, which has the advantages of simple process, low production cost, low energy consumption and obvious economic benefit and is beneficial to promoting the recovery and development of lithium iron phosphate batteries.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for selectively extracting lithium from a waste lithium iron phosphate material comprises the following steps:
(1) immersing the waste lithium iron phosphate material into a sodium hydroxide solution, carrying out alkaline leaching to remove aluminum, filtering, drying the material after aluminum removal obtained by filtering to obtain lithium iron phosphate powder, and recovering the filtered sodium aluminate filtrate;
(2) putting the lithium iron phosphate powder into a heating furnace, introducing selective lithium extraction gas, and roasting to obtain a compound of iron phosphate and lithium;
(3) adding a compound of ferric phosphate and lithium into a ball mill, carrying out wet ball milling, and filtering to respectively obtain a ferric phosphate solid and a lithium-containing solution;
(4) adjusting the pH value of the lithium-containing solution to 9.0-11.0, and removing impurities to obtain a pure lithium solution;
(5) and adding a sodium carbonate solution into the pure lithium solution for reaction, filtering, and washing and drying the solid obtained by filtering to obtain the lithium carbonate.
Preferably, in the step (1), the waste lithium iron phosphate material is obtained from waste lithium iron phosphate materials generated in the production process of lithium iron phosphate batteries and waste lithium iron phosphate materials obtained by disassembling lithium iron phosphate batteries.
Preferably, in the step (1), the molar weight of the sodium hydroxide is 1.2-1.5 times of the molar weight of aluminum in the waste lithium iron phosphate material.
Preferably, in the step (1), the mass ratio of the sodium hydroxide solution to the waste lithium iron phosphate material is 3-5: 1.
Preferably, in the step (1), the alkali leaching aluminum removal is carried out at 90-95 ℃ for 2-3 h.
Preferably, in the step (2), the roasting is carried out at 200-1000 ℃ for 1-6 h.
Preferably, in the step (2), the selective lithium extraction gas is one or more selected from chlorine gas, sulfur dioxide, sulfur trioxide, chlorine dioxide, chlorine monoxide, chlorine peroxide and oxygen.
Preferably, in the step (3), the time of wet ball milling is 0.5-2 hours, the liquid-solid ratio of the wet ball milling slurry is 2-3:1, and the fineness of the wet ball milling material is more than or equal to 100 meshes.
Preferably, in the step (4), the substance added to adjust the pH of the lithium-containing solution to 9.0 to 11.0 is sodium carbonate.
Preferably, in step (5), the reaction time is 2-3 h.
The reaction mechanism of the decomposition of lithium iron phosphate to the conversion of iron phosphate and lithium compounds is as follows:
2LiFePO4+SO2+O2＝Li2SO4+2FePO4
2LiFePO4+Cl2＝2LiCl+2FePO4
namely, under the condition of high temperature, the acidification and oxidation of lithium iron phosphate are realized to generate soluble lithium salts such as lithium sulfate, lithium chloride and the like and iron phosphate slag, and the selective leaching of lithium is realized after water leaching.
Preferably, SO is selected2+ oxygen/air gas atmosphere.
The beneficial technical effects of the invention are as follows:
the method disclosed by the invention is simple in process, low in cost and low in energy consumption, can realize selective extraction of lithium in the waste lithium iron phosphate material, has the leaching rate of the lithium being more than or equal to 97.75%, the leaching rate of iron being less than 0.2%, the recovery rate of the lithium being more than 95%, has high product value, has considerable economic benefits, and is beneficial to promoting recycling of the lithium iron phosphate battery.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail by examples below. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
Example 1
A method for selectively extracting lithium from a waste lithium iron phosphate material comprises the following steps:
(1) alkaline leaching for removing aluminum
Mixing and stirring 1000g of waste lithium iron phosphate material (the content of lithium iron phosphate is 89.32 percent, and the content of aluminum is 2.34 percent) and 3000ml of sodium hydroxide solution (0.380mol/L), heating to 90 ℃, reacting for 2 hours, carrying out alkaline leaching to remove aluminum, filtering to obtain a material after aluminum removal, and drying the material after aluminum removal to obtain 976.9g of lithium iron phosphate powder;
(2) conversion by calcination
Putting 800g of lithium iron phosphate powder into a heating furnace, introducing mixed gas of sulfur dioxide and oxygen at 700 ℃, roasting for 3h, decomposing the lithium iron phosphate, and converting into 983.8g of a compound of iron phosphate and lithium;
(3) ball milling water immersion
Adding 500g of iron phosphate and lithium compound and 1000ml of water into a ball mill for wet ball milling, and filtering to obtain 1000ml of iron phosphate solid and lithium-containing solution, wherein the lithium content is 16.10g/L, and the iron content is 0.21 g/L; calculating to obtain 97.75% of lithium leaching rate and 0.16% of iron leaching rate;
(4) removing impurities from lithium liquid
Adding sodium carbonate solution into 500ml of the lithium-containing solution obtained in the step (3) to adjust the pH value to 10.5, removing impurities in the solution, and filtering to obtain a pure lithium solution;
(5) preparation of lithium carbonate
And (4) adding 200ml of 30% sodium carbonate solution into 400ml of the lithium solution obtained in the step (4), reacting for 2 hours, filtering, washing and drying to obtain a lithium carbonate product.
Example 2
A method for selectively extracting lithium from a waste lithium iron phosphate material comprises the following steps:
(1) alkaline leaching for removing aluminum
Mixing and stirring 1000g of waste lithium iron phosphate material (the content of lithium iron phosphate is 89.32 percent, and the content of aluminum is 2.34 percent) and 3000ml of sodium hydroxide solution (0.380mol/L), heating to 90 ℃, reacting for 2 hours, carrying out alkaline leaching to remove aluminum, filtering to obtain a material after aluminum removal, and drying the material after aluminum removal to obtain 976.9g of lithium iron phosphate powder;
(2) conversion by calcination
Placing 800g of lithium iron phosphate powder into a heating furnace, introducing chlorine gas at 500 ℃, roasting for 3h in a selective atmosphere, and decomposing the lithium iron phosphate to convert into 929.1g of a compound of iron phosphate and lithium;
(3) ball milling water immersion
Adding 500g of roasted and converted material and 1500ml of water into a ball mill for wet ball milling, and filtering to obtain 1500ml of ferric phosphate solid and lithium-containing solution, wherein the lithium content is 10.85g/L, and the iron content is 0.15; calculated, the leaching rate of lithium was 98.82%, and the leaching rate of iron was 0.17%.
(4) Removing impurities from lithium liquid
Adding sodium carbonate solution into 500ml of the lithium-containing solution obtained in the step (3) to adjust the pH value to 10.2, removing impurities in the solution, and filtering to obtain a pure lithium solution;
(5) preparation of lithium carbonate
And (4) adding 150ml of 30% sodium carbonate solution into 400ml of the lithium solution obtained in the step (4), reacting for 2 hours, filtering, washing and drying to obtain a lithium carbonate product.
Example 3
A method for selectively extracting lithium from a waste lithium iron phosphate material comprises the following steps:
(1) alkaline leaching for removing aluminum
Mixing and stirring 1000g of waste lithium iron phosphate material (the content of lithium iron phosphate is 87.68 percent, and the content of aluminum is 5.30 percent) and 3500ml of sodium hydroxide solution (0.750mol/L), heating to 90 ℃, reacting for 2 hours, filtering to obtain a material after aluminum removal, and drying the material after aluminum removal to obtain 945.6g of lithium iron phosphate powder;
(2) conversion by calcination
Placing 800g of lithium iron phosphate powder into a heating furnace, introducing sulfur trioxide gas at 600 ℃, roasting for 4h, decomposing the lithium iron phosphate, and converting into 992.3g of a compound of iron phosphate and lithium;
(3) ball milling water immersion
Adding 500g of roasted and converted material and 1000ml of water into a ball mill for wet ball milling, and filtering to obtain 1000ml of ferric phosphate solid and lithium-containing solution, wherein the lithium content is 16.4g/L, and the iron content is 0.03 g/L; calculated, the leaching rate of lithium is 99.58 percent, and the leaching rate of iron is 0.02 percent.
(4) Removing impurities from lithium liquid
Adding sodium carbonate solution into 500ml of the lithium-containing solution obtained in the step (3) to adjust the pH value to 10.8, removing impurities in the solution, and filtering to obtain a pure lithium solution;
(5) preparation of lithium carbonate
And (4) adding 200ml of 30% sodium carbonate solution into 400ml of the lithium solution obtained in the step (4), reacting for 2 hours, filtering, washing and drying to obtain a lithium carbonate product.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A method for selectively extracting lithium from a waste lithium iron phosphate material is characterized by comprising the following steps:
(1) immersing the waste lithium iron phosphate material into a sodium hydroxide solution, carrying out alkaline leaching to remove aluminum, filtering, drying the material after aluminum removal obtained by filtering to obtain lithium iron phosphate powder, and recovering the filtered sodium aluminate filtrate;
(2) putting the lithium iron phosphate powder into a heating furnace, introducing selective lithium extraction gas, roasting, and decomposing and converting the lithium iron phosphate to obtain a compound of ferric phosphate and lithium;
(3) adding a compound of ferric phosphate and lithium into a ball mill, carrying out wet ball milling, and filtering to respectively obtain a ferric phosphate solid and a lithium-containing solution;
(4) adjusting the pH value of the lithium-containing solution to 9.0-11.0, and removing impurities to obtain a pure lithium solution;
(5) adding a sodium carbonate solution into a pure lithium solution for reaction, filtering, washing and drying a solid obtained by filtering to obtain lithium carbonate; in the step (1), the addition amount of the sodium hydroxide is 1.2-1.5 times of the molar weight of aluminum in the waste lithium iron phosphate material; in the step (2), the selective lithium extraction gas is selected from one or more of chlorine gas, sulfur dioxide, sulfur trioxide, chlorine dioxide, chlorine monoxide or chlorine peroxide; in the step (3), the time of wet ball milling is 0.5-2 hours, the liquid-solid ratio of the wet ball milling slurry is 2-3:1mL/g, and the fineness of the wet ball milling material is more than or equal to 100 meshes.
2. The method for selectively extracting lithium from the waste lithium iron phosphate material according to claim 1, wherein in the step (1), the mass ratio of the sodium hydroxide solution to the waste lithium iron phosphate material is 3-5: 1.
3. The method for selectively extracting lithium from the waste lithium iron phosphate material as claimed in claim 1, wherein in the step (1), the alkali leaching for removing aluminum is carried out at 90-95 ℃ for 2-3 h.
4. The method for selectively extracting lithium from the waste lithium iron phosphate material as claimed in claim 1, wherein in the step (2), the roasting is carried out at 200-1000 ℃ for 1-6 h.
5. The method for selectively extracting lithium from the waste lithium iron phosphate material as claimed in claim 1, wherein in the step (5), the substance added for adjusting the pH value of the lithium-containing solution to 9.0-11.0 is sodium carbonate.
6. The method for selectively extracting lithium from the waste lithium iron phosphate material as claimed in claim 1, wherein in the step (5), the reaction time is 2-3 h.
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| CN110760682A (en) * | 2019-11-05 | 2020-02-07 | 中国科学院生态环境研究中心 | Process for selectively recovering lithium in waste lithium iron phosphate batteries by virtue of mechanochemical activation method |
| CN111483992A (en) * | 2020-03-20 | 2020-08-04 | 中国科学院生态环境研究中心 | Method for extracting phosphorus from waste lithium iron phosphate powder |
| CN112142077B (en) * | 2020-09-08 | 2021-10-29 | 北京科技大学 | Method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste |
| CN112047319A (en) * | 2020-09-11 | 2020-12-08 | 南昌航空大学 | Method for recovering battery-grade iron phosphate from waste iron phosphate slag |
| CN112410556B (en) * | 2020-09-25 | 2022-10-14 | 湖北金泉新材料有限公司 | Method for recovering waste lithium iron phosphate powder |
| CN112694074B (en) * | 2020-12-28 | 2023-01-13 | 湖南邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| CN113061723B (en) * | 2021-03-04 | 2023-01-20 | 长沙友合金属材料有限公司 | Method for recovering lithium from waste lithium iron phosphate batteries and preparing iron phosphate |
| CN113603119B (en) * | 2021-08-03 | 2022-11-15 | 广东邦普循环科技有限公司 | Method for recovering lithium from waste lithium iron phosphate material |
| CN113774225A (en) * | 2021-09-15 | 2021-12-10 | 湖南天泰天润新能源科技有限公司 | Method for selectively leaching lithium from waste lithium iron phosphate batteries |
| CN115140722B (en) * | 2022-06-10 | 2024-02-09 | 广东邦普循环科技有限公司 | Method for preparing positive electrode material by using waste vanadyl phosphate lithium battery |
| CN115627346A (en) * | 2022-10-28 | 2023-01-20 | 中南大学 | Method for recovering anode material of waste lithium battery |
| CN116553510B (en) * | 2023-05-11 | 2024-05-03 | 上饶溢骏鑫环境科技有限公司 | Recycling and regenerating method of lithium iron phosphate waste powder |
| CN118270748B (en) * | 2024-05-31 | 2024-07-26 | 郴州汇能储能材料工程研究中心有限责任公司 | Method for preparing ferric phosphate based on waste lithium iron phosphate battery |
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| US20150259208A1 (en) * | 2014-03-14 | 2015-09-17 | Valence Technology, Inc. | Method of Making Active Materials for Use in Secondary Electrochemical Cells |
| CN106756049A (en) * | 2016-12-23 | 2017-05-31 | 江西合纵锂业科技有限公司 | A kind of method that iron and lithium are reclaimed in the lithium iron phosphate battery positive material from failure |
| CN106684486A (en) * | 2016-12-28 | 2017-05-17 | 天津先众新能源科技股份有限公司 | Method for extracting lithium from waste lithium iron phosphate |
| CN106848473B (en) * | 2017-04-18 | 2021-10-08 | 中科过程（北京）科技有限公司 | Method for selectively recovering lithium in waste lithium iron phosphate batteries |
| CN106910959B (en) * | 2017-05-04 | 2020-02-21 | 北京科技大学 | Method for selectively recovering lithium from lithium iron phosphate waste |
| CN108298514A (en) * | 2017-12-11 | 2018-07-20 | 中国科学院过程工程研究所 | A kind of method of lithium in high temperature solid-state method selective recovery waste lithium iron phosphate positive electrode |
| CN109179359A (en) * | 2018-11-27 | 2019-01-11 | 成都绿锂环保科技有限公司 | A method of extracting lithium and ferric phosphate from LiFePO4 waste material |
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