CN112093785A - Method for efficiently recycling lithium in lithium iron phosphate cathode waste and preparing iron phosphate for battery - Google Patents
Method for efficiently recycling lithium in lithium iron phosphate cathode waste and preparing iron phosphate for battery Download PDFInfo
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- CN112093785A CN112093785A CN202010937358.2A CN202010937358A CN112093785A CN 112093785 A CN112093785 A CN 112093785A CN 202010937358 A CN202010937358 A CN 202010937358A CN 112093785 A CN112093785 A CN 112093785A
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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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- 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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Abstract
The invention relates to a method for efficiently recycling lithium as a lithium iron phosphate cathode waste material and preparing battery-grade iron phosphate, belonging to the field of resource treatment of electronic wastes. According to the method, the lithium iron phosphate anode waste is directly oxidized by using cheap air, so that lithium is removed from the waste and enters a solution, and the selective extraction of the lithium is realized. Mixing the water leaching residue with iron powder and a small amount of sulfuric acid, performing ball milling activation reduction, and stirring and dissolving out a solid product obtained after activation by using a sulfuric acid solution. And reacting the obtained iron and phosphorus solution with hydrogen peroxide and sodium hydroxide solution, and aging, washing and calcining to obtain the iron phosphate for the battery. The method has the advantages of cheap reagent, good product quality, high recovery rate of valuable elements and the like, can realize medium internal circulation in the process, has no discharged waste liquid, and has low treatment cost of three wastes.
Description
Technical Field
The invention relates to a method for efficiently recycling lithium as a lithium iron phosphate cathode waste material and preparing iron phosphate for batteries, belonging to the field of resource treatment of electronic wastes.
Background
In recent years, new energy industry in China has been rapidly developed. The lithium iron phosphate battery occupies an important position in the aspects of lithium ion power batteries, energy storage power stations and the like by virtue of the characteristics of good electrochemical performance, high safety, long service life and the like. With the development of lithium ion batteries, the number of waste lithium iron phosphate batteries is increasing, and the report of 2019 in 2 months of Ministry of industry and communications indicates that the scrappage of the lithium ion power batteries in 2020 is predicted to reach 25 ten thousand tons. Therefore, if the waste batteries are not recycled, the waste of resources and the pollution of the environment are caused. Therefore, the development of a green and efficient treatment method of the waste lithium iron phosphate battery is of great significance.
The existing recovery method of the lithium iron phosphate anode waste mainly comprises direct repair, wet leaching and a selective lithium extraction method. A lithium source is added into the lithium iron phosphate anode waste material, and the anode material can be directly repaired and regenerated by methods such as solid phase repair and hydrothermal repair. But the direct repair method is only applicable to the anode waste material with low impurity content in the same batch. The wet leaching method generally uses acid to leach all metal ions of the lithium iron phosphate waste, and recovers and obtains the iron phosphate and the lithium carbonate by a fractional precipitation method. In chinese patent CN108899601A, lithium, iron, and phosphorus in the lithium iron phosphate positive electrode material are all leached by sulfuric acid, an oxidant is added to form an iron phosphate precipitate, and sodium carbonate is added to the filtered filtrate to obtain lithium carbonate. The wet leaching method has high acid consumption, can generate a large amount of salt-containing wastewater, and can not economically recover lithium ions in the solution after iron phosphate precipitation. By selectively extracting lithium from the lithium iron phosphate waste and retaining other elements in the leaching slag, the defects of the traditional wet method can be effectively overcome. In the chinese patent CN106910959A, one or a mixture of several of sodium persulfate, ozone, hypochlorite, oxygen, and hydrogen peroxide is used to directly oxidize the slurry of the lithium iron phosphate cathode waste, and the pH of the reaction is controlled under an acidic condition to realize efficient recovery of lithium. In the existing selective lithium extraction process of the lithium iron phosphate anode waste, the price of the used oxidant is generally higher, so that the economic benefit of recovery is reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the method provides a method for efficiently recycling lithium as the lithium iron phosphate cathode waste material and preparing iron phosphate for batteries. And (3) using cheap air as an oxidant to selectively remove lithium from the lithium iron phosphate waste material into the solution, wherein the obtained lithium solution has low impurity content, and the battery-grade lithium carbonate can be obtained through simple purification. The iron-phosphorus slag after water leaching achieves the purpose, and the invention adopts the specific technical scheme that:
a method for efficiently recycling lithium as a lithium iron phosphate positive waste material and preparing battery-grade iron phosphate is characterized by comprising the following steps of:
(1) adding the lithium iron phosphate waste into water, blowing air and stirring, reacting for a certain time, and then carrying out solid-liquid separation, wherein the filtrate is a lithium-containing solution and can be used for preparing a lithium product;
(2) mixing the water leaching slag obtained in the step (1), iron powder and a small amount of sulfuric acid, and putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.55-1 time of that of iron in the water leaching slag, and the ball milling time is 0.5-2 hours;
(3) stirring and dissolving the solid product obtained after the activation in the step (2) by using a sulfuric acid solution, and filtering to obtain an iron and phosphorus solution; analyzing the concentration of iron and phosphorus in the solution, and adding ferrous sulfate or phosphoric acid to make the concentration ratio of iron to phosphorus in the solution be 1; and synchronously adding the solution, hydrogen peroxide and sodium hydroxide solution into a reaction container containing iron phosphate crystal seeds, stirring, controlling the reaction pH to be 1.5-2.0, stirring, reacting, aging, filtering, washing and calcining the solid product to obtain the iron phosphate for the battery.
Further, in the step (1), the pH value of the solution should be controlled to be 3.5-5, the solid-to-liquid ratio should be 200-500 g/L, the reaction time should be 1-10 h, and the reaction temperature should be 20-90 ℃ in the reaction process of the lithium iron phosphate and the air.
Further, the solid-liquid ratio of the sulfuric acid dissolved out in the step (3) by stirring is controlled to be 250-500 g/L, and the molar weight of the sulfuric acid is 1.1-1.5 times of the molar weight of iron in the solid material.
Compared with the prior art, the invention has the following advantages:
(1) the recovery rate of lithium is up to more than 95%, and the purity of the further prepared lithium carbonate is over 99%; the iron-phosphorus slag is activated and reduced by adopting iron powder and leached by sulfuric acid, the leaching rate of iron and phosphorus is more than 95 percent, and high-quality battery-grade iron phosphate can be prepared;
(2) the method has the advantages that cheap air is used as an oxidant to directly oxidize the lithium iron phosphate anode waste, iron phosphorus slag is reduced by iron powder, efficient leaching of iron and phosphorus can be achieved without adding excessive acid after reduction, and the whole process is wide in reagent source, low in price and good in economical efficiency;
(3) the waste water treatment capacity is less, and the environment is friendly.
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 lithium iron phosphate anode waste powder into water for size mixing, then introducing air into the aqueous solution, controlling the oxidation leaching conditions to be a solid-to-liquid ratio of 500g/L, a reaction time of 1 hour, a reaction temperature of 25 ℃, and slowly adding dilute sulfuric acid to maintain the pH value at about 5 in the process. After the reaction is finished, lithium-containing aqueous solution and iron-phosphorus slag are obtained by filtering, and the leaching rate of lithium is 98.5%. Adjusting pH of the lithium solution to 11, filtering to remove solid impurities, heating the filtrate to 95 deg.C, and adding saturated Na2CO3And (3) reacting the solution to obtain lithium carbonate precipitate, and washing and drying the lithium carbonate precipitate to obtain a lithium carbonate product. Adding iron powder into the water-immersed slagBall 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 2 hours; dissolving the product after ball milling activation by using sulfuric acid, controlling the solid-liquid ratio of stirring dissolution to be 250g/L, using the molar weight of the sulfuric acid to be 1.2 times of the molar weight of iron in the material, filtering to obtain iron and phosphorus solutions, and analyzing the leaching rates of iron and phosphorus to be 96.3% and 95.7% respectively. Adding phosphoric acid to adjust the molar ratio of iron to phosphorus in the solution to be 1, synchronously adding the solution, hydrogen peroxide and sodium hydroxide solution into a reaction container containing iron phosphate crystal seeds, stirring, controlling the reaction pH to be 2.0, carrying out stirring reaction, ageing, filtering, washing and calcining a solid product to obtain the iron phosphate for the battery.
Example 2
Adding lithium iron phosphate anode waste powder into water for size mixing, then introducing air into the aqueous solution, controlling the oxidation leaching conditions to be a solid-to-liquid ratio of 200g/L, a reaction time of 3 hours, a reaction temperature of 50 ℃, and slowly adding dilute sulfuric acid to maintain the pH value at about 3.5 in the process. After the reaction is finished, lithium-containing aqueous solution and iron-phosphorus slag are obtained by filtering, and the leaching rate of lithium is 99.1%. Adjusting pH of the lithium solution to 11, filtering to remove solid impurities, heating the filtrate to 95 deg.C, and adding saturated Na2CO3And (3) reacting the solution to obtain lithium carbonate precipitate, and washing and drying the lithium carbonate precipitate to obtain a lithium carbonate product. Adding iron powder into the water leaching residues 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 residues, and the ball milling time is 0.5 hour; dissolving the product after ball milling activation by using sulfuric acid, controlling the solid-liquid ratio of stirring dissolution to be 500g/L, using the molar weight of the sulfuric acid to be 1.1 times of the molar weight of iron in the material, filtering to obtain iron and phosphorus solutions, and analyzing the leaching rates of iron and phosphorus to be 95.3% and 96.2% respectively. Adding phosphoric acid to adjust the molar ratio of iron to phosphorus in the solution to be 1, synchronously adding the solution, hydrogen peroxide and sodium hydroxide solution into a reaction container containing iron phosphate crystal seeds, stirring, controlling the reaction pH to be 1.5, carrying out stirring reaction, ageing, filtering, washing and calcining a solid product to obtain the iron phosphate for the battery.
Example 3
Adding lithium iron phosphate anode waste powderAdding into water for size mixing, then introducing air into the aqueous solution, controlling the oxidation leaching conditions to be 300g/L of solid-liquid ratio, 5 hours of reaction time and 90 ℃ of reaction temperature, and slowly adding dilute sulfuric acid to maintain the pH value to be about 4.0 in the process. After the reaction is finished, lithium-containing aqueous solution and iron-phosphorus slag are obtained by filtering, and the leaching rate of lithium is 98.3%. Adjusting pH of the lithium solution to 11, filtering to remove solid impurities, heating the filtrate to 95 deg.C, and adding saturated Na2CO3And (3) reacting the solution to obtain lithium carbonate precipitate, and washing and drying the lithium carbonate precipitate to obtain a lithium carbonate product. Adding iron powder into the water leaching residues 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 residues, and the ball milling time is 1 hour; dissolving the product after ball milling activation by using sulfuric acid, controlling the solid-liquid ratio of stirring dissolution to be 400g/L, using the molar weight of the sulfuric acid to be 1.4 times of the molar weight of iron in the material, filtering to obtain iron and phosphorus solutions, and analyzing the leaching rates of iron and phosphorus to be 97.2% and 96.9% respectively. Adding phosphoric acid to adjust the molar ratio of iron to phosphorus in the solution to be 1, synchronously adding the solution, hydrogen peroxide and sodium hydroxide solution into a reaction container containing iron phosphate crystal seeds, stirring, controlling the reaction pH to be 1.8, carrying out stirring reaction, ageing, filtering, washing and calcining a solid product to obtain the iron phosphate for the battery.
Claims (3)
1. A method for efficiently recycling lithium as a lithium iron phosphate positive waste material and preparing battery-grade iron phosphate is characterized by comprising the following steps of:
(1) adding the lithium iron phosphate waste into water, blowing air and stirring, reacting for a certain time, and then carrying out solid-liquid separation, wherein the filtrate is a lithium-containing solution and can be used for preparing a lithium product;
(2) mixing the water leaching slag obtained in the step (1), iron powder and a small amount of sulfuric acid, and putting the mixture into a planetary ball mill for ball milling activation, wherein the molar weight of the added iron powder is 0.55-1 time of that of iron in the water leaching slag, and the ball milling time is 0.5-2 hours;
(3) stirring and dissolving the solid product obtained after the activation in the step (2) by using a sulfuric acid solution, and filtering to obtain an iron and phosphorus solution; analyzing the concentration of iron and phosphorus in the solution, and adding ferrous sulfate or phosphoric acid to make the concentration ratio of iron to phosphorus in the solution be 1; and synchronously adding the solution, hydrogen peroxide and sodium hydroxide solution into a reaction container containing iron phosphate crystal seeds, stirring, controlling the reaction pH to be 1.5-2.0, stirring, reacting, aging, filtering, washing and calcining the solid product to obtain the iron phosphate for the battery.
2. The method for efficiently recycling lithium as the lithium iron phosphate positive electrode waste material and preparing the battery-grade iron phosphate according to claim 1, wherein in the step (1), the pH of the solution should be controlled to be 3.5-5, the solid-to-liquid ratio should be 200-500 g/L, the reaction time should be 1-10 h, and the reaction temperature should be 20-90 ℃.
3. The method for efficiently recycling lithium as the lithium iron phosphate cathode waste material and preparing battery-grade phosphoric acid according to claim 1, wherein the solid-to-liquid ratio of stirring and dissolving sulfuric acid in the step (3) is controlled to be 250-500 g/L, and the molar weight of the sulfuric acid is 1.1-1.5 times of the molar weight of iron in the solid material.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603119A (en) * | 2021-08-03 | 2021-11-05 | 广东邦普循环科技有限公司 | Method for recovering lithium from waste lithium iron phosphate material |
| CN113666397A (en) * | 2021-08-21 | 2021-11-19 | 福州大学 | Method for economically recycling lithium from waste lithium iron phosphate material by acid process |
| CN113800488A (en) * | 2021-10-13 | 2021-12-17 | 中南大学 | Resource recovery method of lithium iron phosphate waste |
| CN113912035A (en) * | 2021-11-29 | 2022-01-11 | 材料科学姑苏实验室 | Method for recovering battery-grade iron phosphate material from phosphorus-iron slag |
| CN114408888A (en) * | 2021-12-23 | 2022-04-29 | 广东臻鼎环境科技有限公司 | Method for preparing battery-grade iron phosphate powder by using aluminum-containing waste acid solution |
| CN115448279A (en) * | 2022-10-25 | 2022-12-09 | 四川长虹格润环保科技股份有限公司 | Method for preparing battery-grade iron phosphate material by recycling phosphorus-iron slag after lithium extraction |
| CN115924879A (en) * | 2023-01-18 | 2023-04-07 | 河南佰利新能源材料有限公司 | Method for recycling lithium iron phosphate from scrap lithium iron phosphate material |
| CN116409764A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院过程工程研究所 | Method for preparing ferric phosphate from refined phosphoric acid |
| CN116409766A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院过程工程研究所 | Method for flexibly regulating and controlling iron-phosphorus ratio of iron phosphate |
| CN116409765A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院过程工程研究所 | Regeneration method of iron phosphate-containing waste |
| 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 |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603119A (en) * | 2021-08-03 | 2021-11-05 | 广东邦普循环科技有限公司 | Method for recovering lithium from waste lithium iron phosphate material |
| 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 |
| CN113666397A (en) * | 2021-08-21 | 2021-11-19 | 福州大学 | Method for economically recycling lithium from waste lithium iron phosphate material by acid process |
| CN113800488B (en) * | 2021-10-13 | 2023-02-21 | 中南大学 | Resource recovery method of lithium iron phosphate waste |
| CN113800488A (en) * | 2021-10-13 | 2021-12-17 | 中南大学 | Resource recovery method of lithium iron phosphate waste |
| CN113912035A (en) * | 2021-11-29 | 2022-01-11 | 材料科学姑苏实验室 | Method for recovering battery-grade iron phosphate material from phosphorus-iron slag |
| CN114408888B (en) * | 2021-12-23 | 2023-09-19 | 广东臻鼎环境科技有限公司 | Method for preparing battery grade ferric phosphate powder by using aluminum-containing waste acid liquid |
| CN114408888A (en) * | 2021-12-23 | 2022-04-29 | 广东臻鼎环境科技有限公司 | Method for preparing battery-grade iron phosphate powder by using aluminum-containing waste acid solution |
| CN116409764A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院过程工程研究所 | Method for preparing ferric phosphate from refined phosphoric acid |
| CN116409766A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院过程工程研究所 | Method for flexibly regulating and controlling iron-phosphorus ratio of iron phosphate |
| CN116409765A (en) * | 2021-12-30 | 2023-07-11 | 中国科学院过程工程研究所 | Regeneration method of iron phosphate-containing waste |
| CN115448279A (en) * | 2022-10-25 | 2022-12-09 | 四川长虹格润环保科技股份有限公司 | Method for preparing battery-grade iron phosphate material by recycling phosphorus-iron slag after lithium extraction |
| CN115448279B (en) * | 2022-10-25 | 2024-03-26 | 四川长虹格润环保科技股份有限公司 | Method for preparing battery grade ferric phosphate material by recycling lithium-extracted ferrophosphorus slag |
| CN115924879A (en) * | 2023-01-18 | 2023-04-07 | 河南佰利新能源材料有限公司 | Method for recycling lithium iron phosphate from scrap lithium iron phosphate material |
| 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 |
| CN116864851B (en) * | 2023-09-05 | 2023-11-21 | 赣州市力道新能源有限公司 | Process for deeply removing phosphorus from retired battery recovery feed liquid |
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