CN106848472B - Method for recycling lithium from waste lithium iron phosphate batteries - Google Patents
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- H01—ELECTRIC ELEMENTS
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- H01M10/00—Secondary cells; Manufacture thereof
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- 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 provides a method for efficiently recovering lithium from waste lithium iron phosphate batteries, which comprises the steps of roasting and sorting the waste lithium iron phosphate batteries to obtain lithium-containing positive electrode powder, reacting the lithium-containing powder with a calcium-containing alkaline solution under an oxidation condition, converting iron and phosphate radicals into water-insoluble compounds, converting lithium into water-soluble lithium hydroxide, filtering to obtain a lithium hydroxide solution, and further preparing a lithium hydroxide or lithium carbonate product; the method abandons wet acid leaching conventionally adopted in the waste battery recovery process, avoids the use of strong acid, and thus avoids the generation of a large amount of high-salinity wastewater; the process selectively leaches lithium elements, avoids the problem that iron impurities enter leachate from the source, finally obtains a high-purity lithium product, has short flow, wide sources of chemical agents and simple process conditions, can obtain the high-purity lithium product by one-step method, greatly improves the recovery efficiency of the waste lithium iron phosphate batteries, and has good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of secondary resource recycling and circular economy, and particularly relates to a method for recycling lithium from waste lithium iron phosphate batteries.
Background
Energy and environment become increasingly interesting issues. With the gradual depletion of petroleum resources and the aggravation of air pollution caused by the emission of automobile exhaust, electric vehicles and hybrid electric vehicles are valued by governments and automobile enterprises. With the development of electric automobiles, lithium iron phosphate batteries are widely used due to the advantages of abundant raw material resources, low price, no environmental pollution, stable structure, good thermal stability and the like. Along with the use of a large number of lithium iron phosphate batteries, the recycling of the waste batteries becomes a new task, the recycling of the waste batteries can reduce the influence of the waste batteries on the environment, and can bring certain economic benefits and reduce the battery cost.
The recovery technology of the waste lithium iron phosphate batteries combines hydrometallurgy and high-temperature metallurgy, and lithium iron phosphate anode materials are obtained through wet leaching and high-temperature calcination regeneration, for example, CN102280673A, CN104362408A and CN102751548A respectively disclose process methods for preparing lithium iron phosphate products through wet leaching and calcination in an oxidizing atmosphere of the waste batteries. The method for directly recovering lithium iron phosphate by high-temperature calcination needs a plurality of processes such as ball milling, high-temperature calcination, ball milling again, sintering again and the like, and has harsh process conditions, large energy consumption and complex flow, so the method is not widely used. In order to simplify the recovery process and reduce the recovery cost, researchers at home and abroad develop various recovery technologies based on wet metallurgy, the main process is to roast and crush waste batteries to obtain a mixed material, then remove aluminum by an alkaline method to obtain iron and lithium mixed slag, simultaneously leach out iron and lithium elements, and then selectively precipitate to obtain a lithium product. For example, CN102285673A discloses a method for recovering iron and lithium from an electric vehicle lithium iron phosphate power battery, which comprises leaching iron and lithium simultaneously with an acid and a reducing agent, adjusting the pH of the leachate to 1.5-3, precipitating iron hydroxide to obtain an iron oxide product, adjusting the pH of the filtrate with an alkali, and removing impurities to prepare lithium carbonate. CN101847763A is prepared by dissolving in organic solvent and acid hydrolyzing to obtain Cu, Fe, Li and P solution, adding sodium sulfide and adjusting pH to remove Cu and Fe. In the above-mentioned methods for recovering lithium by wet leaching, iron and lithium are leached out simultaneously, and then further separation of iron and lithium is performed, which often consumes a large amount of acid liquor and is accompanied by the problems of impurity in leachate and generation of a large amount of high-salinity wastewater.
Disclosure of Invention
The invention aims to solve the problems that the existing recovery leaching process is long in flow, low in leaching rate, accompanied with generation of a large amount of high-salinity wastewater and the like, and provides a method for recovering lithium from waste lithium iron phosphate batteries. The method selectively leaches lithium element, so that the problem that iron impurities enter a leaching solution is avoided from the source, and the lithium product obtained by recovery has high purity. And roasting and sorting the waste lithium iron phosphate batteries to obtain lithium-containing anode powder. The lithium-containing powder is reacted with a calcium-containing alkaline solution under oxidizing conditions to convert iron and phosphate to water-insoluble compounds and lithium to water-soluble lithium hydroxide. And filtering to obtain a lithium hydroxide solution which can be used for further preparing a lithium hydroxide or lithium carbonate product. The method abandons wet acid leaching conventionally adopted in the waste battery recovery process, and avoids the use of strong acid, thereby avoiding the generation of a large amount of high-salinity wastewater. The method has the advantages of short flow, wide chemical agent source and simple process conditions, can obtain high-purity lithium products by one step, greatly improves the recovery efficiency of the waste lithium iron phosphate batteries, and has good industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for recovering lithium from waste lithium iron phosphate batteries comprises the following steps:
(1) roasting and sorting the waste lithium iron phosphate batteries to obtain lithium-containing anode powder;
(2) adding the positive electrode powder obtained in the step (1) into a calcium-containing alkaline solution in an oxidizing environment, converting iron and phosphate radicals into water-insoluble compounds, and converting lithium into water-soluble lithium hydroxide;
(3) filtering the solution obtained in the step (2) to remove water-insoluble iron compounds and phosphates to obtain a lithium hydroxide solution;
(4) and (4) further preparing a lithium hydroxide or lithium carbonate product from the lithium hydroxide solution obtained in the step (3).
The method of claim 1, wherein the lithium iron phosphate waste battery is crushed, roasted and sorted in the step (1) to obtain lithium-containing positive electrode powder;
preferably, the battery positive electrode material is crushed into fragments of 1-20 mm multiplied by 1-20 mm through mechanical crushing;
preferably, the roasting temperature is 200-1200 ℃;
preferably, the roasting time is 1-6 h.
In the roasting process of the step (1), calcium-containing powder can be sprayed to absorb the generation of fluorine-containing gas;
preferably, the calcium-containing powder is one or a combination of any more of a calcium-containing inorganic substance, a calcium-containing organic substance and a calcium-containing biomass;
preferably, the calcium-containing powder is CaC2、CaCl2、CaCO3、Ca(NO3)2、CaO、Ca(OH)2、Ca5(PO4)3(OH)、C36H70CaO4、C6H10CaO6、C6H10CaO6、Ca(HCO2)2、Ca(CH3COO)2、CaC2O4One or any combination of a plurality of the components;
preferably, the mass ratio of the battery waste to the calcium-containing powder is 0.1-3000: 1, and more preferably 20-300: 1;
preferably, after roasting, metals such as aluminum, copper and the like can be removed by adopting gravity separation, cyclone or screening to obtain lithium-containing powder.
Adding the obtained positive electrode powder into a calcium-containing alkaline solution, reacting in an oxidizing environment, converting iron and phosphate radicals into water-insoluble compounds, and converting lithium into water-soluble lithium hydroxide;
preferably, the oxidizing environment is formed by adding or introducing oxidant air and H into the solution2O2、MnO2、KMnO4、O2One or a combination of several of (1);
preferably, the calcium-containing alkaline solution is an alkaline solution containing calcium ions or an alkaline suspension containing calcium;
preferably, the mass concentration of the calcium element (ions or solids) in the calcium-containing solution or suspension is 0.1 to 100%.
And (3) filtering the obtained solution, and removing water-insoluble iron compounds and phosphates to obtain a lithium hydroxide solution.
Concentrating the obtained lithium hydroxide solution, removing impurities and extracting, directly preparing lithium hydroxide, cleaning to obtain high-purity lithium hydroxide, or concentrating until the concentration of lithium ions is 200-500 g/L, adding a saturated sodium carbonate solution to precipitate lithium carbonate, separating and cleaning to obtain high-purity lithium carbonate, wherein the concentration temperature is 40-100 ℃, the precipitation temperature is 20-100 ℃, the precipitation stirring speed is 100-2000 rpm, the precipitation stirring adjustment time is 0.5-72 h, and the temperature of washing water is 10-100 ℃;
preferably, the concentration temperature is 70-100 ℃;
preferably, the precipitation temperature is 60-100 ℃;
preferably, the precipitation stirring speed is 100-500 rpm;
preferably, the precipitation stirring adjustment time is 2-12 h;
preferably, the molar ratio of carbonate ions added by precipitation to lithium ions in the solution is 1-3: 2;
preferably, the temperature of the water used for washing is 40-100 ℃.
Drawings
Fig. 1 is a process flow chart of a method for efficiently recovering lithium from waste lithium iron phosphate batteries.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the examples described are only for the aid of understanding the present invention and should not be construed as specifically limiting the present invention.
Examples
Some, but not all embodiments of the invention are intended to cover all alternative embodiments, which can be devised by those skilled in the art based on the embodiments of the invention without any creative effort.
Example 1
(1) Crushing the waste lithium iron phosphate battery positive electrode material into fragments with the size of 1-20 mm multiplied by 1-20 mm, roasting for 2 hours at the high temperature of 800 ℃, spraying CaO in the roasting process to prevent the generation of fluorine-containing gas, and controlling the mass ratio of the battery waste to calcium-containing powder to be 300: 1. After the baking and sintering, the metals such as aluminum, copper and the like are removed by screening to obtain the lithium-containing powder.
TABLE 1 lithium iron phosphate battery roasting and sorting to obtain lithium-containing powder component (wt%)
| Fe | P | Li |
| 25.7 | 14.4 | 3.2 |
(2) Adding the obtained positive electrode powder into a solution containing Ca (OH)2And (3) introducing oxygen (the volume ratio of the oxidant to the powder solution containing the positive electrode is 10) in the reaction process to convert iron and phosphate radicals into water-insoluble compounds and convert lithium into water-soluble lithium hydroxide. SolutionThe mass concentration of liquid calcium element (ions or solids) is 15%, and the mass ratio of the positive electrode powder to the calcium element is 2: 1.
(3) and filtering the obtained solution to remove ferric hydroxide, calcium phosphate and calcium hydroxide which is not completely reacted to obtain a lithium hydroxide solution.
(4) The obtained lithium hydroxide solution was concentrated to a lithium ion concentration of 250g/L, a saturated sodium carbonate solution was added to precipitate lithium carbonate, and the obtained high-purity lithium carbonate (purity 99.97%) was separated and washed. The precipitation temperature of the sodium carbonate is 95 ℃, the precipitation stirring speed is 500rpm, the stirring adjustment time is 2-12 h, the molar ratio of carbonate ions to lithium ions in the solution is 1.5:1, and the temperature of water for washing is 90 ℃.
Example 2
(1) Crushing the waste lithium iron phosphate battery positive electrode material into fragments with the size of 1-20 mm multiplied by 1-20 mm, roasting for 2 hours at the high temperature of 1000 ℃, spraying CaO in the roasting process to prevent the generation of fluorine-containing gas, and controlling the mass ratio of the battery waste to calcium-containing powder to be 300: 1. After the baking and sintering, the metals such as aluminum, copper and the like are removed by screening to obtain the lithium-containing powder.
TABLE 2 lithium iron phosphate battery roasting and sorting to obtain lithium-containing powder component (wt%)
| Fe | P | Li |
| 19.2 | 8.7 | 1.7 |
(2) Adding the obtained positive electrode powder into a solution containing Ca (OH)2Alkaline suspension and at the same timeAdding KMnO2Solution (anode powder solution/KMnO2The mass ratio of the solution is 20, KMnO2Solution concentration of 10%), iron and phosphate are converted to water insoluble compounds, and lithium is converted to water soluble lithium hydroxide. The mass concentration of the solution calcium element (ions or solids) is 15 percent, and the mass ratio of the positive electrode powder to the calcium element is 2: 1.
(3) and filtering the obtained solution to remove ferric hydroxide, calcium phosphate and calcium hydroxide which is not completely reacted to obtain a lithium hydroxide solution.
(4) And concentrating the obtained lithium hydroxide solution to directly prepare lithium hydroxide, wherein the concentration temperature is 95 ℃, removing impurities and extracting to obtain high-purity lithium hydroxide (the purity reaches 99.95%), and the temperature of water for washing is 90 ℃.
Example 3
(1) Crushing the anode material of the waste lithium iron phosphate battery into fragments of 1-20 mm multiplied by 1-20 mm, roasting for 2 hours at the high temperature of 1200 ℃, and spraying CaCO in the roasting process3Prevent the generation of fluorine-containing gas, and control the mass ratio of the battery waste to the calcium-containing powder at 300: 1. After the baking and sintering, the metals such as aluminum, copper and the like are removed by screening to obtain the lithium-containing powder.
TABLE 3 lithium-containing powder component (wt%) obtained by roasting and sorting lithium iron phosphate battery
| Fe | P | Li |
| 23.1 | 10.5 | 2.1 |
(2) To obtainAdding the superfine powder into the Ca-containing solution, and adding H2O2Solution (anode powder solution/H)2O2Solution mass ratio of 30, H2O2Solution concentration 15%), iron and phosphate were converted to water insoluble compounds, and lithium was converted to water soluble lithium hydroxide. The mass concentration of the solution calcium element (ions or solids) is 15 percent, and the mass ratio of the positive electrode powder to the calcium element is 2: 1.
(3) and filtering the obtained solution to remove ferric hydroxide, calcium phosphate and calcium hydroxide which is not completely reacted to obtain a lithium hydroxide solution.
(4) The obtained lithium hydroxide solution was concentrated to a lithium ion concentration of 250g/L, a saturated sodium carbonate solution was added to precipitate lithium carbonate, and the obtained high-purity lithium carbonate (purity 99.98%) was separated and washed. The precipitation temperature of the sodium carbonate is 95 ℃, the precipitation stirring speed is 500rpm, the stirring adjustment time is 2-12 h, the molar ratio of carbonate ions to lithium ions in the solution is 1.5:1, and the temperature of water for washing is 90 ℃.
The applicant states that the present invention is illustrated by the above examples of the process of the present invention, but the present invention is not limited to the above process steps, i.e. it is not meant that the present invention must rely on the above process steps to be carried out. It will be apparent to those skilled in the art that any modification of the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific modes and the like, which are within the scope and disclosure of the present invention, are contemplated by the present invention.
Claims (17)
1. A method for recovering lithium from waste lithium iron phosphate batteries is characterized by comprising the following steps:
(1) roasting and sorting the waste lithium iron phosphate batteries to obtain lithium-containing anode powder;
(2) adding the positive electrode powder obtained in the step (1) into a calcium-containing alkaline solution in an oxidizing environment, converting iron and phosphate radicals into water-insoluble compounds, and converting lithium into water-soluble lithium hydroxide;
(3) filtering the solution obtained in the step (2) to remove water-insoluble iron compounds and phosphates to obtain a lithium hydroxide solution;
(4) further preparing a lithium hydroxide or lithium carbonate product from the lithium hydroxide solution obtained in the step (3);
spraying calcium-containing powder to absorb the generation of fluorine-containing gas in the roasting process in the step (1);
the calcium-containing alkaline solution contains Ca (OH)2Alkaline suspension; the Ca (OH) containing2The mass concentration of calcium element in the alkaline suspension is 0.1-15%;
the oxidizing environment is formed by adding or introducing air and H into the solution2O2、MnO2、KMnO4、O2One or a combination of several of them.
2. The method of claim 1, wherein the lithium iron phosphate waste battery is crushed, roasted and sorted in the step (1) to obtain lithium-containing positive electrode powder.
3. The method according to claim 2, wherein the battery positive electrode material is crushed into pieces of 1 to 20mm x 1 to 20mm by mechanical crushing.
4. The method of claim 1, wherein the calcination temperature is 200 to 1200 ℃.
5. The method of claim 1, wherein the calcination time is 1 to 6 hours.
6. The method of claim 1, wherein the calcium-containing powder is one or a combination of any of inorganic calcium-containing material, organic calcium-containing material, and biomass calcium-containing material.
7. The method of claim 6, wherein the calcium-containing powder is CaC2、CaCl2、CaCO3、Ca(NO3)2、CaO、Ca(OH)2、Ca5(PO4)3(OH)、C36H70CaO4、C6H10CaO6、C6H10CaO6、Ca(HCO2)2、Ca(CH3COO)2、CaC2O4One or any combination of several of them.
8. The method according to claim 1, wherein the mass ratio of the waste lithium iron phosphate battery to the calcium-containing powder is 0.1-3000: 1.
9. The method according to claim 1, wherein the mass ratio of the waste lithium iron phosphate battery to the calcium-containing powder is 20-300: 1.
10. The method of claim 1, wherein the aluminum and/or copper is removed by gravity separation, swirling or screening after firing to obtain the lithium-containing powder.
11. The method according to claim 1, wherein the lithium hydroxide solution obtained in the step (4) is concentrated, the lithium hydroxide is directly prepared after impurity removal and extraction, and is washed to obtain high-purity lithium hydroxide, or the lithium hydroxide solution is concentrated until the concentration of lithium ions is 200-500 g/L, a saturated sodium carbonate solution is added to precipitate lithium carbonate, and the high-purity lithium carbonate obtained is separated and washed, wherein the concentration temperature is 40-100 ℃, the precipitation temperature is 20-100 ℃, the precipitation stirring speed is 100-2000 rpm, the precipitation stirring adjusting time is 0.5-72 h, and the washing water temperature is 10-100 ℃.
12. The method according to claim 11, wherein the concentration temperature is 70 to 100 ℃.
13. The method according to claim 11, wherein the precipitation temperature is 60 to 100 ℃.
14. The method according to claim 11, wherein the stirring speed for precipitation is 100 to 500 rpm.
15. The method according to claim 11, wherein the settling stirring is adjusted for 2 to 12 hours.
16. The method according to claim 11, wherein the molar ratio of carbonate ions added by precipitation to lithium ions in the solution is 1-3: 2.
17. The method according to claim 14, wherein the temperature of the water used for washing is 40 to 100 ℃.
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| CN115353129B (en) * | 2022-09-27 | 2023-09-01 | 厦门海辰储能科技股份有限公司 | Method for recycling anode material of waste lithium iron phosphate battery |
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| IT1402751B1 (en) * | 2010-11-12 | 2013-09-18 | Ecir Eco Iniziativa E Realizzazioni S R L | METHOD FOR CONDITIONING SCORES ARISING FROM DISPOSAL OF NUCLEAR PLANTS |
| KR101405486B1 (en) * | 2012-04-05 | 2014-06-13 | 주식회사 포스코 | Method for manufacturing lithium hydroxide and method for manufacturing lithium carbonate using the same |
| CN104310690B (en) * | 2014-10-28 | 2016-01-20 | 中冶南方工程技术有限公司 | Metal nitrate, the regeneration of hydrofluoric acid spent pickle liquor and the recovery process of metallic element |
| CN104909497A (en) * | 2015-06-07 | 2015-09-16 | 长春黄金研究院 | Method for treating acid waste water of nonferrous metal mine |
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