CN112626357B - Method for extracting lithium from waste lithium iron phosphate powder - Google Patents

Method for extracting lithium from waste lithium iron phosphate powder Download PDF

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CN112626357B
CN112626357B CN202011474742.XA CN202011474742A CN112626357B CN 112626357 B CN112626357 B CN 112626357B CN 202011474742 A CN202011474742 A CN 202011474742A CN 112626357 B CN112626357 B CN 112626357B
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lithium
iron phosphate
leaching
sulfuric acid
waste
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CN112626357A (en
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周有池
郭春平
文小强
刘雯雯
洪侃
赖华生
王玉香
普建
周新华
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Ganzhou Nonferrous Metallurgy Research Institute Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10Obtaining alkali metals
    • C22B26/12Obtaining lithium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/02Roasting processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/54Reclaiming serviceable parts of waste accumulators
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/84Recycling of batteries or fuel cells

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  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for extracting lithium from waste lithium iron phosphate powder, belonging to the technical field of lithium resource recovery. The method provided by the invention comprises the following steps: mixing waste lithium iron phosphate powder with sulfuric acid to obtain a raw material; the concentration of the sulfuric acid is 45-55 wt%, and the mass of the sulfuric acid is 10-50% of that of the waste lithium iron phosphate powder; roasting the raw material by microwave to obtain clinker; mixing the clinker with water and then carrying out leaching treatment to obtain leaching slurry; carrying out solid-liquid separation on the leaching slurry to obtain a lithium solution and iron phosphate slag; and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution. The method provided by the invention can selectively extract valuable metal lithium from the waste lithium iron phosphate powder by controlling the dosage of sulfuric acid and adopting a microwave roasting mode, and can extract phosphorus and iron in the waste lithium iron phosphate powder asynchronously, so that the operation process is simple and the cost is low.

Description

Method for extracting lithium from waste lithium iron phosphate powder
Technical Field
The invention relates to the technical field of lithium resource recovery, in particular to a method for extracting lithium from waste lithium iron phosphate powder.
Background
The lithium iron phosphate power battery has excellent safety, stability and cycle performance, and is low in price and pollution-free, and widely applied to buses and cars. After the lithium ion power battery is periodically charged and discharged, the internal structure of the battery can be irreversibly changed, so that a lithium ion channel is blocked, and the lithium ion power battery fails. Therefore, the lithium ion power battery has a certain service cycle, the service cycle of a common lithium iron phosphate battery is 3-5 years, and how to effectively recycle the waste lithium iron phosphate battery is a focus of attention of researchers at present.
The waste lithium iron phosphate battery is subjected to discharging, disassembling and screening treatment to obtain waste lithium iron phosphate powder, wherein the waste lithium iron phosphate powder contains valuable metal lithium, and the content of the valuable metal lithium is about 3.7%. At present, a method for recovering lithium from waste lithium iron phosphate powder is mainly based on a wet method, in patent CN106684485B, Li, Cu and Fe in the waste lithium iron phosphate powder are all leached by using inorganic acid and hydrogen peroxide, and then the pH value is adjusted back by using alkali, so that iron is precipitated in the form of iron phosphate, and lithium is retained in a solution, thereby respectively obtaining a lithium product and iron phosphate; however, the process has the problems of high acid and alkali consumption and high production cost.
In order to overcome the drawbacks of the conventional process, it is proposed in patent application CN109473691A to use H 3 PO 4 -H 2 O 2 The system selectively leaches lithium in the form of lithium dihydrogen phosphate by regulating and controlling the pH value of the slurry, and the filter residue is ferric phosphate and carbon powder. The use of HCl-H has also been proposed by scholars 2 O 2 The pH value of the system is controlled to be 3.5-4.0, so that lithium is selectively leached in the form of lithium chloride, and filter residues are ferric phosphate and carbon powder. Although lithium can be selectively recovered by the above process, it is preferable to use H 3 PO 4 -H 2 O 2 In terms of a system, the price of phosphoric acid and hydrogen peroxide is high, the content of phosphate radicals in a leaching solution is high, and the further treatment cost is high; while in HCl-H 2 O 2 In the system, H 2 O 2 The dosage of the catalyst is more than 2 times of the theoretical value, and Cl is formed in the leaching process 2 The equipment requirements are high, resulting in high costs for lithium recovery.
Patent application CN110331288A proposes that waste lithium iron phosphate powder is introduced into selective gas (such as sulfur dioxide or chlorine gas) for roasting, so that lithium iron phosphate is decomposed into iron phosphate and lithium-containing compounds, and the lithium-containing solution and iron phosphate solid are obtained by filtering after wet ball milling. The process can reduce the recovery cost of lithium to a certain extent, but selective gas is required to be introduced, so that the problems of tail gas recovery, poor operating environment and the like exist in industrial production, and the total treatment cost is still higher.
Disclosure of Invention
The invention aims to provide a method for extracting lithium from waste lithium iron phosphate powder, and the method provided by the invention can selectively extract valuable metal lithium from the waste lithium iron phosphate powder by controlling the using amount of sulfuric acid and adopting a microwave roasting mode, and can extract phosphorus and iron from the waste lithium iron phosphate powder asynchronously, and has the advantages of simple operation process and low cost.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for extracting lithium from waste lithium iron phosphate powder, which comprises the following steps:
mixing waste lithium iron phosphate powder with sulfuric acid to obtain a raw material; the concentration of the sulfuric acid is 45-55 wt%, and the mass of the sulfuric acid is 10-50% of that of the waste lithium iron phosphate powder;
roasting the raw material by microwave to obtain clinker;
mixing the clinker with water and then carrying out leaching treatment to obtain leaching slurry;
carrying out solid-liquid separation on the leaching slurry to obtain a lithium solution and iron phosphate slag;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
Preferably, the lithium content in the waste lithium iron phosphate powder is 3.5-3.7 wt%.
Preferably, the microwave roasting temperature is 400-800 ℃.
Preferably, the microwave roasting time is 60-240 min.
Preferably, the microwave roasting is performed in an air atmosphere.
Preferably, the mass ratio of the clinker to the water is 1: (2.5-3.5).
Preferably, the temperature of the leaching treatment is 40-60 ℃.
Preferably, the leaching time is 30-60 min.
Preferably, the solid-liquid separation mode is filtration.
Preferably, the solid-liquid separation device further comprises: the resulting solid material was washed with water.
The invention provides a method for extracting lithium from waste lithium iron phosphate powder, which comprises the following steps: mixing waste lithium iron phosphate powder with sulfuric acid to obtain a raw material; the concentration of the sulfuric acid is 45-55 wt%, and the mass of the sulfuric acid is 10-50% of that of the waste lithium iron phosphate powder; roasting the raw material by microwave to obtain clinker; mixing the clinker with water and then carrying out leaching treatment to obtain leaching slurry; carrying out solid-liquid separation on the leaching slurry to obtain a lithium solution and iron phosphate slag; and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution. The method provided by the invention can selectively extract valuable metal lithium in the waste lithium iron phosphate powder, and synchronously extract phosphorus and iron in the waste lithium iron phosphate powder, and has the advantages of simple operation process and low cost; according to the invention, by controlling the use amount of sulfuric acid and adopting a microwave roasting mode, lithium is preferentially leached, the impurity content in the lithium-rich solution obtained by twice countercurrent leaching is low (the total content of iron and phosphorus can be as low as 1.53g/L), the lithium concentration is high (20-26 g/L), other concentration processes are not needed, the preparation of a lithium salt high-purity product can be easily realized, and the method has the advantages of energy conservation, environmental protection, simplicity and easiness in implementation.
Furthermore, compared with the conventional roasting mode, the microwave roasting mode adopted by the invention has low roasting temperature and short roasting time, and is beneficial to saving energy consumption.
Furthermore, the method provided by the invention can destroy the structure of lithium iron phosphate in the waste lithium iron phosphate powder by adopting sulfuric acid and microwave roasting at the same time, so that lithium in the lithium iron phosphate is converted into lithium salt which is easy to dissolve in the solution, the lithium solution can be obtained after subsequent water leaching treatment and solid-liquid separation, other auxiliaries are not needed, selective gas is not needed, the cost is low, the impurity content in the lithium-rich solution obtained by performing countercurrent leaching twice on the finally obtained lithium solution is low, the impurity removal process is simplified, and the iron phosphate slag can be comprehensively recycled. The method provided by the invention has the advantages of mild reaction conditions, simple flow and strong operability, and is suitable for industrial production.
Detailed Description
The invention provides a method for extracting lithium from waste lithium iron phosphate powder, which comprises the following steps:
mixing waste lithium iron phosphate powder with sulfuric acid to obtain a raw material; the concentration of the sulfuric acid is 45-55 wt%, and the mass of the sulfuric acid is 10-50% of that of the waste lithium iron phosphate powder;
roasting the raw material by microwave to obtain clinker;
mixing the clinker with water and then carrying out leaching treatment to obtain leaching slurry;
carrying out solid-liquid separation on the leaching slurry to obtain a lithium solution and iron phosphate slag;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
The method mixes the waste lithium iron phosphate powder with sulfuric acid to obtain the raw material. The source of the waste lithium iron phosphate powder is not specially limited, and any waste lithium iron phosphate powder needing to be treated can be used. In the invention, the waste lithium iron phosphate powder specifically refers to waste lithium iron phosphate anode powder, and the waste lithium iron phosphate anode powder is specifically obtained by discharging, disassembling and screening the waste lithium iron phosphate battery. The particle size of the waste lithium iron phosphate powder is not particularly limited, and the particle size known by the technical personnel in the field can be adopted; the content of lithium in the waste lithium iron phosphate powder is preferably 3.5-3.7 wt%.
In the invention, the concentration of the sulfuric acid is preferably 45-55 wt%, and more preferably 50 wt%; the mass of the sulfuric acid is preferably 10-50% of that of the waste lithium iron phosphate powder, and more preferably 15-25%. According to the invention, sulfuric acid can destroy the structure of lithium iron phosphate in the waste lithium iron phosphate powder, so that lithium in the lithium iron phosphate is converted into lithium salt which is easy to dissolve in a solution, and the lithium solution can be obtained after subsequent water leaching treatment and solid-liquid separation; meanwhile, the sulfuric acid can also play an oxidizing role to oxidize ferrous iron in the system into ferric iron, so that iron and phosphorus are not leached synchronously. The invention controls the dosage of the sulfuric acid within the range, ensures that lithium in the lithium iron phosphate is fully converted into lithium salt which is easy to dissolve in the solution, and simultaneously ensures that the impurity content in the lithium solution is lower; if the dosage of the sulfuric acid is too small, lithium in the lithium iron phosphate cannot be fully converted into lithium salt which is easily dissolved in the solution, and the leaching rate of the lithium is low; if the using amount of the sulfuric acid is too much, the content of iron and phosphorus in the lithium solution is high, the recovery rate of the iron and the phosphorus is reduced, meanwhile, the iron and the phosphorus in the lithium solution are not easy to remove, the treatment cost is increased, and the using amount of the sulfuric acid is too much, so that the production cost is high.
The method has no special limitation on the mixing mode of the waste lithium iron phosphate powder and the sulfuric acid, and can realize the full mixing of the waste lithium iron phosphate powder and the sulfuric acid.
After the raw material is obtained, the raw material is subjected to microwave roasting to obtain the clinker. In the invention, the temperature of the microwave roasting is preferably 400-800 ℃, and more preferably 500-700 ℃; the time is preferably 60-240 min, and more preferably 120-180 min; the microwave calcination is preferably carried out in an air atmosphere. In the present invention, the microwave firing is preferably performed in a microwave sintering furnace. In the invention, in the microwave roasting process, sulfuric acid can destroy the structure of lithium iron phosphate in the waste lithium iron phosphate powder, so that lithium in the lithium iron phosphate is converted into a lithium salt which is easily dissolved in a solution, the lithium solution can be obtained after subsequent water leaching treatment and solid-liquid separation, and the lithium-rich solution obtained through subsequent two times of countercurrent leaching has high concentration, other concentration processes are not needed, the preparation of a high-purity lithium salt product can be easily realized, and the cost is saved; the microwave roasting belongs to roasting in an internal heating mode, and has a good heat transfer effect.
After the clinker is obtained, the clinker is mixed with water and then is subjected to leaching treatment to obtain leaching slurry. In the invention, the clinker obtained by microwave roasting is preferably mixed with water for leaching treatment after being cooled. In the present invention, the mass ratio of the clinker to water is preferably 1: (2.5 to 3.5), more preferably 1: 3. in the invention, the leaching temperature is preferably 25-100 ℃, and more preferably 50-60 ℃; the time is preferably 10 to 120min, and more preferably 30 to 90 min. In the present invention, during the leaching treatment, the lithium salt is leached to a liquid phase, while iron and phosphorus exist in a solid phase in the form of iron phosphate precipitate.
After the leaching slurry is obtained, the solid-liquid separation is carried out on the leaching slurry to obtain a lithium solution and iron phosphate slag. The solid-liquid separation method is not particularly limited, and a method known to those skilled in the art can be used. In the present invention, the solid-liquid separation is preferably performed by filtration. In the present invention, it is preferable that the solid-liquid separation further comprises: and washing the obtained solid material with water to obtain the iron phosphate slag. In the present invention, the washing is preferably performed by countercurrent washing; according to the invention, lithium carried in the iron phosphate slag can be removed by washing; the washing liquid resulting from the water washing is preferably reused in the leaching treatment step.
After the lithium solution is obtained, the lithium solution is subjected to two times of countercurrent leaching to obtain a lithium-rich solution. The present invention does not specifically limit the operation of the countercurrent leaching, and the countercurrent leaching known to those skilled in the art can be used. According to the invention, through twice countercurrent leaching, the concentration of the lithium solution can be improved, and the lithium-rich solution can be obtained without evaporation and concentration, thereby being beneficial to saving the cost.
In the invention, after the treatment by the method, the obtained lithium-rich solution has low impurity content, and the invention preferably removes impurities from the lithium-rich solution to further remove a small amount of impurities; the specific operation mode of the impurity removal is not specially limited, and the impurity removal mode known by the technicians in the field can be adopted; in the invention, the waste residue obtained after impurity removal can be mixed with raw materials and then subjected to microwave roasting, and can also be mixed with iron phosphate slag and then further processed to recover phosphorus and iron.
The method for extracting lithium from waste lithium iron phosphate powder provided by the invention can be specifically carried out according to the following steps: mixing waste lithium iron phosphate powder with sulfuric acid to obtain a raw material; the concentration of the sulfuric acid is 45-55 wt%, and the mass of the sulfuric acid is 10-50% of that of the waste lithium iron phosphate powder; roasting the raw material by microwave to obtain clinker; mixing the clinker with water and then carrying out leaching treatment to obtain leaching slurry; carrying out solid-liquid separation on the leaching slurry to obtain a lithium solution and iron phosphate slag; and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution. In the invention, after the treatment by the method, lithium is preferentially leached, and the lithium-rich solution obtained by twice countercurrent leaching has high lithium concentration of 20-26 g/L and low impurity content, and the total content of iron and phosphorus can be as low as 1.53 g/L; the purity of lithium carbonate prepared by taking the lithium-rich solution as a raw material is more than 99.5 percent, and the total lithium yield is up to 97.23 percent.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing 100g of waste lithium iron phosphate positive electrode powder (the lithium content is 3.7 wt%) with 15g of sulfuric acid with the concentration of 50 wt% to obtain a raw material; placing the raw material in a microwave sintering furnace, and roasting for 120min at 500 ℃ in an air atmosphere to obtain clinker;
according to the mass ratio of clinker to water of 1: 2.5, mixing the clinker with water, and leaching for 30min at 50 ℃ to obtain leaching slurry; filtering the leaching slurry to obtain filtrate and filter residue, wherein the filtrate is a lithium solution, and the filter residue is washed by water in a countercurrent manner to obtain iron phosphate residue;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
The lithium concentration of the lithium-rich solution obtained in the embodiment is 25.3g/L, the total content of iron and phosphorus is 1.53g/L, the purity of lithium carbonate prepared by using the lithium-rich solution as a raw material is more than 99.5%, and the total yield of lithium reaches 90.08%.
Example 2
Mixing 100g of waste lithium iron phosphate anode powder (the lithium content is 3.7 wt%) with 20g of sulfuric acid with the concentration of 50 wt% to obtain a raw material; placing the raw material in a microwave sintering furnace, and roasting for 180min at 500 ℃ in an air atmosphere to obtain clinker;
according to the mass ratio of clinker to water of 1: 3, mixing the clinker with water, and leaching for 60min at 50 ℃ to obtain leaching slurry; filtering the leaching slurry to obtain filtrate and filter residue, wherein the filtrate is a lithium solution, and the filter residue is washed by water in a countercurrent manner to obtain iron phosphate residue;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
The lithium concentration of the lithium-rich solution obtained in the embodiment is 23.15g/L, the total content of iron and phosphorus is 2.13g/L, the purity of lithium carbonate prepared by using the lithium-rich solution as a raw material is more than 99.5%, and the total yield of lithium reaches 95.48%.
Example 3
Mixing 100g of waste lithium iron phosphate anode powder (the lithium content is 3.7 wt%) with 25g of sulfuric acid with the concentration of 50 wt% to obtain a raw material; placing the raw material in a microwave sintering furnace, and roasting for 180min at 600 ℃ in an air atmosphere to obtain clinker;
according to the mass ratio of clinker to water of 1: 3.5, mixing the clinker with water, and leaching for 120min at the temperature of 60 ℃ to obtain leaching slurry; filtering the leaching slurry to obtain filtrate and filter residue, wherein the filtrate is a lithium solution, and the filter residue is washed by water in a countercurrent manner to obtain iron phosphate residue;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
The lithium concentration of the lithium-rich solution obtained in the embodiment is 20.48g/L, the total content of iron and phosphorus is 2.78g/L, the purity of lithium carbonate prepared by using the lithium-rich solution as a raw material is more than 99.5%, and the total yield of lithium reaches 97.12%.
Example 4
Mixing 100g of waste lithium iron phosphate positive electrode powder (the lithium content is 3.7 wt%) with 50g of sulfuric acid with the concentration of 50 wt% to obtain a raw material; placing the raw material in a microwave sintering furnace, and roasting for 180min at 600 ℃ in an air atmosphere to obtain clinker;
according to the mass ratio of clinker to water of 1: 3, mixing the clinker with water, and leaching for 90min at 50 ℃ to obtain leaching slurry; filtering the leaching slurry to obtain filtrate and filter residue, wherein the filtrate is a lithium solution, and the filter residue is washed by water in a countercurrent manner to obtain iron phosphate residue;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
The lithium concentration of the lithium-rich solution obtained in the embodiment is 21.38g/L, the total content of iron and phosphorus is 4.78g/L, the purity of lithium carbonate prepared by using the lithium-rich solution as a raw material is more than 99.5%, and the total yield of lithium reaches 85.97%.
Example 5
Mixing 100g of waste lithium iron phosphate anode powder (the lithium content is 3.7 wt%) with 20g of sulfuric acid with the concentration of 50 wt% to obtain a raw material; placing the raw material in a microwave sintering furnace, and roasting for 150min at 700 ℃ in an air atmosphere to obtain clinker;
according to the mass ratio of clinker to water of 1: 3, mixing the clinker with water, and leaching for 120min at 50 ℃ to obtain leaching slurry; filtering the leaching slurry to obtain filtrate and filter residue, wherein the filtrate is a lithium solution, and the filter residue is washed by water in a countercurrent manner to obtain iron phosphate residue;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
The lithium concentration of the lithium-rich solution obtained in the embodiment is 24.16g/L, the total content of iron and phosphorus is 2.09g/L, the purity of lithium carbonate prepared by using the lithium-rich solution as a raw material is more than 99.5%, and the total yield of lithium reaches 97.23%.
Comparative example 1
The waste lithium iron phosphate positive electrode powder is treated according to the method of the embodiment 1, except that the amount of the sulfuric acid is 5 g.
The lithium-rich solution obtained in the comparative example had a lithium concentration of 10.57g/L, a total iron and phosphorus content of 0.1g/L, and a total lithium yield of 46.38%.
Comparative example 2
The waste lithium iron phosphate positive electrode powder was treated according to the method of example 5, except that the amount of sulfuric acid was 70 g.
The lithium concentration of the lithium solution obtained in the comparative example is 24.05g/L, the total content of iron and phosphorus is 7.76g/L, and the impurity content is higher; the overall yield of lithium was 97.52%.
Comparative example 3
The waste lithium iron phosphate positive electrode powder is treated according to the method of the embodiment 5, except that the waste lithium iron phosphate positive electrode powder is roasted in a conventional manner, specifically, in a muffle furnace.
The lithium-rich solution obtained in the comparative example had a lithium concentration of 10.87g/L, a total iron and phosphorus content of 2.18g/L, and a total lithium yield of 45.82%.
Comparative example 4
The waste lithium iron phosphate positive electrode powder is treated according to the method of the embodiment 5, except that the waste lithium iron phosphate positive electrode powder is roasted in a conventional mode, specifically, the waste lithium iron phosphate positive electrode powder is roasted in a muffle furnace, and the roasting temperature is 900 ℃.
In the comparative example, the clinker is hardened and harder, and can be leached after being crushed, the lithium concentration of the obtained lithium-rich solution is 22.45g/L, the total content of iron and phosphorus is 5.76g/L, and the total yield of lithium is 92.82%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (7)

1. A method for extracting lithium from waste lithium iron phosphate powder comprises the following steps:
mixing waste lithium iron phosphate powder with sulfuric acid to obtain a raw material; the concentration of the sulfuric acid is 45-55 wt%, and the mass of the sulfuric acid is 10-50% of that of the waste lithium iron phosphate powder;
microwave roasting the raw material in an air atmosphere to obtain clinker; the microwave roasting temperature is 400-800 ℃, and the time is 60-240 min;
mixing the clinker with water and then carrying out leaching treatment to obtain leaching slurry;
carrying out solid-liquid separation on the leaching slurry to obtain a lithium solution and iron phosphate slag;
and carrying out countercurrent leaching on the lithium solution twice to obtain a lithium-rich solution.
2. The method according to claim 1, wherein the lithium content in the waste lithium iron phosphate powder is 3.5-3.7 wt%.
3. The method according to claim 1, wherein the mass ratio of clinker to water is 1: (2.5-3.5).
4. A method according to claim 1 or 3, wherein the temperature of the leaching process is 40-60 ℃.
5. The method according to claim 4, wherein the leaching treatment time is 30-60 min.
6. The method according to claim 1, wherein the solid-liquid separation is by filtration.
7. The method according to claim 1 or 6, further comprising, after the solid-liquid separation: and washing the obtained solid material with water to obtain the iron phosphate slag.
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