CN110331288A - A kind of method that waste lithium iron phosphate material selectivity mentions lithium - Google Patents
A kind of method that waste lithium iron phosphate material selectivity mentions lithium Download PDFInfo
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- CN110331288A CN110331288A CN201910571967.8A CN201910571967A CN110331288A CN 110331288 A CN110331288 A CN 110331288A CN 201910571967 A CN201910571967 A CN 201910571967A CN 110331288 A CN110331288 A CN 110331288A
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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
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- 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
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a kind of methods that waste lithium iron phosphate material selectivity mentions lithium, the following steps are included: waste lithium iron phosphate material is immersed in sodium hydroxide solution, carry out alkali leaching aluminium, filtering, expect to be dried after removing aluminium to what is be obtained by filtration, the sodium aluminate filtrate recycling that obtains LiFePO4 powder, and will filter out；LiFePO4 powder is put into heating furnace, selectivity is passed through and mentions lithium gas, then roasted, obtain the compound of ferric phosphate and lithium；Ball mill is added in the compound of ferric phosphate and lithium, carries out wet ball grinding, filtering respectively obtains ferric phosphate solid and lithium-containing solution；The pH value of lithium-containing solution is adjusted to 9.0-11.0, cleans, obtains pure lithium solution；Sodium carbonate liquor is added in pure lithium solution and is reacted, filtered, the solid being obtained by filtration is washed, is dried, lithium carbonate is obtained.With the lithium in method recycling waste lithium iron phosphate material of the invention, the lithium rate of recovery is up to 95% or more.
Description
Technical field
The invention belongs to the technical field of comprehensive utilization of lithium ion battery electrode material, and in particular to a kind of waste and old ferric phosphate
The method that lithium material selectively mentions lithium.
Background technique
LiFePO4 is a kind of most lithium ion battery material of current usage amount, is regarded as not by many row insiders
Carry out the developing direction of lithium battery.Since 21 century, with the eruptive growth in lithium electricity new energy market, waste lithium iron phosphate battery
Processing problem it is increasingly prominent.
Most LiFePO is reported at present4Waste material treatment process is mainly from waste recoveries such as cobalt acid lithium, nickle cobalt lithium manganates
It is used for reference in technique.Patent of invention CN104953200A (recycles battery-grade iron phosphate and utilizes waste and old in ferric phosphate lithium cell
The method that ferric phosphate lithium cell prepares lithium iron phosphate positive material) by LiFePO4 waste material using heat treatment-acidleach-sink phosphoric acid
Iron-sinks lithium carbonate-LiFePO4 synthesis technology, LiFePO4 waste material is re-prepared as LiFePO 4 material, but in the technique
Because of material composition complexity, a large amount of impurity (such as aluminium) will be mingled in ferric phosphate, so that the LiFePO 4 material performance of synthesis is by shadow
It rings, and the lithium rate of recovery of this method recycling lithium carbonate is difficult to ensure.Patent of invention CN106450547A is (a kind of useless from LiFePO4
The method of ferric phosphate and lithium carbonate is recycled in material) oxidizing roasting-phosphoric acid leaching-solid-liquor separation-precipitating lithium carbonate technique is used, it is real
Existing lithium and ferrophosphorus efficiently separate, and effect is preferable, but technique is cumbersome.
Therefore, it needs to develop that a kind of simple process, production cost is low, low energy consumption, economic benefit is obvious, may advantageously facilitate phosphorus
The method that the waste lithium iron phosphate material selectivity of the recycling development of sour lithium iron battery mentions lithium.
Summary of the invention
The purpose of the present invention is to provide a kind of method that waste lithium iron phosphate material selectivity mentions lithium, simple process,
Production cost is low, low energy consumption, economic benefit is obvious, may advantageously facilitate the recycling development of ferric phosphate lithium cell.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of method that waste lithium iron phosphate material selectivity mentions lithium, comprising the following steps:
(1) waste lithium iron phosphate material is immersed in sodium hydroxide solution, carries out alkali leaching aluminium, filtering, to being obtained by filtration
Except expect to be dried after aluminium, the sodium aluminate filtrate that obtains LiFePO4 powder, and will filter out is recycled；
(2) LiFePO4 powder is put into heating furnace, is passed through selectivity and mentions lithium gas, then roasted, obtains ferric phosphate
With the compound of lithium；
(3) ball mill is added in the compound of ferric phosphate and lithium, carries out wet ball grinding, it is solid to respectively obtain ferric phosphate for filtering
Body and lithium-containing solution；
(4) pH value of lithium-containing solution is adjusted to 9.0-11.0, cleans, obtains pure lithium solution；
(5) sodium carbonate liquor is added in pure lithium solution and is reacted, filtered, the solid being obtained by filtration is washed,
It is dry, obtain lithium carbonate.
Preferably, in step (1), the waste lithium iron phosphate material generates in ferric phosphate lithium cell production process
Discarded LiFePO 4 material and ferric phosphate lithium cell dismantling obtain waste lithium iron phosphate material.
Preferably, in step (1), the addition mole of the sodium hydroxide is aluminium mole in waste lithium iron phosphate material
1.2-1.5 times.
Preferably, in step (1), the mass ratio of the sodium hydroxide solution and waste lithium iron phosphate material is 3-5:1.
Preferably, in step (1), the alkali leaching aluminium carries out at 90 DEG C -95 DEG C, time 2-3h.
Preferably, in step (2), the roasting carries out at 200 DEG C -1000 DEG C, time 1-6h.
Preferably, in step (2), the selectivity mentions lithium gas and is selected from chlorine, sulfur dioxide, sulfur trioxide, titanium dioxide
One or more of chlorine, chlorine monoxide, chlorine peroxide and oxygen.
Preferably, in step (3), the time of the wet ball grinding is 0.5-2 hours, and the liquid-solid ratio of wet ball grinding slurry is
2-3:1, fineness >=100 mesh of wet ball grinding material.
Preferably, in step (4), the substance that the pH of lithium-containing solution is adjusted to 9.0-11.0 addition is sodium carbonate.
Preferably, in step (5), the time of the reaction is 2-3h.
LiFePO4 decomposes, and being converted into the compound of ferric phosphate and lithium, the reaction mechanism is as follows:
2LiFePO4+SO2+O2=Li2SO4+2FePO4
2LiFePO4+Cl2=2LiCl+2FePO4
I.e. under the high temperature conditions, the acidification oxidation for realizing LiFePO4, generate the soluble lithium salts such as lithium sulfate/lithium chloride and
Phosphoric acid scum realizes the Selectively leaching of lithium after water logging.
Preferably, that selection is SO2The atmosphere of+oxygen/air.
The method have the benefit that:
Method and process of the invention is simple, at low cost, low energy consumption, and the selection of lithium in waste lithium iron phosphate material may be implemented
Property extract, leaching rate >=97.75% of lithium, the leaching rate < 0.2% of iron, the lithium rate of recovery can achieve 95% or more, product valence
Value is high, has considerable economic benefit, may advantageously facilitate the recycling of ferric phosphate lithium cell.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, below by embodiment, to the present invention into
Row is further described.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
In limiting the scope of the invention.
Embodiment 1
A kind of method that waste lithium iron phosphate material selectivity mentions lithium, comprising the following steps:
(1) alkali leaching aluminium
Take the hydrogen of waste lithium iron phosphate material 1000g (LiFePO4 content 89.32%, aluminium content 2.34%) and 3000ml
Sodium hydroxide solution (0.380mol/L) is mixed, and is heated to 90 DEG C, reacts 2h, carries out alkali leaching aluminium, and filtering is obtained except after aluminium
Material will expect to obtain LiFePO4 powder 976.9g after drying after removing aluminium；
(2) roasting conversion
LiFePO4 powder 800g is put into heating furnace, under the conditions of 700 DEG C, is passed through sulfur dioxide and oxygen mixture
Body roasts 3h, and LiFePO4 decomposes, and is converted into the compound 983.8g of ferric phosphate and lithium；
(3) ball milling water logging
By the compound 500g of ferric phosphate and lithium, water 1000ml is added in ball mill and carries out wet ball grinding, after filtering
To ferric phosphate solid and lithium-containing solution 1000ml, lithium content 16.10g/L, iron content 0.21g/L；Calculate to obtain lithium leaching
Rate 97.75%, the leaching rate of iron are 0.16%；
(4) lithium liquid cleans
The lithium-containing solution 500ml that step (3) is obtained is added sodium carbonate liquor and adjusts pH to 10.5, removes therein miscellaneous
Pure lithium solution is obtained by filtration in matter；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 200ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
Embodiment 2
A kind of method that waste lithium iron phosphate material selectivity mentions lithium, comprising the following steps:
(1) alkali leaching aluminium
Take the hydrogen of waste lithium iron phosphate material 1000g (LiFePO4 content 89.32%, aluminium content 2.34%) and 3000ml
Sodium hydroxide solution (0.380mol/L) is mixed, and is heated to 90 DEG C, reacts 2h, carries out alkali leaching aluminium, is obtained by filtration except after aluminium
Material, except after aluminium material drying after obtain LiFePO4 powder 976.9g；
(2) roasting conversion
LiFePO4 powder 800g is put into heating furnace, under the conditions of 500 DEG C, chlorine gas is passed through, in selective atmosphere
Under, 3h is roasted, LiFePO4 is decomposed, the compound 929.1g of ferric phosphate and lithium is converted into；
(3) ball milling water logging
By the material 500g after roasting conversion, water 1500ml is added in ball mill and carries out wet ball grinding, obtains after filtering
Ferric phosphate solid and lithium-containing solution 1500ml, lithium content 10.85g/L, iron content 0.15；Calculate to obtain lithium leaching rate
98.82%, the leaching rate of iron is 0.17%.
(4) lithium liquid cleans
The lithium-containing solution 500ml that step (3) is obtained is added sodium carbonate liquor and adjusts pH value to 10.2, removes therein
Pure lithium solution is obtained by filtration in impurity；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 150ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
Embodiment 3
A kind of method that waste lithium iron phosphate material selectivity mentions lithium, comprising the following steps:
(1) alkali leaching aluminium
Take waste lithium iron phosphate material 1000g's (LiFePO4 content 87.68%, aluminium content 5.30%) and 3500ml
Sodium hydroxide solution (0.750mol/L) is mixed, and is heated to 90 DEG C, reacts 2h, is obtained by filtration except expecting after aluminium, except expecting after aluminium
LiFePO4 powder 945.6g is obtained after drying；
(2) roasting conversion
LiFePO4 powder 800g is put into heating furnace, under the conditions of 600 DEG C, sulfur trioxide gas is passed through, roasts 4h, it will
LiFePO4 decomposes, and is converted into the compound 992.3g of ferric phosphate and lithium；
(3) ball milling water logging
By the material 500g after roasting conversion, water 1000ml is added in ball mill and carries out wet ball grinding, obtains after filtering
Ferric phosphate solid and lithium-containing solution 1000ml, lithium content 16.4g/L, iron content 0.03g/L；Calculate to obtain lithium leaching rate
99.58%, the leaching rate of iron is 0.02%.
(4) lithium liquid cleans
The lithium-containing solution 500ml that step (3) is obtained is added sodium carbonate liquor and adjusts pH value to 10.8, removes therein
Pure lithium solution is obtained by filtration in impurity；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 200ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of method that waste lithium iron phosphate material selectivity mentions lithium, which comprises the following steps:
(1) waste lithium iron phosphate material is immersed in sodium hydroxide solution, carries out alkali leaching aluminium, filtering is removed to what is be obtained by filtration
Material is dried after aluminium, obtains LiFePO4 powder, and the sodium aluminate filtrate recycling that will filter out；
(2) LiFePO4 powder is put into heating furnace, is passed through selectivity and mentions lithium gas, then is roasted, LiFePO4, which decomposes, to be turned
Change obtains the compound of ferric phosphate and lithium；
(3) by the compound of ferric phosphate and lithium be added ball mill, carry out wet ball grinding, filtering, respectively obtain ferric phosphate solid and
Lithium-containing solution；
(4) pH of lithium-containing solution is adjusted to 9.0-11.0, cleans, obtains pure lithium solution；
(5) sodium carbonate liquor is added in pure lithium solution and is reacted, filtered, the solid being obtained by filtration is washed, is dried,
Obtain lithium carbonate.
2. the method that waste lithium iron phosphate material selectivity according to claim 1 mentions lithium, which is characterized in that step (1)
In, the additive amount of the sodium hydroxide is 1.2-1.5 times of aluminium mole in waste lithium iron phosphate material.
3. the method that waste lithium iron phosphate material selectivity according to claim 1 or 2 mentions lithium, which is characterized in that step
(1) in, the mass ratio of the sodium hydroxide solution and waste lithium iron phosphate material is 3-5:1.
4. the method that waste lithium iron phosphate material selectivity according to claim 1 or 2 mentions lithium, which is characterized in that step
(1) in, the alkali leaching aluminium carries out at 90 DEG C -95 DEG C, time 2-3h.
5. the method that waste lithium iron phosphate material selectivity according to claim 1 mentions lithium, which is characterized in that step (2)
In, the roasting carries out at 200 DEG C -1000 DEG C, time 1-6h.
6. the method that waste lithium iron phosphate material selectivity mentions lithium according to claim 1 or 5, which is characterized in that step
(2) in, the selectivity mentions lithium gas and is selected from chlorine, sulfur dioxide, sulfur trioxide, chlorine dioxide, chlorine monoxide, chlorine peroxide
One or more of with oxygen.
7. the method that waste lithium iron phosphate material selectivity according to claim 1 mentions lithium, which is characterized in that step (3)
In, time of the wet ball grinding is 0.5-2 hour, and the liquid-solid ratio of wet ball grinding slurry is 2-3:1, wet ball grinding material it is thin
Spend >=100 mesh.
8. the method that waste lithium iron phosphate material selectivity according to claim 1 mentions lithium, which is characterized in that step (5)
In, the substance that the pH of lithium-containing solution is adjusted to 9.0-11.0 addition is sodium carbonate.
9. the method that waste lithium iron phosphate material selectivity according to claim 1 mentions lithium, which is characterized in that step (5)
In, the time of the reaction is 2-3h.
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Cited By (12)
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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 |
| 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 |
| CN112142077A (en) * | 2020-09-08 | 2020-12-29 | 北京科技大学 | Method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste |
| CN112410556A (en) * | 2020-09-25 | 2021-02-26 | 湖北金泉新材料有限公司 | Method for recovering waste lithium iron phosphate powder |
| CN113061723A (en) * | 2021-03-04 | 2021-07-02 | 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 |
| 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 |
| 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 |
| WO2022142583A1 (en) * | 2020-12-28 | 2022-07-07 | 湖南邦普循环科技有限公司 | Method for recycling lithium iron phosphate waste and use thereof |
| CN115140722A (en) * | 2022-06-10 | 2022-10-04 | 广东邦普循环科技有限公司 | Method for preparing anode 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 |
| CN116553510A (en) * | 2023-05-11 | 2023-08-08 | 江苏大学 | Recycling and regenerating method of lithium iron phosphate waste powder |
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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 |
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| CN112142077A (en) * | 2020-09-08 | 2020-12-29 | 北京科技大学 | Method for preparing battery-grade lithium carbonate and iron phosphate by recycling lithium iron phosphate positive electrode waste |
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| 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 |
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| CN113061723A (en) * | 2021-03-04 | 2021-07-02 | 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 |
| 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 |
| WO2023010973A1 (en) * | 2021-08-03 | 2023-02-09 | 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 |
| 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 |
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| 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 |
| CN115140722A (en) * | 2022-06-10 | 2022-10-04 | 广东邦普循环科技有限公司 | Method for preparing anode material by using waste vanadyl phosphate lithium battery |
| 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 |
| CN116553510A (en) * | 2023-05-11 | 2023-08-08 | 江苏大学 | Recycling and regenerating method of lithium iron phosphate waste powder |
| 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 |
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