CN106997973A - The phosphatic method of ferric phosphate and lithium is prepared in a kind of anode material from waste lithium iron phosphate - Google Patents
The phosphatic method of ferric phosphate and lithium is prepared in a kind of anode material from waste lithium iron phosphate Download PDFInfo
- Publication number
- CN106997973A CN106997973A CN201710333115.6A CN201710333115A CN106997973A CN 106997973 A CN106997973 A CN 106997973A CN 201710333115 A CN201710333115 A CN 201710333115A CN 106997973 A CN106997973 A CN 106997973A
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- Prior art keywords
- lithium
- phosphate
- anode material
- iron
- filtrate
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Classifications
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a kind of phosphatic method that ferric phosphate and lithium are prepared in anode material from waste lithium iron phosphate.Comprise the following steps:Waste lithium iron phosphate anode material is aoxidized, obtain containing lithium, iron, phosphorus mixture A;A is added in the phosphoric acid solution B of stirring, reacts, obtains the phosphatic solidliquid mixture C of ferric phosphate and lithium;C is filtered, washed, filtrate D and filter cake E is obtained respectively, by filter cake E drying, acquisition high-purity phosphoric acid iron is crushed;Filtrate D is cooled down, filters, wash, filter cake F drying, the crushing of acquisition the phosphate of lithium is obtained into, filtrate H is recycled.Product has granularity controllable made from the inventive method, purity is high, better crystallinity degree the advantages of, available for the raw material for making LiFePO4.Meanwhile, whole flow process of the present invention is closed cycle, and purification technique is simple, and cost is low.
Description
Technical field
The invention belongs to the recovery of waste lithium ion cell anode material, technical field of regeneration, and in particular to one kind from useless
The phosphatic method of ferric phosphate and lithium is prepared in old iron phosphate lithium positive pole material.
Background technology
With greatly developing for new-energy automobile, lithium ion battery is widely used in electric automobile and hybrid vehicle
On.And lithium ion battery after the use of 3 ~ 5 years, is having different degrees of scrap.According to incompletely statistics, 2015 it is waste and old
Ferrous phosphate lithium battery reaches more than 20,000 tons, it is contemplated that the waste and old ferrous phosphate lithium battery of the year two thousand twenty is up to more than 150,000 tons.Together
Sample, in lithium ion battery material and its battery manufacturing process, also due to technology is immature, technique is unstable etc., factor is caused
Lithium ion battery material and pole piece are scrapped.Ferric phosphate lithium cell is so that its safe, cycle performance is excellent, energy density is high etc.
Advantage is widely used on new-energy automobile.So, substantial amounts of waste lithium iron phosphate anode material can be produced, if not in time
Processing, causes the wasting of resources, environmental pollution.
Method is to junked-auto dynamic lithium battery disclosed in Publication No. CN102956936A Chinese invention patent application
In iron phosphate lithium positive pole material material handled, pass through roasting, acid(Hydrochloric acid, sulfuric acid, nitric acid or perchloric acid)Leaching, alkali leaching, with hydrogen
The form of oxide recycles valuable metal, meanwhile, soluble lithium salt solution is added in filtrate(Lithium sulfate, lithium nitrate or
Lithium chloride)Prepare lithium phosphate.The method not only introduces SO4 2-、Cl-、NO3 -Deng foreign ion, and complex process, long flow path, cost
It is high.
Method is to the phosphorus in ferric phosphate lithium cell disclosed in Publication No. CN104953200A Chinese invention patent application
Sour iron lithium anode material is reclaimed, and by heat treatment, hydrochloric acid or sulfuric acid dissolution, is added surfactant and alkali lye, is prepared phosphorus
Sour iron;Sodium carbonate, which is added, after filtrate concentration, heating prepares lithium carbonate.The method is carrying out dissolving phosphoric acid iron lithium just using hydrochloric acid or sulfuric acid
Pole material, introduces impurity SO4 2-Or Cl-, complicated purification process technique is needed to the ferric phosphate for obtaining high-purity, filtrate is entered
Row concentration, heating, power consumption are high.
Method is to waste lithium iron phosphate positive plate disclosed in Publication No. CN106549195A Chinese invention patent application
Reclaim ferric phosphate presoma.Iron phosphate lithium positive pole piece is calcined first, screening separating active substances and collector add hydrochloric acid,
Dissolving, filtering adds lithium hydroxide regulation pH into filtrate, and filtering is washed and dry cake, obtains ferric phosphate.The invention makes
Hydrochloric acid equally introduces impurity Cl-。
Doucheng Bian of HeFei University of Technology et al. directly add using the lithium iron phosphate positive material of recovery as raw material
Enter phosphoric acid, pass through reaction, dissolving, filtering insoluble matter(Carbon coating layer, bonding agent, conductive agent etc.), it is then refluxed for, evaporates, filtering,
Distilled water and absolute ethyl alcohol washing filter cake obtain phosphate dihydrate iron.Filtrate is evaporated at 100 DEG C, anhydrous second is then added
Alcohol, filtering, washing obtains lithium dihydrogen phosphate.The technique without first remove reclaim lithium iron phosphate positive material in bonding agent,
The impurity such as conductive agent, carbon coating layer, during acidleach, these impurity particularly carbon coating layer can seriously hinder H+With Li,
Fe, P contact, cause reaction rate slow, leaching rate is low, and product purity is low.And technique power consumption is high, long flow path.
In view of the shortcomings of the prior art, the present invention uses waste lithium iron phosphate anode material for raw material, first passes through oxidation removal
Its impurity contained(Conductive agent, binding agent, carbon coating layer etc.), obtain containing lithium, iron, phosphorus mixture, then using phosphoric acid as reaction
Agent, directly obtains the phosphate of ferric phosphate and lithium, and whole technological process does not introduce other impurities ion, realizes closed cycle, only
Chemical industry skill is simple, and product granularity is controllable, and purity is high, better crystallinity degree.
The content of the invention
The present invention is using waste lithium iron phosphate anode material as raw material, the impurity that it contains by oxidation removal(Conductive agent, bonding
Agent, carbon coating layer etc.), obtain containing lithium, iron, phosphorus mixture, especially propose using phosphoric acid as reactant, other do not introduced miscellaneous
Matter ion, the phosphate of ferric phosphate and lithium is prepared using wet chemistry method, and filtrate cycle is utilized.Using the method prepare ferric phosphate and
The phosphate granularity of lithium is controllable, and purity is high, better crystallinity degree.
The technical scheme of use:
1)Waste lithium iron phosphate anode material is aoxidized, obtain containing lithium, iron, phosphorus mixture A;
2)A is added in the phosphoric acid solution B of stirring, reacted, the phosphatic solidliquid mixture C of ferric phosphate and lithium is obtained, point
Not Huo get filtrate D and filter cake E, filter cake E is washed to neutrality, drying, crushes and obtains high-purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Wherein, described waste lithium iron phosphate anode material derives from the ferric phosphate lithium cell scrapped, waste lithium iron phosphate pole
One or more of combinations in piece, LiFePO4 defect ware.
Wherein, described oxidizing temperature is 400 ~ 800 DEG C.
Wherein, described reaction temperature is 60 ~ 150 DEG C, and the reaction time is 4 ~ 20h.
Wherein, described phosphoric acid solution B concentration is 0.05 ~ 3mol/L.
The phosphatic method that the present invention prepares ferric phosphate and lithium using waste lithium iron phosphate anode material and phosphoric acid solution is imitated
It is really:Other impurities ion is not introduced during preparation, the product purity of preparation is high, and better crystallinity degree, granularity are controllable, is to use
In the main material of manufacture lithium-ion battery lithium iron phosphate anode material, recycling for resource is realized, and whole technological process is real
Existing closed cycle, purification technique is simple, and cost is low.
Brief description of the drawings
Fig. 1 is the technique stream for the phosphatic method that the present invention prepares ferric phosphate and lithium from waste lithium iron phosphate anode material
Cheng Tu.
Embodiment:
Embodiment 1
1)The ferric phosphate lithium cell scrapped is disassembled, waste lithium iron phosphate anode material is obtained, it is aoxidized at 400 DEG C,
Obtain containing lithium, iron, phosphorus mixture A;
2)By A be added to concentration be 0.05mol/L stirring phosphoric acid solution B in, at 60 DEG C react 20h obtain ferric phosphate and
The phosphatic solidliquid mixture C of lithium, obtains filtrate D and filter cake E respectively, filter cake E is washed to neutrality, drying, crushing are obtained
High-purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Embodiment 2
1)Waste and old LiFePO4 pole piece is crushed, separation, obtain waste lithium iron phosphate anode material and aoxidized at 800 DEG C, obtained
Containing lithium, iron, phosphorus mixture A;
2)In the phosphoric acid solution B that A is added to the stirring that concentration is 3mol/L, at 60 DEG C reacting 4h obtains ferric phosphate and lithium
Phosphatic solidliquid mixture C, obtains filtrate D and filter cake E respectively, filter cake E is washed to neutrality, drying, crushing obtain high-purity
Spend ferric phosphate;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Embodiment 3
1)LiFePO4 defect ware is aoxidized at 650 DEG C, obtain containing lithium, iron, phosphorus mixture A;
2)By A be added to concentration be 1.5mol/L stirring phosphoric acid solution B in, at 150 DEG C react 10h obtain ferric phosphate and
The phosphatic solidliquid mixture C of lithium, obtains filtrate D and filter cake E respectively, filter cake E is washed to neutrality, drying, crushing are obtained
High-purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Embodiment 4
1)The ferric phosphate lithium cell scrapped is disassembled, waste lithium iron phosphate anode material is obtained, it is aoxidized at 600 DEG C,
Obtain containing lithium, iron, phosphorus mixture A;
2)In the phosphoric acid solution B that A is added to the stirring that concentration is 1mol/L, 15h acquisition ferric phosphates and lithium are reacted at 90 DEG C
Phosphatic solidliquid mixture C, filtrate D and filter cake E is obtained respectively, filter cake E is washed to neutrality, drying, crushes and obtains high
Purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Embodiment 5
1)Waste and old LiFePO4 pole piece is crushed, separation, obtain waste lithium iron phosphate anode material and aoxidized at 550 DEG C, obtained
Containing lithium, iron, phosphorus mixture A;
2)In the phosphoric acid solution B that A is added to the stirring that concentration is 2mol/L, 8h acquisition ferric phosphates and lithium are reacted at 105 DEG C
Phosphatic solidliquid mixture C, filtrate D and filter cake E is obtained respectively, filter cake E is washed to neutrality, drying, crushes and obtains high
Purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Embodiment 6
1)The ferric phosphate lithium cell scrapped is disassembled, waste lithium iron phosphate anode material is obtained, it is aoxidized at 700 DEG C,
Obtain containing lithium, iron, phosphorus mixture A;
2)By A be added to concentration be 2.5mol/L stirring phosphoric acid solution B in, at 130 DEG C react 13h obtain ferric phosphate and
The phosphatic solidliquid mixture C of lithium, obtains filtrate D and filter cake E respectively, filter cake E is washed to neutrality, drying, crushing are obtained
High-purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
Claims (5)
1. preparing the phosphatic method of ferric phosphate and lithium in a kind of anode material from waste lithium iron phosphate, this method step is as follows:
1)Waste lithium iron phosphate anode material is aoxidized, obtain containing lithium, iron, phosphorus mixture A;
2)A is added in the phosphoric acid solution B of stirring, reacted, the phosphatic solidliquid mixture C of ferric phosphate and lithium, mistake is obtained
Filter, washing, obtain filtrate D and filter cake E respectively, filter cake E are washed to neutrality, drying, crushing obtain high-purity phosphoric acid iron;
3)Filtrate D is cooled down, filters, wash, by phosphate of the filter cake F drying of acquisition for lithium, filtrate H is recycled.
2. the phosphatic method of ferric phosphate and lithium is prepared in the anode material according to claim 1 from waste lithium iron phosphate,
It is characterized in that:Step 1)Described in waste lithium iron phosphate anode material derive from ferric phosphate lithium cell, the waste and old phosphoric acid scrapped
One or more of combinations in iron pole piece, LiFePO4 defect ware.
3. the phosphatic method of ferric phosphate and lithium is prepared in the anode material according to claim 1 from waste lithium iron phosphate,
It is characterized in that:Step 1)Described in oxidizing temperature be 400 ~ 800 DEG C.
4. the phosphatic method of ferric phosphate and lithium is prepared in the anode material according to claim 1 from waste lithium iron phosphate,
It is characterized in that:Step 2)Described in phosphoric acid solution B concentration be 0.05 ~ 3mol/L.
5. the phosphatic method of ferric phosphate and lithium is prepared in the anode material according to claim 1 from waste lithium iron phosphate,
It is characterized in that:Step 2)Described in reaction temperature be 60 ~ 150 DEG C, the reaction time be 4 ~ 20h.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107352524A (en) * | 2017-08-03 | 2017-11-17 | 清华大学 | A kind of recovery method of waste lithium iron phosphate positive electrode |
CN108218690A (en) * | 2018-01-20 | 2018-06-29 | 湖南省正源储能材料与器件研究所 | A kind of method that waste lithium iron phosphate anode material prepares the oxalates of lithium |
CN109193059A (en) * | 2018-09-26 | 2019-01-11 | 王书珍 | A kind of regeneration treating method of LiFePO4 waste material |
CN109775678A (en) * | 2019-04-01 | 2019-05-21 | 中钢集团南京新材料研究院有限公司 | The method that battery-grade iron phosphate and PHOSPHORIC ACID TECH.GRADE lithium are prepared in waste lithium iron phosphate battery |
CN109818100A (en) * | 2019-03-25 | 2019-05-28 | 南京工程学院 | A kind of modified LiFePO4 anode waste reuse method of reparation |
CN112938921A (en) * | 2021-04-07 | 2021-06-11 | 贵州唯特高新能源科技有限公司 | Method for preparing iron phosphate |
CN113415793A (en) * | 2021-05-10 | 2021-09-21 | 北京科技大学 | Method for preparing high-purity iron phosphate from lithium iron phosphate battery waste |
CN115504446A (en) * | 2022-09-22 | 2022-12-23 | 河南鑫再生新材料科技有限公司 | Method for green recovery of lithium iron phosphate cathode material |
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CN102903985A (en) * | 2012-10-22 | 2013-01-30 | 四川天齐锂业股份有限公司 | Method for recycling lithium carbonate from lithium iron phosphate waste material |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107352524A (en) * | 2017-08-03 | 2017-11-17 | 清华大学 | A kind of recovery method of waste lithium iron phosphate positive electrode |
CN108218690A (en) * | 2018-01-20 | 2018-06-29 | 湖南省正源储能材料与器件研究所 | A kind of method that waste lithium iron phosphate anode material prepares the oxalates of lithium |
CN109193059A (en) * | 2018-09-26 | 2019-01-11 | 王书珍 | A kind of regeneration treating method of LiFePO4 waste material |
CN109818100A (en) * | 2019-03-25 | 2019-05-28 | 南京工程学院 | A kind of modified LiFePO4 anode waste reuse method of reparation |
CN109818100B (en) * | 2019-03-25 | 2021-08-10 | 南京工程学院 | Recycling method for repairing and modifying LiFePO4 anode waste |
CN109775678A (en) * | 2019-04-01 | 2019-05-21 | 中钢集团南京新材料研究院有限公司 | The method that battery-grade iron phosphate and PHOSPHORIC ACID TECH.GRADE lithium are prepared in waste lithium iron phosphate battery |
CN109775678B (en) * | 2019-04-01 | 2022-05-10 | 中钢集团南京新材料研究院有限公司 | Method for preparing battery-grade iron phosphate and industrial-grade lithium phosphate from waste lithium iron phosphate batteries |
CN112938921A (en) * | 2021-04-07 | 2021-06-11 | 贵州唯特高新能源科技有限公司 | Method for preparing iron phosphate |
CN113415793A (en) * | 2021-05-10 | 2021-09-21 | 北京科技大学 | Method for preparing high-purity iron phosphate from lithium iron phosphate battery waste |
CN115504446A (en) * | 2022-09-22 | 2022-12-23 | 河南鑫再生新材料科技有限公司 | Method for green recovery of lithium iron phosphate cathode material |
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Application publication date: 20170801 |