CN102403554A - Method for recycling waste lithium iron phosphate ion battery anode material - Google Patents
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- CN102403554A CN102403554A CN2011103553525A CN201110355352A CN102403554A CN 102403554 A CN102403554 A CN 102403554A CN 2011103553525 A CN2011103553525 A CN 2011103553525A CN 201110355352 A CN201110355352 A CN 201110355352A CN 102403554 A CN102403554 A CN 102403554A
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a method for recycling a waste lithium iron phosphate ion battery anode material, which comprises the steps of: dissolving collected waste lithium iron phosphate ion battery anode material with hydrochloric acid, measuring contents of phosphorus, iron and lithium; adding iron or/and lithium to prepare a lithium iron phosphorus solution with a certain mass ratio; regulating the pH value to be 2-9 by using ammonia water, then adding a reducing agent therein, finally adding water to be diluted to reach 1/3 of the volume of a hydrothermal reactor; reacting at a temperature of 140-180 DEG C for 6-12h in the hydrothermal reactor, filtering, washing and drying a product to obtain lithium iron phosphate powder; carrying out X-ray diffraction (XRD) test on the lithium iron phosphate powder to be lithium iron phosphate with an olivine structure, and displaying with a scanning electron microscope (SEM) as an integral crystal structure. The invention has the beneficial effects of simple processing process, remarkable effect, capabilities of batch processing and realizing recycling of the lithium battery electrode material, reduction in cost, energy source saving and environment protection.
Description
Technical field
The present invention relates to secondary battery technology, relate in particular to the recycle of ferric phosphate anode material for lithium-ion batteries.
Background technology
Nowadays lithium battery be widely used each the row field.The lithium ion battery applications amount is ten hundreds of.According to U.S. Frost & Sullivan survey data, the lithium battery whole world supply of goods was about 1,700,000,000 6,000 ten thousand in 2007, estimated will reach 3,900,000,000 9,000 ten thousand in 2013.A large amount of lithium battery applications like this, the waste material number that its old and useless battery produces also will be surprising.At present, the waste material of these old and useless batterys great majority have only to obtain on a small quantity recycling as garbage loading embeading.Utility is run off.In the prior art, the recovery of lithium iron phosphate positive material in the waste lithium iron phosphate battery is mainly contained following method:
The patent No. is 200710129898.2 patent; The recovery method of lithium iron phosphate positive material in a kind of lithium ion battery waste material is disclosed, be with the waste lithium iron phosphate positive electrode under inert gas atmosphere, 450～600 ℃ of down bakings 2-5 hour; Mix in the ethanolic solution with gained powdered product adding soluble ferric iron salt; Drying, then under inert gas atmosphere 300～500 ℃ of following roastings 2～5 hours, reclaim and to obtain lithium iron phosphate positive material.
The patent No. is 200710076890.4 patent, discloses a kind of comprehensive recovering process of positive pole waste tablet from ferric phosphate lithium cell, is the anode material waste sheet Mechanical Crushing of collecting is fragmentated; Fragment is placed by the sintering furnace under vacuum atmosphere, inert gas and/or reducibility gas and/or the nitrogen protection, under 150～750 ℃ temperature, handle; Fragment after the processing is separated the aluminium foil body portion with mechanical separation or ultrasonic oscillation method, obtains the mixture of lithium iron phosphate positive material, conductive agent and adhesive residue thing; With the mixture of lithium iron phosphate positive material, conductive agent and adhesive residue thing, under 80～150 ℃ of temperature, toast 8-24h; With classification behind the mixture abrasive dust after the baking, the particle diameter of control powder is not more than 20 μ m, promptly gets the iron phosphate lithium positive pole reclaimed materials.
The patent No. is 20081003093 patent; A kind of recovery cobalt acid lithium battery material is disclosed; Its step is electric core Mechanical Crushing to the 1～5mm with waste lithium cell, handles under 150～600 ℃, and the powder after the processing passes through vibrosieve; The lower part of screen is divided into cobalt acid lithium and carbon powder, and sieve top is divided into copper sheet and aluminium flake.
The deficiency of above-mentioned recovery technology is: recovery LiFePO4 or other electrode material that can only machinery reach the purpose that recycles and reuses for the electrode material of inactivation.
Summary of the invention
The method that the purpose of this invention is to provide a kind of positive electrode of recycle waste lithium iron phosphate battery, the method for utilizing chemistry is with the synthetic active electrode material of lithium ion cell positive with higher capacity of the positive electrode of the LiFePO4 ion battery of inactivation.
Technical scheme of the present invention is: waste lithium iron phosphate ion battery positive electrode recycle method; Comprise and collect the anodal coating material mixture of waste lithium iron phosphate; The coating material mixture is the mixture of LiFePO4 and electric conducting material, it is characterized in that said recycle method may further comprise the steps:
A, the anodal coating material mixture of waste lithium iron phosphate is used concentration is 18～36wt% dissolving with hydrochloric acid, filters with close filter paper and removes carbon dust and collect filtrating, detects the content of phosphorus, iron and lithium that gained filtrates;
B, consider liquid at 50～80 ℃ of following evaporation-concentration step a gained; Consider liquid to gained and reach the half the of original volume; The content of phosphorus, iron and lithium that the gained that detects with step a is then filtrated is the basis; Add lithium source and/or source of iron to filtrating, make filtrating reach lithium: iron: the phosphorus mass concentration ratio is 1～3: 1: 1; Thin up is added the filtrating of lithium source and/or source of iron, makes Fe in the filtrating
2+Concentration is 0.4～1mol/L with the concentration of iron metering;
C, in solution, add reducing agent, guarantee in the follow-up water-heat process Fe in the solution through step b
2+Not oxidized, reducing agent adding method is to add at interval several times, and the reducing agent addition be each 0.001～0.01 gram that adds, and at the interval that adds reducing agent, dropper is drawn 0.5～1 milliliter of filtrating and is added dropwise to potassium rhodanate, checks the whether variable color of filtrating.To the no longer variable color of filtrating, then add last reducing agent 0.001～0.01 gram, make the excessive 0.5～2.0wt% of reducing agent;
D, with the pH value of ammoniacal liquor regulating step c gained solution, the scope that makes the pH value is 2～9;
E, the liquid that steps d is prepared are transferred in the water heating kettle, and 1/3rd of thin up to water heating kettle volume reacted 6～12 hours down at 140～180 ℃ then;
After f, the cooling product is taken out, filters, will filter gains with deionized water wash after, in drying box under 100 ℃, under vacuum or the inert gas conditions dry 4-12 hour, promptly obtain the iron phosphate powder of grey.
Waste lithium iron phosphate ion battery positive electrode recycle method according to the invention is characterized in that the said lithium source that adds is a lithium carbonate, lithium chloride, the mixing of one or more in the lithium hydroxide; The said source of iron that adds is one or both the mixing in ferrous sulfate and the frerrous chloride.
Waste lithium iron phosphate ion battery positive electrode recycle method according to the invention is characterized in that said reducing agent is a kind of in hydrazine and the ascorbic acid.
The iron phosphate powder that the inventive method obtains; Doing X-ray diffraction (XRD) test and scanning electron microscopy (SEM) observes: X-ray diffraction (XRD) test can be found out; Crystal type is the forsterite structure; Can see (011), (120), (111), (121), (131) crystal face, the XRD figure that obtains shows that assorted peak is less, possibly contain the carbon of base metal ion and doping; But do not influence crystal structure and its activity, can be good at corresponding with standard card as anode material for lithium-ion batteries; Scanning electron microscopy (SEM) is observed, and visible particles is evenly distributed, and has tangible crystal to form; Through the electrochemistry capacitance test, the iron phosphate powder that the inventive method obtains reaches peak capacity and is about 39.4mAhg
-1(without the carbon parcel) and 140mAhg
-1(carbon parcel).
The invention has the beneficial effects as follows: treatment process is simple, and effect is remarkable, can carry out batch process, can realize the recycle of electrode material of lithium battery, reduces cost energy savings, protection environment.
Description of drawings
The present invention has accompanying drawing 6 width of cloth, wherein
Fig. 1 is the lithium that makes with the inventive method: iron: phosphorus ratio is 1: 1: 1, and the pH value is the x-ray diffraction pattern of 5.3 iron phosphate powder,
Fig. 2 is the lithium that makes with the inventive method: iron: phosphorus ratio is 3: 1: 1, and the pH value is the x-ray diffraction pattern of 4.5 iron phosphate powder,
Fig. 3 is the lithium that makes with the inventive method: iron: phosphorus ratio is 1: 1: 1, and the pH value is 1000 times of ESEM pictures of 5.3 iron phosphate powder,
Fig. 4 is the lithium that makes with the inventive method: iron: phosphorus ratio is 1: 1: 1, and the pH value is 10000 times of ESEM pictures of 5.3 iron phosphate powder,
Fig. 5 is the lithium that makes with the inventive method: iron: phosphorus ratio is 3: 1: 1, and the pH value is 5000 times of ESEM pictures of 4.5 iron phosphate powder,
Fig. 6 is the lithium that makes with the inventive method: iron: phosphorus ratio is 3: 1: 1, and the pH value is 20000 times of ESEM pictures of 4.5 iron phosphate powder.
Embodiment
Below in conjunction with instance the utility model is done further explanation.
Embodiment 1
First step pre-treatment
At first the electrode material that obtains is taken by weighing 4.1519g, then it is dissolved in the 10ml concentrated hydrochloric acid, placed 2 hours.Filtration is diluted to 30ml with it, surveys the content of its lithium, iron, phosphorus, and the mensuration result of present embodiment is that the mass ratio of lithium, iron, phosphorus is 1: 1: 1, so need not add lithium source and source of iron.The above-mentioned solution of evaporation and concentration to volume is about 15ml, and using ammoniacal liquor to transfer its pH value is 5.3, called after 1# sample.Add the ascorbic acid (is benchmark with potassium rhodanate detection nondiscolouring and excessive slightly 1wt%) about 2g to it.Solution is diluted to 32ml, and being transferred to volume then is in the polytetrafluoroethylene water heating kettle of 80ml.
The second step sample is synthetic
Put into baking oven after above-mentioned water heating kettle tightened,, take out cooling 170 ℃ of reactions 8 hours down.
The sample reprocessing of the 3rd step
Pour out material and filtration under diminished pressure in the water heating kettle after the cooling, and, again the pressed powder product was put into 100 ℃ of vacuum drying chambers dry 12 hours, obtain the iron phosphate powder of field gray at last with deionized water wash pressed powder product.
Embodiment 2
First step pre-treatment
At first the electrode material that obtains is taken by weighing 4.0274g, then it is dissolved in 5ml concentrated hydrochloric acid+5ml deionized water, placed 2 hours.Filtration is diluted to 30ml with it.Survey the content of its lithium, iron, phosphorus; The mensuration result of present embodiment is the mass ratio 0.5: 1: 1.4 of lithium, iron, phosphorus;--lithium hydroxide and source of iron--frerrous chloride of then need adding the lithium source, to the mass ratio of lithium, iron, phosphorus be 3: 1: 1, the above-mentioned solution of evaporation and concentration to volume is about 15ml; Using ammoniacal liquor to transfer pH is 4.5, called after 2# sample; Add the ascorbic acid about 1.8g to it, to be as the criterion about potassium rhodanate detection nondiscolouring and excessive slightly 1wt%; Solution is diluted to 32ml, and being transferred to volume then is in the polytetrafluoroethylene water heating kettle of 80ml.
The second step sample is synthetic
Put into baking oven after above-mentioned water heating kettle tightened, 170 ℃ down reaction take out the agitated reactor cooling after 12 hours
The sample reprocessing of the 3rd step
Pour out material and filtration under diminished pressure in the water heating kettle after the cooling, and, again pressed powder product thing was put into 100 ℃ of vacuum drying chambers dry 12 hours, obtain the iron phosphate powder of field gray at last with deionized water wash pressed powder product
Embodiment 3
First step pre-treatment
At first the electrode material that obtains is taken by weighing 4.2051g, then it is dissolved in the 10ml concentrated hydrochloric acid, placed 2 hours.Filtration is diluted to 30ml with it.Survey the content of its phosphorus, iron, lithium, the mensuration result of present embodiment is that the mass ratio of lithium, iron, phosphorus is 0.5: 1: 1.4, then need add the lithium source--lithium chloride) and source of iron--ferrous sulfate, to the mass ratio of lithium, iron, phosphorus be 1: 1: 1.The above-mentioned solution of evaporation and concentration to volume is about 15ml, and using ammoniacal liquor to transfer pH is 4.5, called after 3# sample.Drip the hydrazine hydrate of about 1.5ml to it, to be as the criterion about potassium rhodanate detection nondiscolouring and excessive slightly 1wt%.Solution is diluted to 32ml, and being transferred to volume then is in the polytetrafluoroethylene water heating kettle of 80ml.
The second step sample is synthetic
Put into baking oven after above-mentioned water heating kettle tightened, 170 ℃ down reaction take out the agitated reactor cooling after 10 hours
The sample reprocessing of the 3rd step
Pour out material and filtration under diminished pressure in the water heating kettle after the cooling, and, again pressed powder product thing was put into 100 ℃ of vacuum drying chambers dry 12 hours, obtain the iron phosphate powder of field gray at last with deionized water wash pressed powder product
Embodiment gained sample is done XRD and SEM test, result such as accompanying drawing.
X-ray diffraction (XRD) test can be found out; Crystal type is the forsterite structure; Can see (011), (120), (111), (121), (131) crystal face, the XRD figure that obtains shows that assorted peak is less, possibly contain the carbon of base metal ion and doping; But do not influence crystal structure and its activity, can be good at corresponding with standard card as anode material for lithium-ion batteries; Scanning electron microscopy (SEM) is observed, and visible particles is evenly distributed, and has tangible crystal to form; Through the electrochemistry capacitance test, the iron phosphate powder that the inventive method obtains reaches peak capacity and is about 39.4mAhg
-1(without the carbon parcel) 140mAhg
-1(carbon parcel).
Claims (3)
1. waste lithium iron phosphate ion battery positive electrode recycle method; Comprise and collect the anodal coating material mixture of waste lithium iron phosphate; The coating material mixture is the mixture of LiFePO4 and electric conducting material, it is characterized in that said recycle method may further comprise the steps:
A, the anodal coating material mixture of waste lithium iron phosphate is used concentration is 18～36wt% dissolving with hydrochloric acid, filters with close filter paper and removes carbon dust and collect filtrating, detects the content of phosphorus, iron and lithium that gained filtrates;
B, consider liquid at 50～80 ℃ of following evaporation-concentration step a gained; Consider liquid to gained and reach the half the of original volume; The content of phosphorus, iron and lithium that the gained that detects with step a is then filtrated is the basis; Add lithium source and/or source of iron to filtrating, make filtrating reach lithium: iron: the phosphorus mass concentration ratio is 1～3: 1: 1; The above-mentioned gained filtrating of thin up makes Fe in this filtrating then
2+Concentration is 0.4～1mol/L, measures with concentration of iron;
C, in solution, add reducing agent, guarantee in the follow-up water-heat process Fe in the solution through step b
2+Not oxidized, reducing agent adding method is to add at interval several times, and the reducing agent addition be each 0.001～0.01 gram that adds, and at the interval that adds reducing agent, dropper is drawn 0.5～1 milliliter of filtrating and is added dropwise to potassium rhodanate, checks the whether variable color of filtrating.To the no longer variable color of filtrating, then add last reducing agent 0.001～0.01 gram, make the excessive 0.5～2.0wt% of reducing agent;
D, with the pH value of ammoniacal liquor regulating step c gained solution, the scope that makes the pH value is 2～9;
E, the liquid that steps d is prepared are transferred in the water heating kettle, and 1/3rd of thin up to water heating kettle volume reacted 6～12 hours down at 140～180 ℃ then;
After f, the cooling product is taken out, filters, will filter gains with deionized water wash after, in drying box under 100 ℃, under vacuum or the inert gas conditions dry 4-12 hour, promptly obtain the iron phosphate powder of grey.
2. waste lithium iron phosphate ion battery positive electrode recycle method according to claim 1 is characterized in that the said lithium source that adds is a lithium carbonate, lithium chloride, the mixing of one or more in the lithium hydroxide; The said source of iron that adds is one or both the mixing in ferrous sulfate and the frerrous chloride.
3. waste lithium iron phosphate ion battery positive electrode recycle method according to claim 1 is characterized in that said reducing agent is a kind of in hydrazine and the ascorbic acid.
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| CN2011103553525A CN102403554B (en) | 2011-11-10 | 2011-11-10 | Method for recycling waste lithium iron phosphate ion battery anode material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355837A (en) * | 2015-10-16 | 2016-02-24 | 广东烛光新能源科技有限公司 | Electrochemical cell and method of making same |
| CN106910889A (en) * | 2017-02-27 | 2017-06-30 | 中南大学 | A kind of method that positive active material is regenerated from waste lithium iron phosphate battery |
| CN107181015A (en) * | 2017-07-06 | 2017-09-19 | 湖南天泰天润新能源科技有限公司 | The reclaiming processing method of LiFePO4 waste material |
| CN109075407A (en) * | 2016-05-20 | 2018-12-21 | 魁北克电力公司 | The method for recycling electrode material of lithium battery |
| CN113023703A (en) * | 2021-03-24 | 2021-06-25 | 郑州中科新兴产业技术研究院 | Method for recycling waste lithium iron phosphate powder |
| CN114737060A (en) * | 2022-05-02 | 2022-07-12 | 叶英凤 | Method for recycling anode material of waste lithium battery |
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| WO2011079409A1 (en) * | 2009-12-28 | 2011-07-07 | 深圳市雄韬电源科技股份有限公司 | Method of recycling and reusing spent lithium iron phosphate power battery |
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| EP1148571B1 (en) * | 2000-04-17 | 2009-10-21 | Revatech S.A. | Method for recycling and treating of salt and alkaline batteries |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105355837A (en) * | 2015-10-16 | 2016-02-24 | 广东烛光新能源科技有限公司 | Electrochemical cell and method of making same |
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| CN109075407A (en) * | 2016-05-20 | 2018-12-21 | 魁北克电力公司 | The method for recycling electrode material of lithium battery |
| CN109075407B (en) * | 2016-05-20 | 2021-12-28 | 魁北克电力公司 | Method for recycling electrode material of lithium battery |
| CN106910889A (en) * | 2017-02-27 | 2017-06-30 | 中南大学 | A kind of method that positive active material is regenerated from waste lithium iron phosphate battery |
| CN106910889B (en) * | 2017-02-27 | 2019-07-23 | 中南大学 | A method of regenerating positive active material from waste lithium iron phosphate battery |
| CN107181015A (en) * | 2017-07-06 | 2017-09-19 | 湖南天泰天润新能源科技有限公司 | The reclaiming processing method of LiFePO4 waste material |
| CN107181015B (en) * | 2017-07-06 | 2019-05-10 | 湖南天泰天润新能源科技有限公司 | The reclaiming processing method of LiFePO4 waste material |
| CN113023703A (en) * | 2021-03-24 | 2021-06-25 | 郑州中科新兴产业技术研究院 | Method for recycling waste lithium iron phosphate powder |
| CN114737060A (en) * | 2022-05-02 | 2022-07-12 | 叶英凤 | Method for recycling anode material of waste lithium battery |
| CN114737060B (en) * | 2022-05-02 | 2024-01-12 | 湖南金瑞新能源科技有限公司 | Recycling method of waste lithium battery anode material |
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