CN104810566B - A kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method - Google Patents
A kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method Download PDFInfo
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
Comprise the following steps the invention discloses a kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method：1）Old and useless battery is discharged, and cutting is soaked in solvent after disassembling, and the aluminum plastic film and lug after immersion are directly reclaimed；2）Battery core after immersion is separated, and obtains positive plate, negative plate and barrier film, and its septation is directly reclaimed；3）Respectively by positive plate and negative plate mechanical crushing, soaking and stirring in sig water, washing and filtering, resulting material vacuum drying are placed in；4）Dried positive pole material, negative pole mechanical mass are stirred respectively, then sieved, aluminium foil, positive very coarse powder material and copper foil, negative pole coarse powder material are obtained, the aluminium foil after separation and copper foil are reclaimed, positive very coarse powder material, negative pole coarse powder material are subjected to ball milling, screening respectively；5）Positive mix after screening and negative pole powder are heat-treated, reclaimed afterwards.The recovery method technique of the present invention is simple, and recovery powder is pure, saves energy consumption, does not cause environmental pollution.
Description
Technical field
The invention belongs to processing technology field of recycling used batteries, more particularly to a kind of waste lithium iron phosphate electrokinetic cell is green
Color recovery and treatment method.
Background technology
The existing waste and old lithium ion battery recovery technology of current China is although more, but these equipment and technique are only applicable to
Digital lithium ion battery containing rare precious metals such as Co（LiCoO2Type, ternary form), i.e., first by the molten formation Co of positive electrode acid2+、
Li+Deng, then with extraction, chemical precipitation method, electrolysis reclaim CoSO4、Li2CO3、CoC2O4、Co(OH)2, metal Co etc..But this
A little methods can cause secondary pollution using substantial amounts of organic reagent (acid, extractant) to environment；Complex process, is wanted to equipment
Ask high；Added value is low, and cost is high.Due to low value-added and high cost so that these technologies are not suitable for recycling without dilute
Applying waste lithium ionic electrokinetic cell (the LiFePO of noble metal4、LiMn2O4Deng).Therefore exploitation is specifically designed for lithium-ion-power cell
Recovery technology it is particularly necessary.
Ferric phosphate lithium cell due to extra long life, fast charging and discharging, high temperature resistant, Large Copacity, it is memoryless, use safety
The features such as and as Vehicles Collected from Market lithium battery first choice.With China's electric automobile, the demonstration operation of electric bicycle and popularization
Speed is accelerated, to electrokinetic cell especially with LiFePO4、LiMn2O4Type drastically increases for the consumption of the lithium-ion-power cell of representative
Plus, future will be faced with a large amount of waste and old electrokinetic cell process problems, if these old and useless batterys do not handle or handled bad, not only
Pollute the environment, but also the wasting of resources can be caused.
Chinese patent CN101383441A discloses a kind of comprehensive recovering process of positive pole waste tablet from ferric phosphate lithium cell, although
The pollution of solid waste is avoided, but technique is excessively complicated, it is more using raw material, while the chemical composition of positive electrode is
Change.Chinese patent CN1585180A discloses a kind of recovery method of lithium ion secondary battery positive defective material, this method
The positive pole leftover pieces relic produced when preparing lithium rechargeable battery is heat-treated, remove foil substrate and positive electrode it
Between adhesive, foil substrate and positive electrode are departed from using mechanical means, but the positive electrode system reclaimed using this method
Into lithium rechargeable battery capacity it is relatively low.Chinese patent CN1953269A discloses a kind of recovery of waste and old lithium ion battery
Method, although the isolated rough various materials of energy, but process conditions are higher, the secondary battery capacity that salvage material is made
It is relatively low.United States Patent (USP) US6514311B1 discloses a kind of pollution-free method that metal is reclaimed from used Li ion cell（Clean
Process of Recovering Metals from Water Lithium Iron Batteries）, pass through method for calcinating
Battery is destroyed and decomposed, then the collector of battery and active material are separated with electrolytic method again, valuable gold is therefrom extracted
Category, but method for calcinating destructive power is stronger, easy catching fire, and it is not readily separated relic.Chinese patent CN101847763A
A kind of method of waste lithium iron phosphate battery synthetical recovery is disclosed, using hydrometallurgical processes, by waste lithium iron phosphate material
Obtain being rich in the sediment of iron, lithium, phosphonium ion, then addition source of iron, lithium source in sediment by sour molten, purification and precipitation respectively
Or P source compound is eventually adding carbon source to adjust the mol ratio of iron, lithium, phosphorus, obtain new through being calcined in ball milling, inert atmosphere
Lithium iron phosphate positive material, the method raw material are applied widely, but in the more difficult control of actual mechanical process conditional, operate
The waste water produced in journey is more intractable, meanwhile, operating process requires very high, severe operational environment to equipment anticorrosion.Chinese patent
CN101916889 discloses a kind of method that lithium-ion-power cell recovery prepares LiFePO4, and this method is in separation ferric phosphate
With inorganic Ore Leaching Li after lithium anode material+、Fe2+And PO4 3-, then add lithium salts or molysite and ascorbic acid, control ph
Precipitated, finally ball milling, drying and calcination obtain lacking in LiFePO4, this method technical process in aqueous sucrose solution
The step of except metal impurities, product can be made to also have other a large amount of metals, quality is influenceed.
The content of the invention
High, the complex process for solution lithium iron phosphate dynamic battery cost recovery, the problems such as seriously polluted, we have proposed one
Kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method, use the present invention can with simplification of flowsheet, control cost and
Pollution.
The present invention is achieved by the following technical solutions：The present invention provides a kind of waste lithium iron phosphate electrokinetic cell green
Recovery and treatment method, step is as follows：
1）Old and useless battery is discharged first, according to the capacity of the ferric phosphate lithium cell, in the anode and negative
Load is connected between pole, control initial drain is between 0.1-0.5 times of battery Ah capability values, and discharge time control exists
In 2-20 hours, until cell voltage drops to zero；Battery after discharge process is moved in vacuum glove box, mechanical force is utilized
Battery is disassembled in cutting, is taken out battery core, is soaked in solvent, the aluminum plastic film and lug after immersion are directly reclaimed；
Preferably, when the binding agent that pole piece is used is oil-soluble binding agent, the solvent is 1-METHYLPYRROLIDONE
（NMP）, when the binding agent that pole piece is used is water-soluble binder, the solvent is deionized water.Wherein, nmp solvent is making
Waste liquid during lithium ion battery, herein reusable edible after treatment.
2）Battery core after immersion respectively obtains pure positive plate, negative plate and barrier film, barrier film is direct using mechanically decoupled
Reclaim, positive plate and negative plate remain subsequent operation；
3）Respectively by positive plate and negative plate mechanical crushing, the size of control fragment is not more than 2cm, and fragment is placed in into alkali lye
Middle soaking and stirring, washing and filtering.Resulting material is dried under vacuum, dry material is collected.
Preferably, described sig water is LiOH, NaOH or KOH solution, and pH value is 10 ~ 13, and spent lye can after processing
Recycle.
4）Dried positive pole material, negative pole mechanical mass are stirred respectively, then sieved, aluminium foil, just is obtained
Very coarse powder material（Positive mix and a small amount of aluminium skimmings）With copper foil, negative pole coarse powder material（Negative pole powder and a small amount of copper scale）, will divide
Aluminium foil and copper foil from after are reclaimed.Positive very coarse powder material, negative pole coarse powder material are subjected to ball milling, screening respectively.
5）By the positive mix after screening（LiFePO4 and acetylene black）At the heat for carrying out different temperatures under an inert atmosphere
Reason, negative pole powder（Graphite and acetylene black）The heat treatment of different temperatures is carried out in air atmosphere.Reclaim all powders.
Preferably, positive mix is heat-treated under an inert atmosphere, and negative pole powder is heat-treated in air atmosphere.
Preferably, the temperature of heat treatment, positive mix is 150 DEG C -400 DEG C, and negative pole powder is 200 DEG C -450 DEG C.With showing
There is technology to compare, the temperature of selection is relatively low, reduce a large amount of energy consumptions, obtain the powder of same purity.
Preferably, the inert atmosphere is nitrogen, helium, neon or argon gas.
Whole removal process is in a sealed environment, and the waste gas produced by removal process is located in by purifying column
Reason, to environment compared with prior art, the beneficial effects of the present invention are：
A, saving energy consumption, reduce cost recovery；
B, sig water used and solvent are not discharged, and can be recycled by processing with direct circulation, while cost-effective
It is free from environmental pollution；
C, whole technological process are not related to waste gas and discharge of wastewater, and environment is not polluted；
Powder after d, recovery is pure, can be used to produce battery without reprocessing；
E, reclaim powder reproduction performance of lithium ion battery it is excellent.
Brief description of the drawings
The photo for 5 kinds of accessory substances that Fig. 1 reclaims for the present invention；
A：Barrier film；B：Aluminum plastic film；C：Lug；D：Copper foil；E：Aluminium foil；
The cycle performance curve for the positive mix that Fig. 2 reclaims for the present invention；
The cycle performance curve for the negative pole powder that Fig. 3 reclaims for the present invention；
The process chart that Fig. 4 reclaims for the present invention.
Embodiment
With reference to embodiment, present disclosure is further illustrated.It should be appreciated that the implementation of the present invention is not limited to
In the following examples, any formal accommodation or change made to the present invention both fall within the scope of the present invention；And under
The method in embodiment is stated, is the conventional method of this area unless otherwise instructed.
Embodiment 1
3 waste and old 60Ah electric automobile lithium ferric phosphate power cells are subjected to constant volume, 0.2C electric discharges treat that voltage is down to 0,
Battery is moved in vacuum glove box, battery is disassembled using mechanical force cutting, takes out battery core, battery core is soaked in nmp solution,
Drying process after soaking 6 hours, directly reclaims aluminum plastic film（Figure 1B）And lug（Fig. 1 C）, while reclaiming nmp solution.
Mechanical force separation battery core is continued with, positive plate, negative plate and barrier film is obtained, its septation is directly reclaimed（Figure
1A）.
Respectively by positive plate and negative plate mechanical crushing, stop when no fragment length of side is more than 2cm, fragment is placed in pH
For soaking and stirring in 11 NaON solution 5 minutes, washing and filtering.Resulting material is dried under vacuum, dry material is collected,
Reclaim NaOH solution.
Dried positive pole material, negative pole mechanical mass are stirred respectively, is then sieved, obtains aluminium foil（Figure
1E）, positive very coarse powder material（Positive mix and a small amount of aluminium skimmings）And copper foil（Fig. 1 D）, negative pole coarse powder material（Negative pole powder and a small amount of
Copper scale）, directly reclaim aluminium foil and copper foil after separation.Positive very coarse powder material, negative pole coarse powder material are subjected to ball milling respectively,
400r/min ball milling 10min, after the completion of sieved.
The positive very coarse powder material comprising LiFePO4 and acetylene black after screening is first subjected to 250 DEG C of calcinings under nitrogen protection
5h, then 400 DEG C of calcining 10h are carried out, obtain pure regeneration lithium iron phosphate positive material；After screening comprising graphite and acetylene black
Negative pole powder carries out 400 DEG C of calcinings under air, reclaims all powders.
By the LiFePO4 active material of recovery：Conductive agent：Binding agent mass ratio is 90:5:5 ratio is fabricated to positive pole
Piece, using new graphite cathode piece, barrier film and electrolyte, battery is assembled into the dry glove box full of argon gas, is filled
Discharge test, as a result as shown in Fig. 2 and table 1.
By the graphite cathode material and new iron phosphate lithium positive pole piece, barrier film and electrolyte of recovery in the drying full of argon gas
Battery is assembled into glove box, charge-discharge test is carried out, as a result as shown in Figure 3.
Embodiment 2
The step of embodiment 2 is substantially the same manner as Example 1, it is different be after sieving comprising LiFePO4 and acetylene black
Positive very coarse powder material first carries out 250 DEG C of calcining 5h under nitrogen protection, then carries out 300 DEG C of calcining 10h, obtains pure regeneration ferric phosphate
Lithium anode material；The negative pole powder comprising graphite and acetylene black after screening carries out 300 DEG C of calcinings under air.
By the LiFePO4 active material of recovery：Conductive agent：Binding agent mass ratio is 90:5:5 ratio is fabricated to positive pole
Piece, using new graphite cathode piece, barrier film and electrolyte, battery is assembled into the dry glove box full of argon gas, is filled
Discharge test, as a result as shown in table 1.
By the graphite cathode material and new iron phosphate lithium positive pole piece, barrier film and electrolyte of recovery in the drying full of argon gas
Battery is assembled into glove box, charge-discharge test is carried out.
Embodiment 3
The step of embodiment 3 is substantially the same manner as Example 1, it is different be after sieving comprising LiFePO4 and acetylene black
Positive very coarse powder material carries out 250 DEG C of calcining 15h under nitrogen protection, obtains pure regeneration lithium iron phosphate positive material；After screening
Negative pole powder comprising graphite and acetylene black carries out 250 DEG C of calcinings under air.
By the LiFePO4 active material of recovery：Conductive agent：Binding agent mass ratio is 90:5:5 ratio is fabricated to positive pole
Piece, using new graphite cathode piece, barrier film and electrolyte, battery is assembled into the dry glove box full of argon gas, is filled
Discharge test, as a result as shown in table 1.
By the graphite cathode material and new iron phosphate lithium positive pole piece, barrier film and electrolyte of recovery in the drying full of argon gas
Battery is assembled into glove box, charge-discharge test is carried out.
Comparative example 1
The step of comparative example 1 is substantially the same manner as Example 1, it is different be after sieving comprising LiFePO4 and acetylene black
Positive very coarse powder material first carries out 250 DEG C of calcining 5h under nitrogen protection, then carries out 700 DEG C of calcining 10h, obtains pure regeneration ferric phosphate
Lithium anode material；The negative pole powder comprising graphite and acetylene black after screening carries out 700 DEG C of calcinings under air.
By the LiFePO4 active material of recovery：Conductive agent：Binding agent mass ratio is 90:5:5 ratio is fabricated to positive pole
Piece, using new graphite cathode piece, barrier film and electrolyte, battery is assembled into the dry glove box full of argon gas, is filled
Discharge test, as a result as shown in table 1.
By the graphite cathode material and new iron phosphate lithium positive pole piece, barrier film and electrolyte of recovery in the drying full of argon gas
Battery is assembled into glove box, charge-discharge test is carried out.
Charge-discharge performance test is carried out after above-mentioned recovery positive electrode restructuring battery, as a result such as table 1：
Table 1
| 0.1C discharge capacities（mAh/g） | 0.5C discharge capacities（mAh/g） | Capability retention after 0.1C is circulated 50 times | |
| Embodiment 1 | 144.7 | 128.9 | 100% |
| Embodiment 2 | 139.5 | 125.3 | 99.7% |
| Embodiment 3 | 133.2 | 119.4 | 99.3% |
| Comparative example 1 | 145.3 | 129.2 | 100% |
As can be seen from the results, each products pure degree that the method provided by using the present invention is reclaimed is higher, restructuring
The performance of new material can be reached after battery, and technological process is simple, and any waste water and gas discharge is not related to；Meanwhile, the present invention
Calcining heat is low compared with traditional handicraft in the method for offer, but the product restructuring performance and traditional handicraft that obtain be not substantially poor
Not, the energy is saved, cost recovery is reduced.
Claims (4)
1. a kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method, it is characterised in that comprise the following steps：
1）Old and useless battery is discharged, and cutting is soaked in solvent after disassembling, and the aluminum plastic film and lug after immersion are directly reclaimed；It is described molten
Agent is 1-METHYLPYRROLIDONE or deionized water；
2）Battery core after immersion is separated, and obtains positive plate, negative plate and barrier film, and its septation is directly reclaimed；
3）Respectively by positive plate and negative plate mechanical crushing, soaking and stirring in alkali lye, washing and filtering, resulting material vacuum are placed in
Drying；
4）Dried positive pole material, negative pole mechanical mass are stirred respectively, is then sieved, obtains aluminium foil, positive pole thick
Powder and copper foil, negative pole coarse powder material, the aluminium foil after separation and copper foil are reclaimed, respectively that positive very coarse powder material, negative pole is thick
Powder carries out ball milling, screening；
5）Positive mix after screening and negative pole powder are heat-treated, reclaimed afterwards；Positive mix is warm under an inert atmosphere
Processing, negative pole powder is heat-treated in air atmosphere；The temperature of the heat treatment, positive mix is 150 DEG C -400 DEG C, is born
Pole powder is 200 DEG C -450 DEG C.
2. a kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method according to claim 1, it is characterised in that alkali
Liquid pH value is 10 ~ 13.
3. a kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method according to claim 1, it is characterised in that institute
Battery core separation is stated using mechanically decoupled.
4. a kind of waste lithium iron phosphate electrokinetic cell green reclaim processing method according to claim 1, it is characterised in that whole
Individual removal process is in sealed environment.
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| CN106992328B (en) * | 2016-01-21 | 2019-10-29 | 河南师范大学 | The waste lithium iron phosphate positive electrode method that recycling recycles in Hawkins cell |
| CN105811038A (en) * | 2016-04-21 | 2016-07-27 | 国网北京市电力公司 | Separation technology of electrodes of lithium ion battery |
| CN105826629B (en) * | 2016-05-13 | 2018-05-25 | 国网河南省电力公司电力科学研究院 | A kind of waste lithium cell full constituent feed separation collection device and method |
| CN105895854A (en) * | 2016-06-14 | 2016-08-24 | 天齐锂业股份有限公司 | Recovery method of positive electrode leftover material of lithium-ion battery |
| CN105870533B (en) * | 2016-06-14 | 2018-05-11 | 天齐锂业股份有限公司 | The method for recycling lithium ion cell positive leftover pieces |
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| CN106785171A (en) * | 2017-01-19 | 2017-05-31 | 湖州南浔中连水产养殖有限公司 | A kind of automobile power cell resource reclaiming system and resource utilization method |
| CN107086334A (en) * | 2017-03-14 | 2017-08-22 | 北京赛德美资源再利用研究院有限公司 | A kind of waste and old dynamic lithium battery automation splits the clean recovery method of full constituent |
| CN107069134A (en) * | 2017-03-24 | 2017-08-18 | 孙志廷 | A kind of method that waste lithium cell positive electrode is separated with collector |
| CN107317064A (en) * | 2017-06-22 | 2017-11-03 | 中南大学 | A kind of recovery method of waste lithium cell |
| CN107706478B (en) * | 2017-10-13 | 2020-06-09 | 宁波中车新能源科技有限公司 | Recovery method of battery capacitor |
| CN108110359A (en) * | 2017-12-16 | 2018-06-01 | 淄博国利新电源科技有限公司 | The circulation utilization method of positive electrode |
| CN109550568A (en) * | 2018-10-31 | 2019-04-02 | 株洲鼎端装备股份有限公司 | A kind of used Li ion cell cracking and sorting technique |
| CN111072023B (en) * | 2019-12-27 | 2022-02-08 | 北京蒙京石墨新材料科技研究院有限公司 | Method for recycling graphite from scrapped lithium ion battery |
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