CN104593606B - Waste and old cobalt acid lithium ion battery defective positive and negative pole material method of resource - Google Patents

Waste and old cobalt acid lithium ion battery defective positive and negative pole material method of resource Download PDF

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CN104593606B
CN104593606B CN201510017033.1A CN201510017033A CN104593606B CN 104593606 B CN104593606 B CN 104593606B CN 201510017033 A CN201510017033 A CN 201510017033A CN 104593606 B CN104593606 B CN 104593606B
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ion battery
lithium ion
waste
vibrating screen
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CN104593606A (en
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李佳
许振明
王光旭
齐婷
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Shanghai Jiaotong University
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    • 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

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Abstract

Just the invention discloses a kind of waste and old cobalt acid lithium ion battery, negative pole defective material method of resource, employing high speed impact crushes, vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, the techniques such as alternating temperature filtration combine and just utilize in waste and old cobalt acid lithium ion battery, negative pole defective material prepares simple substance cobalt, the products such as lithium carbonate and graphite powder, employing high speed impact crushes, vibrosieve, the modes such as wet magnetic separation carry out material separation and enrichment, maintain the original physical property of material, effectively make use of negative pole graphite material, prepared by the original position achieving resource, cost-effective, use anaerobic normal pressure roasting, reaction condition is looser, reduce graphite material loss, simple flow, whole set process is without adding any chemical agent, non-secondary pollution, it is beneficial to commercial Application practice.The present invention solves the pollution-free process problem of the corner relic that cell production companies produces during manufacturing lithium ion battery, provides the recovery method of a kind of secondary mineral products-cobalt resource simultaneously.

Description

Waste and old cobalt acid lithium ion battery defective positive and negative pole material method of resource
Technical field
The present invention relates to the resource reclaim to waste and old lithium ion battery valuable component, in particular for cobalt acid lithium battery Produced positive pole, negative pole leftover pieces and effective Environmental-protection recycling method of relic in production process, belong to environment and protect Electron wastes in protector for collar territory processes, resource field.
Background technology
Global lithium ion battery shipment amount about 42.98 hundred million in 2011, market scale reaches 92,400,000,000 yuans, relatively Within 2010, increase by 24.16%.Between anticipated 2012-2020, portable Li-like ions battery, power lithium-ion battery will divide Not with 7.58%, 26.84% compound growth rate sustainable growth, the year two thousand twenty whole world lithium ion battery market scale is up to 386600000000 yuan.Along with the extensive application of lithium ion battery, its usage amount increases year by year, in production and the system of lithium ion battery The leftover pieces and the relic that produce during making the most drastically increase, most producers to these leftover pieces relics only with at a low price Manage to relevant unit or use acid-alkali treatment to obtain cobalt salt, lithium salts etc..And with discarded cobalt acid lithium ion battery be Example, wherein valuable metal such as cobalt (Co) accounts for 15%, is the hundred times of China's cobalt ore average grade 0.02%, potential value Accounting for the 82.40% of whole battery, copper (Cu), aluminum (Al) tenor reach 18.7%, have significant resource.? Today that resource day is becoming tight, recovery and the resource meaning of the positive and negative electrode defective material of waste lithium cell also become apparent from.
The positive active material of lithium ion battery typically uses slotting lithium compound, such as LiCoO2, LiNiO2, LiMn2O4 and LiFePO4 etc., by a kind of doping therein and conductive agent (such as graphite, acetylene black) and binding agent (such as poly-inclined difluoro second PVDF, polytetrafluoroethylene PTFE) etc. mix homogeneously by a certain percentage, then stir into pasty state, be uniformly coated on aluminium foil Both sides, and under an inert atmosphere be dried remove organic dispersing agent, make anode finally by chaser is compressing. And negative electrode active material is generally adopted by amorphous carbon material or graphitized carbon material, it is mixed homogeneously with binding agent, even It is coated in Copper Foil both sides, is dried and rolls and make battery cathode.
At present, technology both domestic and external bias toward use physics combine with chemical method Mechanical Crushing, acidleach, chemistry sink Positive electrode containing cobalt is reclaimed, if Chinese invention patent is " from waste and old lithium ion battery by the modes such as shallow lake, solvent extraction The method of middle Call Provision " (Li Jinhui etc., the patent No. 200810116297.2), it is provided that a kind of from waste and old lithium-ion electric The method of Call Provision in pond, after discharging waste and old lithium ion battery, uses coarse crushing to isolate Fe, Al, Cu, moulds Material and organic film and siftage matter, ultrasonic stirring is cleaned to obtain LiCoO2 powder on aluminium foil, and salt Ore Leaching Metallic element, chemical precipitation obtains cobalt oxalate and is thermally treated resulting in Co2O3.The method uses a large amount of chemical agents to give back to knock off Skill brings secondary pollution, can cause the waste of some electrode materials powder during coarse crushing, and a large amount of hydrochloric acid used are to setting Standby corrosion-resistant require high-leveled and difficult in commercial Application.
Chinese invention patent " a kind of method reclaiming valuable metal from waste lithium cell " (Zhang Yongxiang, the patent No. 201010262198.2), a kind of method reclaiming valuable metal from waste lithium cell is disclosed, after Mechanical Crushing Waste lithium cell, through 350 DEG C-400 DEG C calcinings of pyrogenic process high temperature, obtains the material containing cobalt, copper and aluminum, adds alkali liquor afterwards Except aluminum, recycling sulphuric acid and extractant copper removal.Alkali liquor discharges a large amount of gas during removing aluminum and operator is produced harm, Broken waste lithium cell is directly carried out high-temperature calcination, wastes negative pole graphite material, the use of a large amount of business extractants Add process costs to put into.
Chinese invention patent " a kind of process processed from waste lithium cell " (Fang Weiqing, the patent No. 201010295586.0), nmp solvent will be used to dissolve after waste lithium cell primary separation, cobalt acid lithium slag passes through water Wash, filter, be dried, leaching etc. obtains B-Co (OH) after obtaining the further complex-precipitation of cobalt liquid2.This process technique obtains To end-product be precipitate B-Co (OH)2, not cobalt simple substance, it is unfavorable for recycling further of product, puts into industry The value of application is relatively low.
(Wei enters equality, the patent No. to Chinese invention patent " recovery method of lithium ion secondary battery positive defective material " 200410019542X), positive pole leftover pieces produced when preparing lithium rechargeable battery and relic are carried out heat treatment, removes Debindered dose, mechanical means is used foil substrate to be departed from positive electrode；Or utilize ultrasonic wave concussion or mechanical agitation To depart from positive electrode in foil substrate etc. method, then separated by positive electrode, obtaining after dried can be direct The positive electrode of the function admirable used.Introducing impurity during broken or concussion, also needing to process further could again The secondary manufacturing being applied to battery, and negative pole relic does not obtain Appropriate application.
The recycling recovery process of current lithium ion battery is mainly hydrometallurgical processes associated with acidleach and solvent extraction, During processing cobalt acid lithium battery electrode material, need the leaching carrying out cobalt to process with Chemical deep, produce a large amount of high The chemical acid alkali waste liquid of concentration, brings secondary pollution, commercial extractant to cause the raising of processing cost.And concentrate positive pole material In material, valuable metal cobalt and the extraction of lithium, ignore the recycling of other resources.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide a kind of waste and old cobalt acid lithium ion battery positive and negative electrode Defective material method of resource, uses that high speed impact is broken, vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, alternating temperature filter Combining etc. technique utilizes positive and negative electrode defective material in waste and old cobalt acid lithium ion battery to prepare simple substance cobalt, lithium carbonate and graphite powder Deng product.
The present invention includes that high speed impact crushes-vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, alternating temperature filtration etc. four Step, specifically comprises the following steps that
Step one, adds the first impact crusher by positive pole relic and pulverizes, and the material after pulverizing is through the first vibrosieve Extension set sieves, and this first vibrating screen classifier uses double mesh structure, and sieve aperture is respectively 0.3mm, 2mm；Negative pole is residual Sheet adds the second impact crusher and pulverizes, and the material after pulverizing sieves through the second vibrating screen classifier, and this is second years old Vibrating screen classifier uses single mesh structure, and sieve aperture is 2mm.The tup that disintegrating machine high speed rotates makes LiCoO2Powder is from aluminum Peel off on paper tinsel, powdered graphite is peeled off from Copper Foil.Positive pole relic sieve upper for be not completely exfoliated containing LiCoO2The Copper Foil of powder Add disintegrating machine by device for transporting objects to crush again, sieve is the aluminium foil containing a small amount of electrode powder, it is achieved the resource of aluminum. Sieve is lower is the electrode powder mixing material produced in shattering process, is mainly composed of LiCoO2Powder, powdered graphite and binding agent Mixture.Negative pole relic sieve is upper for the Copper Foil containing a small amount of electrode powder, it is achieved the resource of copper.Sieve is lower for shattering process The electrode powder mixing material of middle generation, is mainly composed of the mixture of powdered graphite and binding agent.
Step 2, being mixed by minus sieve powder in step one, carry out roasting under protective atmosphere, sintering temperature is 850～900 DEG C, Temperature retention time is 20～40 minutes.Roasting process reacts: 4LiCoO2+ 3C=2Li2CO3+4Co+CO2, produce Thing is simple substance cobalt, lithium carbonate powder, powdered graphite mixture.
Step 3, by the product powder wet magnetic separation of step 2 kind, medium is water.Magnetic separator is general wet magnetic separator, from Magnetic separator concentrate mouth is discharged material room temperature and is filtrated to get product is that simple substance thick cobalt powder (Co) purity reaches 97%, it is achieved that high The resource of added value cobalt.
In step 4, step 3, the mine tailing mouth of wet magnetic separation get rid of material room temperature to be filtrated to get product is graphite powder, it is achieved that The resource of graphite powder.
Step 5, in step 3, the filtrate of wet magnetic separation is heated to 80～90 DEG C, and being filtrated to get product is lithium carbonate (Li2CO3) Powder, it is achieved that the resource of high added value lithium carbonate.
Preferably, in step one, process the selection of broken rear positive pole relic and the negative pole different mesh structure of relic vibrosieve, Based on the difference of Binder Properties in the preparation process of positive and negative material pole.Positive pole uses PVDF to make binding agent, at N- Having viscosity higher and caking property in methyl pyrrolidone (NMP) solvent, the consumption of organic solvent of this binding agent is big And combination ratio is stronger.And negative pole uses water-soluble binder butadiene-styrene rubber (SBR) etc., combination is relatively Destructible.
Preferably, step 2 is with step 3, and vibrating screen classifier is continuous feed, and sifting bed inclination angle is 3-5 degree.
Preferably, in step 4, described roasting process can use batch (-type) to feed with continuous way, and protective atmosphere is optional With the noble gas such as nitrogen or argon.
Preferably, in step 3, the selection of described wet magnetic separator, based on the physical property of product powder in step 2 Can difference.In step 2, product powder is simple substance cobalt, lithium carbonate powder, powdered graphite mixture, and simple substance cobalt is magnetic gold Belonging to, lithium carbonate is slightly soluble in water, and powdered graphite is water insoluble.
Preferably, in step 5, filtrate is without discharge, makes directly as the liquid medium circulation of wet magnetic separator in step 3 With, it is achieved that without discharging of waste liquid.
Preferably, the impact grinding described in technique, vibrosieve, anaerobic normal pressure roasting technique equipment use hermetically sealed, and Arranging air vent, air-flow is provided negative pressure to eliminate harmful substance through activated carbon by centrifugal blower.
The operation principle of the present invention: utilize Mechanical Crushing and vibrosieve to realize the electrode being attached on positive and negative electrode relic Coming off of material powder；Through anaerobic constant-pressure and high-temperature roasting, promote to react 4LiCoO2+ 3C=2Li2CO3+4Co+CO2Enter OK；Magnetic according to product and dissolubility difference, utilize wet magnetic separation and filter type of heating obtains final products, it is achieved The high added value resource of waste and old cobalt acid lithium ion battery positive and negative electrode defective material.
Compared with prior art, the present invention has a following beneficial effect:
(1) utilize the techniques such as impact grinding, vibrosieve, magnetic separation, anaerobic normal pressure roasting to combine and realize the acid of waste and old cobalt The complete resource of valuable component in lithium ion battery positive and negative electrode defective material, with mineral acid leaching, chemical precipitation, extraction Take agent extraction phase ratio and there is the feature such as low cost, efficient, non-secondary pollution.
(2) process collaborative for the positive and negative electrode powder of electrode material, effectively make use of negative pole graphite material, it is achieved that Prepared by the original position of resource, cost-effective.
(3) using anaerobic normal pressure roasting, reaction condition is relatively loose, reduces graphite material loss, simple flow, the whole series Technique is without adding any chemical agent, and non-secondary pollution, beneficially commercial Application are put into practice.
(4) the pollution-free process of the corner relic that cell production companies produces during manufacturing lithium ion battery is solved Problem, provides the recovery method of a kind of secondary mineral products-cobalt resource simultaneously.
Accompanying drawing explanation
The detailed description made non-limiting example with reference to the following drawings by reading, other of the present invention is special Levy, purpose and advantage will become more apparent upon:
Fig. 1 is the flow chart of the inventive method；
Fig. 2 is X-ray diffraction (XRD) figure of mixed-powder after step 4 anaerobic normal pressure roasting of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following example will assist in those skilled in the art Member is further appreciated by the present invention, but limits the present invention the most in any form.It should be pointed out that, the common skill to this area For art personnel, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement.These broadly fall into Protection scope of the present invention.
As it is shown in figure 1, waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, the method uses high-speed punching Break up the techniques such as broken, vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, alternating temperature filtration to combine and utilize waste and old cobalt acid lithium In lithium ion battery, positive and negative electrode defective material prepares the products such as simple substance cobalt, lithium carbonate and graphite powder.Including high speed impact broken- Four steps such as vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, alternating temperature filtration are concrete:
Step one, positive pole relic are separately added into impact crusher with negative pole relic and pulverize, and the material after pulverizing is through shaking Dynamic sieve screening.Positive pole relic screening machine uses double mesh structure, and sieve aperture is respectively 0.3mm, 2mm；Negative pole relic screening machine Using single mesh structure, sieve aperture is 2mm.The tup that disintegrating machine high speed rotates makes LiCoO2Powder peels off from aluminium foil, Powdered graphite is peeled off from Copper Foil.Positive pole relic sieve upper for be not completely exfoliated containing LiCoO2The Copper Foil of powder is defeated by material Send device to add disintegrating machine to crush again, sieve is the aluminium foil containing a small amount of electrode powder, it is achieved the resource of aluminum.Sieve is lower to be broken The electrode powder mixing material produced during broken, is mainly composed of LiCoO2Powder, powdered graphite and the mixture of binding agent. Negative pole relic sieve is upper for being the Copper Foil containing a small amount of electrode powder, it is achieved the resource of copper.Sieve is lower for generation in shattering process Electrode powder mixing material, is mainly composed of the mixture of powdered graphite and binding agent.
Step 2, being mixed by minus sieve powder in step one, carry out roasting under protective atmosphere, sintering temperature is 850～900 DEG C, Temperature retention time is 20～40 minutes.Roasting process reacts: 4LiCoO2+ 3C=2Li2CO3+4Co+CO2, roasting Burn afterproduct and be detected as simple substance cobalt, lithium carbonate powder, powdered graphite through X-ray diffraction (XRD) (as shown in Figure 2) Mixture.
Step 3, by the product powder wet magnetic separation of step 2 kind, medium is water.Magnetic separator is general wet magnetic separator, from Magnetic separator concentrate mouth discharge material room temperature is filtrated to get product and is detected as through X-ray diffraction (XRD) (as shown in Figure 2) Simple substance cobalt powder (Co), detects through inductive coupling plasma emission spectrograph (ICP), and result is as shown in table 1, products C o Purity reaches 97%, it is achieved that the resource of high added value cobalt.
Table 1 product coarse Co meal component icp analysis (%)
In step 4, step 3, the mine tailing mouth of wet magnetic separation get rid of material room temperature to be filtrated to get product is graphite powder, it is achieved that The resource of negative material.In step 5, the filtrate of wet magnetic separation is heated to 80～90 DEG C, and being filtrated to get product is lithium carbonate (Li2CO3) powder, it is achieved that the resource of high added value lithium carbonate.
In the present embodiment, process broken after positive pole relic and the selection of the negative pole different mesh structure of relic vibrosieve, based on just, The difference of Binder Properties in the preparation process of negative material pole.Positive pole uses PVDF to make binding agent, at N-methylpyrrole Having viscosity higher and caking property in alkanone (NMP) solvent, the consumption of organic solvent of this binding agent is big and combination side Formula ratio is stronger.And negative pole uses water-soluble binder butadiene-styrene rubber (SBR) etc., combination relatively destructible.
In the present embodiment, vibrating screen classifier is continuous feed, and sifting bed inclination angle is 3-5 degree.
In the present embodiment, roasting process can use batch (-type) to feed with continuous way, and protective atmosphere can be selected for nitrogen or argon etc. Noble gas.
In the present embodiment, the selection of wet magnetic separator, based on the physical property difference of product powder in step 3.Step In two, product powder is simple substance cobalt, lithium carbonate powder, powdered graphite mixture, and simple substance cobalt is magnetic metal, and lithium carbonate is micro- Being dissolved in water, powdered graphite is water insoluble.As in figure 2 it is shown, wet magnetic separator concentrate mouth discharge is simple substance cobalt.
The present embodiment uses the technique phases such as impact grinding, vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, alternating temperature filtration It is implemented in combination with valuable component method of resource in waste and old cobalt acid lithium ion battery positive and negative electrode relic, there is low cost, height Effect, simple in construction, the feature such as pollution-free；The present embodiment processes collaborative for the positive and negative electrode powder of electrode material, effectively Make use of negative pole graphite material, it is achieved that prepared by the original position of resource.Using anaerobic normal pressure roasting, reaction condition is relatively loose, Reduce graphite material loss, simple flow, whole set process without adding any chemical agent, non-secondary pollution, beneficially work Industry application practice.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in Stating particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, This has no effect on the flesh and blood of the present invention.

Claims (6)

1. a waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, it is characterised in that the method includes: high speed impact is broken-and vibrosieve, anaerobic normal pressure roasting, wet magnetic separation, alternating temperature filter four steps, concrete:
Step one, adds the first impact crusher by positive pole relic and pulverizes, and the material after pulverizing sieves through the first vibrating screen classifier, and this first vibrating screen classifier uses double mesh structure, and sieve aperture is respectively 0.3mm, 2mm；Negative pole relic being added the second impact crusher pulverize, the material after pulverizing sieves through the second vibrating screen classifier, and this second vibrating screen classifier uses single mesh structure, and sieve aperture is 2mm；
Step 2, by after the minus sieve powder mixing of the minus sieve powder of the first vibrating screen classifier in step one and the second vibrating screen classifier; roasting is carried out under protective atmosphere; sintering temperature is 800～900 DEG C, and temperature retention time is 20～40 minutes, reacts in roasting process: 4LiCoO2+ 3C=2Li2CO3+4Co+CO2, obtaining product is simple substance cobalt, lithium carbonate powder, powdered graphite mixture；
Step 3, product step 2 obtained carry out magnetic separation by wet magnetic separator powder, and medium is water, the material that the concentrate mouth of wet magnetic separator is discharged is carried out room temperature filtration, obtains the thick cobalt powder of simple substance；
Step 4, by step 3 wet magnetic separation mine tailing mouth discharge material carry out room temperature filtration, obtain graphite powder；Filter after the filtrate of wet magnetic separation is heated to 80～90 DEG C in step 3, obtain lithium carbonate powder.
One the most according to claim 1 waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, it is characterised in that in step one, the first described vibrating screen classifier uses double mesh structure, makees binding agent with PVDF；Second vibrating screen classifier uses single mesh structure, makees binding agent with water-soluble binder butadiene-styrene rubber (SBR).
One the most according to claim 1 waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, it is characterised in that in step one, described the first vibrating screen classifier, the second vibrating screen classifier are continuous feed, and sifting bed inclination angle is 3-5 degree.
One the most according to claim 1 waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, it is characterised in that in step 2, described roasting process uses batch (-type) or continuous way charging, and described protective atmosphere selects nitrogen or argon.
One the most according to claim 1 waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, it is characterized in that, the filtrate water carrying out after the filtrate of wet magnetic separation is heated to 80～90 DEG C in step 3 being filtrated to get is recycled as the liquid medium of wet magnetic separator in step 3.
One the most according to claim 1 waste and old cobalt acid lithium ion battery positive and negative electrode defective material method of resource, it is characterized in that, described the first impact crusher, the second impact crusher, the first vibrating screen classifier, the second vibrating screen classifier and anaerobic normal pressure roasting apparatus all use hermetically sealed, and air vent is set, air-flow is provided negative pressure to eliminate harmful substance through activated carbon by centrifugal blower.
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