CN103066343A - Method for processing separated active matter and aluminum in lithium ion battery positive plate - Google Patents
Method for processing separated active matter and aluminum in lithium ion battery positive plate Download PDFInfo
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- CN103066343A CN103066343A CN2012105622717A CN201210562271A CN103066343A CN 103066343 A CN103066343 A CN 103066343A CN 2012105622717 A CN2012105622717 A CN 2012105622717A CN 201210562271 A CN201210562271 A CN 201210562271A CN 103066343 A CN103066343 A CN 103066343A
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- aluminium
- chlorine
- oxygen
- chlorination
- lithium ion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Abstract
Provided is a method for processing separated active matter and aluminum in a lithium ion battery positive plate. After a failure lithium ion battery positive plate is smashed and dried, under the temperature of 300-380 DEG C, chlorine is piped in to carry out chlorination separating treatment, and hot volatile components and solid products containing positive active matters are obtained; and the hot volatile components are directly condensed to obtain aluminum chloride or are oxidized to obtain alumina. According to the method, the aluminum and the positive active matters are efficiently separated to facilitate later processing and machining; and the process is short in line, the separating effect is good, aluminum salt yield is high, and energy consumption is low.
Description
Technical field
The invention belongs to the resource circulation utilization field, the method that is specifically related to from based lithium-ion battery positive plate, to separate aluminium and the valency active matter is arranged.
Background technology
Lithium ion battery is modern advanced chemical power source, the power source that is widely used in consumption electronic product, war products, aeronautical product, instrument and shipping products etc., also be the light high-energy electrokinetic cell of following electric automobile first-selection, have huge market in the whole world.The structure that lithium ion battery is similar to other chemical power sources: shell, battery core, electrolyte; Wherein battery core is formed with certain textural association by positive plate, negative plate, barrier film.Positive plate is that positive electrode is coated on the aluminium plasma membrane and forms, and negative plate is that negative material is coated on the copper film and forms.As the positive electrode of the lithium ion " depots " of lithium ion battery, be the composite oxide material take non-ferrous metal elements such as Li, Co, Ni, Mn as chief component, such as LiCoO
2, Li (Co, Ni) O
2, Li (Co, Ni, Mn) O
2Deng.As seen, anode material for lithium-ion batteries has become one of important applied field of nonferrous materials.
Take mobile communication as example, Global Mobile Phone Users surpasses 3,500,000,000 at present, and Chinese user surpasses 600,000,000, and at increase year after year.As rechargeable battery, after lithium ion battery discharges and recharges through hundreds of times (normal operation 1 ~ 2 year), owing to dilatancy, capacity loss etc. cause scrapping, then scrap pending lithium ion battery enormous amount every year, and will increase substantially year by year.A large amount of discarded lithium ion batteries that lost efficacy have become the important secondary resource of Li, Co, Ni, Mn, Cu and Al etc.The battery core of dead battery after removing shell (metal or plastics), its metal element content is listed in the table 1.Wherein copper is the current collector material as battery cathode, and aluminium is the current collector material of anode, and cobalt (nickel, manganese) and lithium are the main components of positive electrode active materials.Therefore, waste and old lithium ion battery is the important secondary resource of copper, aluminium, lithium, cobalt (nickel, manganese) etc., has the content higher than its first resource.
Tenor in the common lithium ion battery core body of table 1 material
| Element term | Co(Ni,Mn) | Cu | Al | Li |
| Content/% | 20.0~22.0 | 18.0~20.0 | 6.0~6.4 | 2.2~2.5 |
For cobalt most valuable in the battery, lithium and copper, it is the most convenient that both positive and negative polarity is separately processed.Adopt special disintegration separation equipment, battery can be disintegrated, and positive and negative electrode is separated; From negative plate, reclaim and obtain copper, from positive plate, reclaim cobalt, nickel, manganese and lithium.For present lithium ion battery with graphite cathode material, the recovery of negative pole copper and graphite is relative simple, can reach target with simple high melt.And the processing relative complex of positive plate and have higher economic worth.
In the process of processing positive plate, the aluminium plasma membrane is the first step with separating of active material; The method of separating aluminium film and active material has Physical, chemical method, and respectively by different approach: l) the dissolving binding agent destroys contact interface; 2) dissolving collector.In lithium ion battery manufacture process, binding agent PVDF is adjoined pyrrolidone with the NMP(N-methyl) dissolving, with positive active material or negative electrode active material mixing furnishing slurry, be coated in again and make membrane coated electrode on the metal collector
[1]In the research that now has been reported, adopt the organic solvent dissolution aluminium foil base binding agent PVDF on the useless pole piece that films, can conveniently reclaim positive electrode active material and metal A l
[2]Utilize positive electrode active material to be insoluble to the character of alkali, dissolve in advance most of aluminium in the useless pole piece of filming with NaOH, and positive electrode active material is all stayed alkali and soaked in the slag and separated
[3]But the organic solvent kind that can dissolve PVDF is few, price is high, and limited to the solvability of PVDF; Although solvent can be recycled, separate PVDF difficulty and purifies and separates cycle weak point.The aluminium foil alkali solution technique adopts the highly basic operation, increase the molten acid consumption of follow-up acid, and operating environment is poor; Generate Al (OH)
3Particle is tiny, and carries carbon dust particulate and organic binder bond colloid secretly, filters, washs difficulty; The Al that obtains (OH)
3Impurity is high, is difficult to utilize.The method separating effect of pyrolysis PVDF is not good, and the active matter rate of recovery is lower.
List of references:
1. Wu Yu is flat, Dai Xiaobing, and the horse army flag, etc. lithium ion battery one application and practice [M]. Beijing: Chemical Industry Press, 2004
2. Qin Yi is red, Qi Shen. Treatment of Waste Lithium-ion Batteries by Organic Solvent Partition Process [J]. and non-ferrous metal (Smelting Part), 2006,1:13-16
3. Wu Fang. from spent lithium-ion secondary batteries, reclaim cobalt and lithium [J]. China YouSe Acta Metallurgica Sinica, 2004,14 (4): 697-701
Summary of the invention
The present invention be directed to the deficiency that present processing method exists, propose the method for the lithium ion anode sheet of easily handling failure, efficiently separate aluminium and positive electrode active material, so that follow-up treatment and processing; And process route is short, good separating effect, and the aluminium salt yield of gained is high; Energy consumption is low.
Technical scheme of the present invention is: after the fragmentation of disabled lithium ion cell positive plate process, drying, under 300 ~ 380 ℃ of temperature, pass into chlorine and carry out the chlorination separating treatment, obtain hot volatile matter and solid product positive electrode active material; With the direct condensation of described hot volatile matter, or carry out oxidation and obtain aluminium oxide.
The aluminium chloride that the heat volatilization is divided into gaseous state can obtain aluminium chloride through condensation.
Should control in the technique of the present invention and process 1kg aluminium total chlorine gas amount 4.1 ~ 4.5kg.
In the technique of the present invention, the inventor is by repeatedly putting into practice the chlorination separating effect of finding that chlorine flowrate can be obtained goodly by 1kg aluminium 0.14 ~ 0.42kg/min.
Described hot volatile matter oxidation obtains alumina process and is: hot volatile matter gas is directly passed in the oxidation reactor, obtain aluminium oxide and chlorine with the reaction of preheating purity oxygen; Gained chlorine returns for the chlorination separating treatment after red-hot carbon granules removes oxygen.
Enter in the oxidation reactor 250 ~ 350 ℃ of volatile matter gas temperatures; Preheated oxygen temperature to 300 ~ 400 ℃.Through gathering dust, purifying, get ultra-fine alumina and chlorine through oxidation reactor fluid-mixing out.
Oxidizing process oxygen aluminum ratio: control is processed 1kg aluminium with total amount of oxygen 0.90 ~ 0.95kg.
In the technique of the present invention, the inventor is advisable by 1kg aluminium 0.030 ~ 0.092kg/min by repeatedly putting into practice the discovery oxygen flow.
Except oxygen, 350 ~ 400 ℃ of carbon granules temperature are reacted (carbon-coating stop) time 2 ~ 6min to the chlorine that oxidation reaction produces through red-hot carbon granules pull-up.
Aluminium in the lithium ion anode sheet be a kind of relatively active metal, very easily with the performance of chlorine reaction, realize the effective separation of aluminium and active material by following series reaction:
2/3Al+Cl
2==1/3Al
2Cl
6(g)
⊿G
0=-101460+1.65TlogT+1.41T(cal/mol)(453~933K)
Product aluminium chloride volatilizees with dimeric form, separates with solid material.
Active material after the separation can be processed the compound that reclaims non-ferrous metal lithium, cobalt, nickel and manganese etc. through processing; The aluminium chloride of hot volatile matter gaseous state can obtain aluminium chloride through condensation, or obtains ultra-fine alumina and reclaim chlorine (returning use) through dioxygen oxidation.Can realize the chlorine circulation with oxidizing process:
Al
2Cl
6+O
2==Al
2O
3+Cl
2(g)
The chlorination of metallic aluminium and the oxidation of aluminium chloride are exothermic process, when lower temperature operates, can take full advantage of reaction heat, only need to supply with a small amount of energy.
According to above principle, the present invention processes the based lithium-ion battery positive plate separating active substances and specifically can be divided into the technical process of aluminium: material is prepared, chlorination separates, volatile matter processing etc.; It is most important link that wherein chlorination, volatile matter are processed.
The material set-up procedure: the positive plate of disassembling out from old and useless battery is the long strip type tablet, and activity and binding agent are through applying, be compacted at aluminium film surface.In order to make aluminium film obtain larger respond, with the carrying out of accelerated reaction, must carry out to material the processing in early stage.Processing to the lithium ion anode sheet is relatively simple, and main program is broken, oven dry.
The chlorination separation process: the present invention changes into aluminium chloride, also volatilization with metallic aluminium in the lithium ion anode sheet under chlorination, to realize the Selective Separation of aluminium and positive active material.Simultaneously, the inventor decomposes generation HF participation reaction for fear of binding agent PVDF in the present invention, adopts lower temperature.
Volatile matter is processed: metallic aluminium changes volatile matter over to after chlorination, remains to be entered to process to obtain the aluminium compound product.The aluminium chloride of gaseous state can obtain aluminium chloride through condensation, also can obtain aluminium oxide, reclaim chlorine simultaneously through dioxygen oxidation; In the present technique, in order to guarantee oxygen not to be introduced the chlorination separation process, the gaseous product of oxidizing process is processed deoxidation to obtain pure chlorine through red-hot carbon.
The present invention is directed to the processing of disabled lithium ion cell positive plate, but the short flow process of whole technique and high efficiente callback raffinal product salt; Can effectively reduce the cost that the valency complex materials is arranged of processing based lithium-ion battery positive plate and containing metal aluminium, the construction cost that reduces the shop equipment facility; Improve equipment capacity, energy efficient; The more important thing is and do not adopt alkali or organic solvent, be easy to environmental improvement.
Concrete treatment step of the present invention is as follows:
(1) preliminary treatment: with disabled lithium ion cell positive plate strip of sheet material crushing to being less than 5mm; Oven dry is less than 0.1% to containing water inventory.
(2) chlorination separates: will carry out the chlorination separating treatment directly into stove through broken, dry material; Treatment conditions are: 300 ~ 380 ℃ of temperature; Time 10 ~ 30min; Chlorine flowrate is by 1kg aluminium 0.14 ~ 0.42kg/min.Hot volatile matter is through cooling off to get aluminium chloride, or enters oxidizing process; Solid product is positive electrode active material, collects for further processing.
(3) aluminium oxide and chlorine reclaim: hot volatile matter gas reacts with the preheating purity oxygen directly into oxidation reactor.Process condition: 250 ~ 350 ℃ of volatile matter temperature; 300 ~ 400 ℃ of preheated oxygen temperature; Oxygen flow is by 1kg aluminium 0.030 ~ 0.092kg/min; 300 ~ 400 ℃ of oxidizing temperatures, the chlorination in this step of time 10 ~ 30min(and (2) step separates synchronously to be carried out).Fluid-mixing gets ultra-fine alumina and chlorine through gathering dust, purifying; Chlorine, returns for chlorination process except behind the oxygen through red-hot carbon granules.
The present invention has following advantage and good effect: the process route of technique of the present invention is short, good separating effect, and the aluminium salt yield of gained is high; Adopt the lower temperature process, equipment and not harsh with material, energy consumption is low simultaneously.
Take full advantage of the waste heat of volatile matter, adopt preheated oxygen to carry out the oxidizing process of aluminium chloride, do not use the reactor with thermal source; Reactor has larger washability.
Not only can prepare ultra-fine alumina, the chlorine of regenerating simultaneously; Adopt the pure oxygen raw material, process waste material and obtain the high added value aluminium oxide, reach separating of aluminium and active material in the waste lithium ion cell anode sheet.
Rationalization's operation takes full advantage of heat energy; The process program heat utilization rate is high.
Embodiment:
Below in conjunction with implementation the present invention is described further.The discarded based lithium-ion battery positive plate material that adopts contains aluminium 10.7%; Sheet material is crushed to is less than 5mm, dry to water content and be lower than 0.1%, as the spent material among the following embodiment.
Embodiment 1
The disabled lithium ion cell positive plate of drying is directly added the chlorination reaction stove continuously through the tubular type screw feeder, regenerate 360 ~ 370 ℃ of chlorine temperatures of the deoxidation that enters chlorination furnace, temperature was 360 ~ 380 ℃ when chlorination reaction was carried out; Material reaction (stopping in the stove) time 10min; By discharging spiral organ continuous discharge.Enter 380 ~ 400 ℃ of the preheated oxygen temperature, flow 0.090 ~ 0.092kg/min(of oxidator by reinforced 1.0kg/min aluminium), temperature was about 360 ~ 390 ℃ when oxidation reaction was carried out.Oxidation reaction product is collected ultra-fine alumina through dust-precipitator, and gas removes oxygen through degasifier, 380 ~ 400 ℃ of degasifier carbon-coating temperature, the about 2min of deoxidation; In the material processing procedure, deoxidation chlorine is all sent into the chlorination reaction stove, and presses flow 0.02 ~ 0.03kg/min and replenish chlorine.
The clearance 97.4% of aluminium in the disabled lithium ion cell positive plate, aluminium oxide (in aluminium) yield 91.1%.
Embodiment 2
The disabled lithium ion cell positive plate of drying is directly added the chlorination reaction stove continuously through the tubular type screw feeder, regenerate 310 ~ 330 ℃ of chlorine temperatures of the deoxidation that enters chlorination furnace, temperature was about 300 ~ 330 ℃ when chlorination reaction was carried out; Material reaction (stopping in the stove) time 30min; By discharging spiral organ continuous discharge.Enter 300 ~ 320 ℃ of the preheated oxygen temperature, flow 0.030 ~ 0.031kg/min(of oxidator by reinforced 1.0kg/min aluminium), temperature was about 320 ~ 340 ℃ when oxidation reaction was carried out.Oxidation reaction product is collected ultra-fine alumina through dust-precipitator, and gas removes oxygen through degasifier, 300 ~ 330 ℃ of degasifier carbon-coating temperature, the about 6min of deoxidation; In the material processing procedure, deoxidation chlorine is all sent into the chlorination reaction stove, and presses flow 0.01 ~ 0.02kg/min and replenish chlorine.
The clearance 98.3% of aluminium in the disabled lithium ion cell positive plate, aluminium oxide (in aluminium) yield 95.2%.
Embodiment 3
The disabled lithium ion cell positive plate of drying is directly added the chlorination reaction stove continuously through the tubular type screw feeder, regenerate 330 ~ 350 ℃ of chlorine temperatures of the deoxidation that enters chlorination furnace, temperature was about 350 ~ 370 ℃ when chlorination reaction was carried out; Material reaction (stopping in the stove) time 25min; By discharging spiral organ continuous discharge.Enter 350 ~ 370 ℃ of the preheated oxygen temperature, flow 0.036 ~ 0.037kg/min(of oxidator by reinforced 1.0kg/min aluminium), temperature was about 340 ~ 370 ℃ when oxidation reaction was carried out.Oxidation reaction product is collected ultra-fine alumina through dust-precipitator, and gas removes oxygen through degasifier, 350 ~ 380 ℃ of degasifier carbon-coating temperature, the about 5min of deoxidation; In the material processing procedure, deoxidation chlorine is all sent into the chlorination reaction stove, and presses flow 0.02 ~ 0.03kg/min and replenish chlorine.
The clearance 98.6% of aluminium in the disabled lithium ion cell positive plate, aluminium oxide (in aluminium) yield 93.7%.
Embodiment 4
The disabled lithium ion cell positive plate of drying is directly added the chlorination reaction stove continuously through the tubular type screw feeder, enter 360 ~ 370 ℃ of the preheating chlorine gas temperature, flow 0.40 ~ 0.42kg/min(of chlorination furnace by reinforced 1.0kg/min aluminium), temperature was 360 ~ 380 ℃ when chlorination reaction was carried out; Material reaction (stopping in the stove) time 10min; Solid product is by discharging spiral organ continuous discharge.The gaseous product of chlorination reaction is collected aluminium chloride through cooling, dust-precipitator.
The clearance 97.6% of aluminium in the disabled lithium ion cell positive plate, aluminium chloride yield (in aluminium) 91.4%.
Embodiment 5
The disabled lithium ion cell positive plate of drying is directly added the chlorination reaction stove continuously through the tubular type screw feeder, the deoxidation that enters chlorination furnace is regenerated 310 ~ 330 ℃ of chlorine temperatures, flow 0.14 ~ 0.15kg/min(by reinforced 1.0kg/min aluminium), temperature was about 300 ~ 330 ℃ when chlorination reaction was carried out; Material reaction (stopping in the stove) time 30min; Solid product is by discharging spiral organ continuous discharge.The gaseous product of chlorination reaction is collected aluminium chloride through cooling, dust-precipitator.
The clearance 98.0% of aluminium in the disabled lithium ion cell positive plate, aluminium chloride (in aluminium) yield 95.1%.
Embodiment 6
The disabled lithium ion cell positive plate of drying is directly added the chlorination reaction stove continuously through the tubular type screw feeder, the deoxidation that enters chlorination furnace is regenerated 330 ~ 350 ℃ of chlorine temperatures, flow 0.20 ~ 0.21kg/min(by reinforced 1.0kg/min aluminium), temperature was about 350 ~ 370 ℃ when chlorination reaction was carried out; Material reaction (stopping in the stove) time 20min; Solid product is by discharging spiral organ continuous discharge.The gaseous product of chlorination reaction is collected aluminium chloride through cooling, dust-precipitator.
The clearance 98.5% of aluminium in the disabled lithium ion cell positive plate, aluminium oxide yield 93.4%.
Claims (10)
1. method of processing based lithium-ion battery positive plate isolating active thing and aluminium, it is characterized in that, after the fragmentation of disabled lithium ion cell positive plate process, drying, under 300 ~ 380 ℃ of temperature, pass into chlorine and carry out the chlorination separating treatment, obtain hot volatile matter and the solid product that contains positive electrode active material; The direct condensation of described hot volatile matter is obtained aluminium chloride, or carry out oxidation and obtain aluminium oxide.
2. method according to claim 1 is characterized in that, 1kg aluminium total chlorine gas amount 4.0 ~ 4.2kg is processed in control.
3. method according to claim 1 is characterized in that, chlorine flowrate is by 1kg aluminium 0.14 ~ 0.42kg/min.
4. each described method is characterized in that according to claim 1-3, and described hot volatile matter oxidation obtains alumina process and is: hot volatile matter gas is directly passed in the oxidation reactor, obtain aluminium oxide and chlorine with the reaction of preheating purity oxygen; Gained chlorine returns for the chlorination separating treatment after red-hot carbon granules removes oxygen.
5. method according to claim 4 is characterized in that, enters in the oxidation reactor 250 ~ 350 ℃ of hot volatile matter gas temperatures; Preheated oxygen temperature to 300 ~ 400 ℃.
6. method according to claim 4 is characterized in that, through gathering dust, purifying, gets aluminium oxide and chlorine from oxidation reactor fluid-mixing out.
7. method according to claim 4 is characterized in that, oxidizing process oxygen aluminum ratio: control is processed 1kg aluminium with total amount of oxygen 0.90 ~ 0.95kg.
8. method according to claim 4 is characterized in that, oxygen flow is by 1kg aluminium 0.030 ~ 0.092kg/min.
9. method according to claim 4 is characterized in that, except oxygen, 350 ~ 400 ℃ of carbon granules temperature are 2 ~ 6min in the red-hot carbon granules layer carbon-coating time of staying to the chlorine that oxidation reaction produces through red-hot carbon granules pull-up.
10. method according to claim 1 is characterized in that, (1) preliminary treatment: with disabled lithium ion cell positive plate strip of sheet material crushing to being less than 5mm; Oven dry is less than 0.1% to containing water inventory;
(2) chlorination separates: will carry out the chlorination separating treatment directly into stove through broken, dry material; Treatment conditions are: 300 ~ 380 ℃ of temperature; Time 10 ~ 30min; Chlorine flowrate is by 1kg aluminium 0.14 ~ 0.42kg/min; Hot volatile matter is through cooling off to get aluminium chloride, or enters oxidizing process; Solid product is positive electrode active material;
(3) aluminium oxide and chlorine reclaim: hot volatile matter gas reacts with the preheating purity oxygen directly into oxidation reactor; Wherein: 250 ~ 350 ℃ of hot volatile matter temperature; 300 ~ 400 ℃ of preheated oxygen temperature; Oxygen flow is by 1kg aluminium 0.030 ~ 0.092kg/min; 300 ~ 400 ℃ of oxidizing reaction temperatures, time 10 ~ 30min; Through gathering dust, purifying, get aluminium oxide and chlorine from oxidation reactor fluid-mixing out; Chlorine, returns for the chlorination separating treatment except behind the oxygen through red-hot carbon granules.
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| WO2024055549A1 (en) * | 2022-09-16 | 2024-03-21 | 广东邦普循环科技有限公司 | Method for recycling positive electrode material from scrapped positive electrode sheets by desorption and application |
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| WO2024055549A1 (en) * | 2022-09-16 | 2024-03-21 | 广东邦普循环科技有限公司 | Method for recycling positive electrode material from scrapped positive electrode sheets by desorption and application |
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| CN103066343B (en) | 2015-03-11 |
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