CN107464963A - A kind of method that valuable material is efficiently separated from waste lithium cell - Google Patents
A kind of method that valuable material is efficiently separated from waste lithium cell Download PDFInfo
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- CN107464963A CN107464963A CN201710626490.XA CN201710626490A CN107464963A CN 107464963 A CN107464963 A CN 107464963A CN 201710626490 A CN201710626490 A CN 201710626490A CN 107464963 A CN107464963 A CN 107464963A
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- lithium cell
- waste lithium
- efficiently separated
- flotation
- valuable material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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
The present invention discloses a kind of method that valuable material is efficiently separated from waste lithium cell, and it includes step：Waste lithium cell is classified according to model difference, discharge process is carried out in discharge equipment, disassembles to obtain internal battery core and outsourcing aluminum hull；Battery core adds organic solvent immersion filtering oil removing through broken；Add water stirring and standing separation barrier film；Filter powder is through wet ball-milling and is diluted with water carry out flotation, isolates high purity graphite, aluminium powder；Change pulp density and flotation conditions carry out secondary flotation, can obtain flotation upper strata positive mix, flotation lower floor copper powder.The characteristics of separation method of the present invention is simple, energy consumption is low, environmental pollution is small, production low intensity, and each valuable material is efficiently separated in old and useless battery, good separating effect, and the rate of recovery is high, has preferable productivity effect.
Description
Technical field
The present invention relates to waste lithium cell recycling field, is specifically that one kind efficiently separates valuable material from waste lithium cell
Method.
Background technology
The recyclable part of waste and old lithium ion battery mainly includes positive electrode, negative material, electrolyte, barrier film, shell, cover plate
Deng.Its positive pole is typically with lithium base inlaid scheme LixMyXz（M is common for nickel, cobalt, manganese, vanadium, iron etc.）, PVDF, aluminium foil be main base
Raw material；Negative material generally comprises graphite, adhesive and copper foil etc.；Electrolyte is usually with LiPF6Based on conducting salt, with
Mixed solvent system based on EC, PC, DMC, EMC；Barrier film is generally polyethylene, microporous polypropylene membrane and propylene and ethene
Copolymer, Natene etc.；Shell is generally aluminum material；Cover plate generally comprises both positive and negative polarity lappet, packing ring, top layer
Deng.Because lithium battery species is more, its lattice of being established rules when producing, material, size, electrical property difference are larger, but due to its electrification
Learn that mechanism is similar, and its manufacturing process, raw material, auxiliary material are close, it is different simply doping metals, solvent burden ratio, material filling with
And it is otherwise varied on various modifying agent, this provides possibility to efficiently separate each valuable material from waste lithium cell.
As the application of lithium battery obtains development at full speed, it scraps the separation and recovery of rear valuable material, will turn into important
Technical problem.Separated and handled for waste lithium cell, most of at present patent and manufacturers both at home and abroad all use
Rear roasting direct is simply disassembled, makes organic matter volatilization or high-temperature decomposition reaction occurs, such method can produce substantial amounts of poisonous
Pernicious gas, simultaneously because the presence of hydrogen fluoride, high requirement is proposed to follow-up air flue equipment and handling process.How will
The valuable materials such as waste lithium cell outsourcing aluminum hull, cover plate, organic matter reagent, barrier film, positive mix, negative pole graphite, copper foil, aluminium foil
Efficiently separated, considerable influence will be produced to its subsequent technique.
The content of the invention
The defects of it is an object of the invention to overcome prior art to exist, there is provided one kind efficiently separates from waste lithium cell
The method of valuable material.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method that valuable material is efficiently separated from waste lithium cell, specifically includes following steps：
（1）Physics discharges：Waste lithium cell is classified according to model difference, discharge process is carried out in discharge equipment, extremely
Voltage reduces to below 0.5V；
（2）Disassemble：To step（1）Gained has discharged lithium battery, is cut under sealing and circulating flow conditions, cut surface is covering
Plate 1~3cm backward, obtains internal battery core and outsourcing aluminum hull after disassembling；
（3）It is closed broken：To step（2）Gained battery core, break process is carried out under sealing and circulating flow conditions, crush the time 2
~10min, 5~20mm of particle size after cracking, disassemble with it is broken when spillage enter overflow launder, the liquefaction of volatile organic matter gas cooling,
Collected；
（4）Immersion dissolving：By step（3）Gained particle, add organic solvent and carry out immersion treatment, positive mix, negative pole graphite
It is able to come off from pole plate, filters, obtain 1# mixed powders；The control of organic solvent addition is in solid-to-liquid ratio 1 in waste lithium cell:
0.5~3,15~40 DEG C of soaking temperature, 1~2h of soak time；
（5）Stand membrane removal：By step（4）Gained 1# mixed powders, add water to stir and stand, and filter to obtain 2# mixed powders；
（6）Wet ball-milling：By step（5）Gained 2# mixed powders, are fitted into ball mill and are ground, enter abrasive grain≤
20mm, abrasive concentration 25~50%, 20~50r/min of mill speed, 0.5~1h of abrasive material time, go out abrasive particle degree≤0.25mm；
（7）1# flotation：By step（6）Gained ball milling powder adds pH adjusting agent control slurry by pulp density 10~20% plus water
PH=6~7,20~40 DEG C, 3~10min of inflationtime of slurry temperature, scrape and steep 10~20min of time, regulator A dosages 5000~
8000g/t, collecting agent A 100~800g/t of dosage, 50~200g/t of frother dosages, carry out selected twice floating of roughing three times
Mode is selected, ball milling powder is isolated high purity graphite, aluminium powder, obtains 3# mixed powders；
（8）2# flotation：By step（7）Gained 3# mixed powders add pH adjusting agent control material by pulp density 10~15% plus water
PH=5~6.5 are starched, 25~40 DEG C, 5~10min of inflationtime of slurry temperature, scrape bubble 8~10min of time, regulator B dosages
8000~10000g/t, collecting agent B 200~300g/t of dosage, 300~500g/t of frother dosages, carry out roughing twice once
Selected flotation mode, isolates positive mix and copper powder.
Further scheme, the step（1）Middle -20~50 DEG C of discharge equipment operating temperature, discharge voltage adjustable range 0~
220V。
Further scheme, the step（2）With（3）Middle sealing and circulating air-flow is in nitrogen, argon gas, helium, carbon dioxide
One or more mixing.
Further scheme, the step（4）Middle organic solvent is styrene, tetrachloro-ethylene, trichloro ethylene, ethylene glycol
One or more mixing in ether, acetone, isopropanol, ethylene glycol monobutyl ether.
Further scheme, the step（6）Middle ball mill is horizontal tank abrading-ball grinding machine, conical ball mill or tubular type ball milling
Machine；Mill ball material used in ball mill is 201 stainless steels, 304 stainless steels or corundum.
Further scheme, the step（7）With（8）Middle pH adjusting agent is one in sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid
Kind or a variety of mixing.
Further scheme, the step（7）With（8）Middle foaming agent is in turpentine oil, 2# flotation oils, cresotinic acid, weight pyridine
One or more mixing.
Further scheme, the step（7）Middle regulator A is one or two kinds of mixing of starch, waterglass；Collecting agent A
For the one or more mixing in kerosene, diesel oil, xanthate, the acetic acid of cetyl two.
Further scheme, the step（8）Middle regulator B is one kind in lime, starch, waterglass, tannin, vulcanized sodium
Or a variety of mixing；Collecting agent B is one or more mixing in kerosene, light diesel, the acetic acid of cetyl two.
Compared with prior art, beneficial effects of the present invention：Waste lithium cell valuable material is separated step by step, technique
Flow is simple, equipment requirement is low, has abandoned and is calcined this committed step to waste lithium cell in the prior art, avoids waste gas dirt
Dye and loss of material；Disassembled and crushed under sealing and circulating air flow system, solved in waste lithium cell removal process
The secondary pollution problem of organic matter and inorganic salts；Each valuable material rate of recovery is good, separation purity is high, battery core contained by waste lithium cell
And aluminum hull, the rate of recovery is up to 99.8%, and the organic matter rate of recovery is up to 95%, and for the barrier film rate of recovery up to 98%, recycling graphite rate is reachable
98%（Purity 99.5%), aluminium powder and the copper powder rate of recovery are up to 99%（Purity 98%), the positive mix rate of recovery is up to 97.8%.
Brief description of the drawings
Fig. 1 is a kind of flow chart for the method that valuable material is efficiently separated from waste lithium cell of the present invention.
Embodiment
In order to illustrate more clearly of the purpose of the present invention, advantage, technical scheme, process route, with reference to embodiment and
Accompanying drawing, the present invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining this hair
It is bright, it is not as a limitation of the invention.
Embodiment 1
Waste lithium cell is classified according to model difference, in lithium battery discharge equipment, electricity is carried out to waste lithium cell
Test, and it is more than 0.5V lithium battery external load to voltage, it is connected by battery with resistance, using exothermic process to consume electricity
The electricity in pond, its single battery voltage is set to reduce to below 0.5V；Under the conditions of sealing and circulating nitrogen atmosphere, cut and torn open
Solution, cut surface obtain internal battery core and outsourcing aluminum hull, the rate of recovery up to 99.8%, pass through by battery core at the 3cm of cover plate end after disassembling
Closed broken, it is 20mm to crush particle mean size, disassemble with it is broken when spillage enter overflow launder, volatile organic matter cooling gaseous fluid
Change, particle presses solid-to-liquid ratio 1:3 add tetrachloro-ethylene, 2h are soaked under the conditions of 15 DEG C, positive mix, negative pole graphite are able to from pole plate
On come off, organic reagent is dissolved in organic phase and separated, the 1# mixed powders after oil removing, by solid-to-liquid ratio 1:2 add water
Stir and stand, be directly separated on the barrier film floating water surface, electrolyte lithium salt, lithium based additive and water react in refuse battery, are formed
Aqueous phase containing lithium, by filtering, reach separation of solid and liquid；2# mixed powders are put into XMQ-67 type conical ball mills, abrasive concentration
25%, drum's speed of rotation 20r/min, 30min is ground, discharging wet screening is crossed 60 mesh sieves, is diluted with water, and controls pulp density
10%, addition salt acid for adjusting pH=6,40 DEG C of slurry temperature, kerosene 800g/t, 2# flotation oil mass 50g/t, starch 5000g/t, three times
Roughing inflation 3min, bubble 8min is scraped, be recycled the graphite of rate 98.1%（Purity 99.7%）, twice selected inflation 5min, scrape bubble
20min, it is recycled the aluminium powder of rate 99.3%（Purity 98.1%）；The gained 3# mixed powders after 1# flotation, adjustment slurry are dense
Degree 15%, add salt acid for adjusting pH=5.0,25 DEG C of slurry temperature, light diesel 300g/t, 2# flotation oil mass 300g/t, starch
8000g/t, lime 2000g/t, inflation 5min, bubble 8min is scraped, flotation upper strata obtains the positive mix rate of recovery 97.8%, and lower floor is
Copper powder, the rate of recovery 99%（Purity 98.4%）.
Embodiment 2
By waste lithium cell（Model：18650）, in lithium battery discharge equipment, electric quantity test is carried out to waste lithium cell, and it is right
Voltage is more than 0.5V lithium battery external load, is connected by battery with resistance, using exothermic process to consume the electricity of battery,
Its voltage is reduced to below 0.5V, under the conditions of sealing and circulating helium atmosphere, cut and disassembled, cut surface is at cover plate end
At 1cm, internal battery core and outsourcing aluminum hull are obtained after disassembling, battery core is by closed broken, and it is 5mm to crush particle mean size, and particle is pressed
Solid-to-liquid ratio 1:0.5 adds styrene, 1h is soaked under the conditions of 40 DEG C, positive mix, negative pole graphite are able to come off from pole plate, had
Machine reagent, which is dissolved in organic phase, to be separated, the 1# mixed powders after oil removing, by solid-to-liquid ratio 1:2 plus water stirring and it is quiet
To put, be directly separated on the barrier film floating water surface, electrolyte lithium salt, lithium based additive and water react in refuse battery, form aqueous phase containing lithium,
By filtering, reach separation of solid and liquid；2# mixed powders are put into horizontal tank abrading-ball grinding machine, abrasive concentration 50%, drum's speed of rotation
50r/min, 1h being ground, discharging wet screening is crossed 60 mesh sieves, is diluted with water, control pulp density 20%, addition sulphur acid for adjusting pH=
7,20 DEG C of slurry temperature, diesel oil 100 g/t, 2#Flotation oil mass 200g/t, waterglass 8000g/t, inflation 5min, bubble 10min is scraped,
It is recycled the graphite of rate 98.5%（Purity 99.6%）, the aluminium powder of the rate of recovery 99.1%（Purity 98.4%）, the institute after 1# flotation
3# mixed powders are obtained, adjust pulp density 20%, add sulphur acid for adjusting pH=6.5,40 DEG C, kerosene 50g/t of slurry temperature, lightweight bavin
Oily 200g/t, 2#Flotation oil mass 500 g/t, starch 10000g/t, inflation 10min, bubble 10min is scraped, flotation upper strata obtains positive pole
The powder rate of recovery 97.4%, lower floor are copper powder, the rate of recovery 99.3%（Purity 98.7%）.
Embodiment 3
By waste lithium cell（Model：20100140）, in lithium battery discharge equipment, electric quantity test is carried out to waste lithium cell,
And it is more than 0.5V lithium battery external load to voltage, it is connected by battery with resistance, using exothermic process to consume battery
Electricity, its voltage is reduced to below 0.5V, under the conditions of sealing and circulating nitrogen atmosphere, cut and disassembled, cut surface exists
At the 2cm of cover plate end, internal battery core and outsourcing aluminum hull are obtained after disassembling, for battery core by closed broken, it is 20mm to crush particle mean size,
Particle presses solid-to-liquid ratio 1:3 add styrene, 1.5h are soaked under the conditions of 30 DEG C, organic reagent, which is dissolved in organic phase, to be divided
From the 1# mixed powders after oil removing, by solid-to-liquid ratio 1:2 add water to stir and stand, and are directly separated, give up on the barrier film floating water surface
Electrolyte lithium salt, lithium based additive and water react in battery, form aqueous phase containing lithium, by filtering, reach separation of solid and liquid；2# is mixed
Powder is put into XMQ-67 type conical ball mills, abrasive concentration 30%, drum's speed of rotation 50r/min, grinds 1h, discharging wet type sieve
Divide 60 mesh sieves, be diluted with water, and controlled pulp density 20%, and add phosphorus acid for adjusting pH=6.8,30 DEG C of slurry temperature, kerosene 150
G/t, 2#Flotation oil mass 200g/t, starch 6000g/t, inflation 5min, bubble 10min is scraped, be recycled the graphite of rate 98.5%（It is pure
Degree 99.5%）, the aluminium powder of the rate of recovery 99.1%（Purity 98.4%）, the gained 3# mixed powders after 1# flotation, adjust pulp density
10%, add phosphorus acid for adjusting pH=6.2,40 DEG C, light diesel 50g/t, turpentine oil mass 450g/t of slurry temperature, soluble starch
8500g/t, inflation 5min, bubble 10min is scraped, flotation upper strata obtains the positive mix rate of recovery 97.8%, and lower floor is copper powder, the rate of recovery
99%（Purity 98.1%）.
Claims (9)
- A kind of 1. method that valuable material is efficiently separated from waste lithium cell, it is characterised in that specifically include following steps：（1）Physics discharges：Waste lithium cell is classified according to model difference, discharge process is carried out in discharge equipment, extremely Voltage reduces to below 0.5V；（2）Disassemble：To step（1）Gained has discharged lithium battery, is cut under sealing and circulating flow conditions, cut surface is covering Plate 1~3cm backward, obtains internal battery core and outsourcing aluminum hull after disassembling；（3）It is closed broken：To step（2）Gained battery core, break process is carried out under sealing and circulating flow conditions, crush the time 2 ~10min, 5~20mm of particle size after cracking, disassemble with it is broken when spillage enter overflow launder, the liquefaction of volatile organic matter gas cooling, Collected；（4）Immersion dissolving：By step（3）Gained particle, add organic solvent and carry out immersion treatment, positive mix, negative pole graphite It is able to come off from pole plate, filters, obtain 1# mixed powders；The control of organic solvent addition is in solid-to-liquid ratio 1 in waste lithium cell: 0.5~3,15~40 DEG C of soaking temperature, 1~2h of soak time；（5）Stand membrane removal：By step（4）Gained 1# mixed powders, add water to stir and stand, and filter to obtain 2# mixed powders；（6）Wet ball-milling：By step（5）Gained 2# mixed powders, are fitted into ball mill and are ground, enter abrasive grain≤ 20mm, abrasive concentration 25~50%, 20~50r/min of mill speed, 0.5~1h of abrasive material time, go out abrasive particle degree≤0.25mm；（7）1# flotation：By step（6）Gained ball milling powder adds pH adjusting agent control slurry by pulp density 10~20% plus water PH=6~7,20~40 DEG C, 3~10min of inflationtime of slurry temperature, scrape and steep 10~20min of time, regulator A dosages 5000~ 8000g/t, collecting agent A 100~800g/t of dosage, 50~200g/t of frother dosages, carry out selected twice floating of roughing three times Mode is selected, ball milling powder is isolated high purity graphite, aluminium powder, obtains 3# mixed powders；（8）2# flotation：By step（7）Gained 3# mixed powders add pH adjusting agent control material by pulp density 10~15% plus water PH=5~6.5 are starched, 25~40 DEG C, 5~10min of inflationtime of slurry temperature, scrape bubble 8~10min of time, regulator B dosages 8000~10000g/t, collecting agent B 200~300g/t of dosage, 300~500g/t of frother dosages, carry out roughing twice once Selected flotation mode, isolates positive mix and copper powder.
- A kind of 2. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（1）Middle -20~50 DEG C of discharge equipment operating temperature, 0~220V of discharge voltage adjustable range.
- A kind of 3. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（2）With（3）Middle sealing and circulating air-flow is one or more mixing in nitrogen, argon gas, helium, carbon dioxide.
- A kind of 4. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（4）Middle organic solvent is styrene, tetrachloro-ethylene, trichloro ethylene, ethylene glycol ether, acetone, isopropanol, second two One or more mixing in alcohol monobutyl ether.
- A kind of 5. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（6）Middle ball mill is horizontal tank abrading-ball grinding machine, conical ball mill or tube mill；Mill ball material used in ball mill Matter is 201 stainless steels, 304 stainless steels or corundum.
- A kind of 6. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（7）With（8）Middle pH adjusting agent is one or more mixing in sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid.
- A kind of 7. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（7）With（8）Middle foaming agent is one or more mixing in turpentine oil, 2# flotation oils, cresotinic acid, weight pyridine.
- A kind of 8. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（7）Middle regulator A is one or two kinds of mixing of starch, waterglass；Collecting agent A is kerosene, diesel oil, xanthate, ten One or more mixing in the acetic acid of six alkyl two.
- A kind of 9. method that valuable material is efficiently separated from waste lithium cell according to claim 1, it is characterised in that The step（8）Middle regulator B is one or more mixing in lime, starch, waterglass, tannin, vulcanized sodium；Collecting agent B For the one or more mixing in kerosene, light diesel, the acetic acid of cetyl two.
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| CN108550940A (en) * | 2018-04-25 | 2018-09-18 | 河南师范大学 | The resource utilization reuse method of waste and old lithium ion battery lithium iron phosphate positive material |
| CN108767353A (en) * | 2018-05-25 | 2018-11-06 | 北京矿冶科技集团有限公司 | The method for producing rich lithium net liquid from waste lithium ion cell anode active material |
| CN109713394A (en) * | 2019-01-18 | 2019-05-03 | 中国矿业大学 | A method of separating cobalt acid lithium and graphite in discarded electrode material |
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| CN111484008A (en) * | 2020-04-16 | 2020-08-04 | 中国恩菲工程技术有限公司 | Composite regulator for graphite flotation in waste lithium ion batteries and recovery method of graphite in waste lithium ion batteries |
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