CN109818097A - A kind of technique of waste lithium cell solvent extraction processing electrolyte and binder - Google Patents
A kind of technique of waste lithium cell solvent extraction processing electrolyte and binder Download PDFInfo
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- CN109818097A CN109818097A CN201811481815.0A CN201811481815A CN109818097A CN 109818097 A CN109818097 A CN 109818097A CN 201811481815 A CN201811481815 A CN 201811481815A CN 109818097 A CN109818097 A CN 109818097A
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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
A kind of technique of waste lithium cell solvent extraction processing electrolyte and binder, belongs to lithium battery recovery technology field.The following steps are included: (1) is crushed after pre-processing lithium ion battery;(2) broken material is extracted using organic solvent;(3) by material initial gross separation extracted, slurry and large granular materials are obtained;(4) the slurry solid-liquor separation for obtaining step (3) obtains black powder product and organic liquid;(5) the large granular materials solid-liquor separation for obtaining step (3), obtains solid bulky grain and organic liquid;(6) organic liquid for obtaining step (4) and step (5) is fractionated, and organic solvent, electrolyte, binder and lithium salts is separately recovered, and organic solvent return step (2) is recycled.The present invention not only eliminates waste and old ion battery electrolyte and binder, and aluminium foil/copper foil of positive and negative pole material and attachment is also made to fall off, and solves active material in waste lithium cell recycling and is difficult to the technical problem removed.
Description
Technical field
The invention belongs to lithium battery recovery technology fields, are related to a kind of processing method of lithium battery, in particular to a kind of to return
Receive the method for disposing of lithium battery of electrolyte and binder.
Background technique
Lithium battery because its voltage is high, capacity is big, it is at low cost, have a safety feature, service life length, memory-less effect, environmental-friendly
Equal remarkable advantages, and it is widely used in the fields such as electronics, traffic.With the popularization to new-energy automobile, China's lithium ion
The yield of power battery keeps staggering growth situation.Currently, the power battery service life is essentially 1000-2000 charge and discharge, press
This cycle life calculates, and a large amount of lithium ion battery is faced with the problem of scrapping processing after using 3-8.Although to lithium from
The recycling of sub- old and useless battery starts gradually to draw attention, but the focus recycled concentrates on the recycling of electrode material valuable metal, and
Processing and recycling to electrolyte and binder simultaneously think little of.In the collection, stacking and removal process of waste and old lithium ion battery,
Electrolyte leakage and volatilization, cause serious pollution for atmosphere, soil and the water body to periphery.
Contain electrolyte lithium hexafluoro phosphate, organic solvent and additive, and hexafluorophosphoric acid in the electrolyte of waste lithium cell
Lithium easily reacts generation with water, gas is toxic and corrosivity very Datong District when electrolyte in organic solvent it is readily volatilized, flash-point is low, easily
Burning.Easily cause the safety issues such as burning, explosion during battery is disassembled and recycled, and the flue gas that is generated in recycling or
Waste water is very big to the pollution of environment.In lithium battery green reclaim technology, before carrying out recycling or harmless treatment to electrolyte,
It need to be by electrolyte centralized collection remaining in battery.Currently, carrying out recycling receipts to electrolyte in waste and old lithium ion battery both at home and abroad
The research of collection is less, and reason is that electrolyte content is few and recycling is difficult, and when electrolyte and pole piece infiltrate, it is less easily separated.
Before dismantling, electrolyte does not collect generally old and useless battery at present, but it is directly burned with old and useless battery, makes residual
It stays electrolyte gasification discharge either directly to crush waste lithium cell, is mixed into entrained electrolyte in solid material, through subsequent place
Comprehend and is emitted in the form of waste liquid.The above method does not carry out concentration receipts to electrolyte during battery is disassembled
Collection, causes atmosphere and water quality by serious pollution, increases the processing pressure of subsequent exhaust gas waste water.
Existing lithium ion battery adhesive treatment technology is mainly using the processing method of thermal decomposition, in heat treatment process
In, lithium salts, which decomposes, generates a large amount of acid+hydrofluoric acid, and sour strong corrosive is to corrosion reclaimer, the high requirements on the equipment, simultaneously
Tail gas absorption waste liquid pollutes the environment, and it is also cumbersome to deal with process, at high cost.
Summary of the invention
The purpose of the present invention is overcoming above-mentioned the deficiencies in the prior art, a kind of waste lithium cell solvent extraction processing electricity is provided
The technique for solving liquid and binder.The purpose of the present invention is achieved through the following technical solutions.
A kind of technique of waste lithium cell solvent extraction processing electrolyte and binder, which is characterized in that including following step
It is rapid:
(1) it is crushed after pre-processing lithium ion battery;
(2) broken material is extracted using organic solvent;
(3) by material initial gross separation extracted, slurry and shedding large granular materials are obtained;
(4) the slurry solid-liquor separation for obtaining step (3) obtains black powder product and organic liquid;
(5) the shedding large granular materials solid-liquor separation for obtaining step (3), obtains solid shedding bulky grain and organic liquor
Body;
(6) organic liquid for obtaining step (4) and step (5) is fractionated, and organic solvent, electrolyte, bonding is separately recovered
Agent and lithium salts, organic solvent return step (2) are recycled.
Pretreatment described in step (1) is to recycle the conventional pretreatment operation of lithium battery, including discharge, dry after cleaning,
Remove oil, water, circuit board, the band large-scale metal component on battery or mould group surface.
In some specific embodiments, step (2) organic solvent is PC (polycarbonate), EC (ethylene carbonate
Ester), DMC (dimethyl carbonate), EMC (methyl ethyl carbonate), NMP (N-Methyl pyrrolidone), DMAc (dimethyl acetamide),
One or more of DMF (n,N-Dimethylformamide), TEP (triethyl phosphate) and DMSO (dimethyl sulfoxide).
In some specific embodiments, being crushed for step (1) carries out in protective atmosphere, broken to divide coarse crushing and fine crushing
Two steps, coarse crushing make material size in 50mm hereinafter, fine crushing make material size in 15mm or less.Further, coarse crushing uses
Equipment be selected from one or more of cyclopentane gas detector, single-shaft shredder, rotary knife crusher and hammer mill, use fine crushing
Equipment be selected from one or more of hammer knife crusher, heavy duty granulator, vertical roller pulverizer and vertical shaft crusher.
In some specific embodiments, the extraction series of step (2) is 1-20 grades.
In some specific embodiments, cyclone classification, vibrating screen panel classification or spiral shell are initially separated into described in step (3)
Rotation classification.
In some specific embodiments, solid-liquor separation described in step (4) and step (5) includes centrifugation, filtering and bears
Pressure drying.Filtering and centrifugation apparatus can be various centrifuge, various filter press, bag filter, various membrane filter, various vacuum mistake
One or more of filter etc..
In some specific embodiments, further includes:
The solid particle that step (7) obtains step (5) sorts, and assorting room is magnetic separation, vortex magnetic separation, gravity treatment, flotation
One or more of, obtain steel, stainless steel, plastics, diaphragm, copper and aluminium.
In some specific embodiments, further includes:
The electrolyte and lithium salt component that step (8) analytical procedure (6) obtains, according to lithium-ion battery electrolytes composition proportion
Electrolysis liquid product is made in electrolyte and lithium salts.
In some specific embodiments, pretreatment described in step (1) includes first by lithium battery in conducting solution
0.5-4h is impregnated, the conducting solution is the aqueous solution of sodium chloride, potassium chloride, sodium sulphate, potassium sulfate or sodium nitrate, solution quality
Concentration is 5%-15%.
The technique of a kind of waste lithium cell solvent extraction processing electrolyte and binder provided by the invention, no high temperature, nothing
Poisonous and harmful corrosive gas generates, emission-free processing equipment, the method solve in waste lithium cell removal process electrolyte with
The problem of the removing and recycling of binder, the used solvent extraction technology of the present invention extract electrolyte and bonding in lithium battery
Agent, equipment is simple, works well, and compared with prior art, the present invention is not only stripped of electrolyte and binder, also makes positive and negative anodes
Material and aluminium foil/copper foil of attachment fall off, and solve active material in waste lithium cell recycling and are difficult to the technical problem removed.
Detailed description of the invention
Fig. 1 is the process flow of a kind of waste lithium cell solvent extraction processing electrolyte and binder provided by the invention
Figure.
Specific embodiment
The following further describes the present invention with reference to the drawings.If without specified otherwise, employed in the embodiment of the present invention
Raw material be raw material commonly used in the art, method employed in embodiment is the conventional method of this field.
Embodiment 1:
(1) pre-process: waste lithium cell monomer or lithium battery mould group are through 5% aqueous sodium persulfate solution immersion 10h discharge operation
Afterwards, through water spray rinsing maching washing, 60 DEG C of thermostatic hot-air drying machines are dry, manual demolition battery modules circuit board and band large-scale metal structure
Part.
(2) be crushed: lithium battery after pretreatment carries out crushing operation, and crusher seals and nitrogen charging gas shielded, level-one are thick
Broken machine uses cyclopentane gas detector, and installed power 90kw, treating capacity 1000-3000kg/h, the shredder structure is simple, processing capacity
Greatly, feed inlet can directly handle greatly big-and-middle pattern group.Second level is fine crushing to use rotary knife crusher, installed power 150kw, treating capacity
1500-5000kg/h, the machine can effectively cut separation of material, and outlet material diameter is in 10-15mm or less.
(3) extract: organic solvent uses 50%NMP+50%DMC, and temperature 60 C extracts mixing time 1.5-2h, uses
Special 5 with strainer cubic metre conical bottom tank strong mixing slot, bottom screen 50-100 mesh, stirred tank are 316 stainless steel materials, slot
Sub- side wall can increase storeroom with spoiler, the double-deck contrarotating agitating paddle, power of agitator 18kw, all-sealed structure, the slot
Phase mutual friction, keep positive and negative anodes active material more easy to fall off in the extraction process of organic solvent, the material to fall off is by bottom
Mesh screen enters cone bottom, and the setting of cone bottom exports and pump, after pump and connects vortrap, fine grained is collected after separation, organic solvent
It squeezes into slot and continues cycling through from slot inner top.
(4) it separates: after organic extraction, solid-liquor separation being carried out to the black powder and shedding material that are obtained, black powder is using after dense
Centrifugation, black powder centrifugation use hermetic type tripod pendulum type batch centrifugal, 0.5h are centrifuged at 3000 turns, and shedding material enters after using filtering
Basket centrifuges are centrifuged, centrifugation time 1h, and black powder and shedding material are respectively fed to negative pressure drying room and carry out constant temperature baking after solid-liquor separation
It is dry, it 120-150 DEG C of drying temperature, recycles organic steam and is recycled after condensing.
(5) sort: shedding material enters multistage continuous sorting machine and is sorted, according to the property of shedding material, wherein steel
Iron uses magnetic separation, and stainless steel uses strong eddy current magnetic separation, and diaphragm uses selection by winnowing, and plastics use gravity treatment, and the separation of copper aluminium foil is using weight
Choosing etc., isolates steel, stainless steel, diaphragm, plastics, copper and aluminium step by step.
(6) be fractionated: repeatedly the spent organic solvent after carries out negative pressure fractionation operation, and cut point is 80-200 DEG C, point
It Hui Shou not organic solvent constituent, electrolyte component, binder component and lithium salts.
Embodiment 2:
The other conditions of recovery test are identical as embodiment in the present embodiment, the difference is that middle organic solvent is 60%
DMF+20%DMC+20%EMC, temperature are 50-60 DEG C, extraction time 1.5h.
Embodiment 3
The other conditions of recovery test are identical as embodiment in the present embodiment, the difference is that middle organic solvent is carbon
30%DMF+30%NMP+20%DMC+20%EMC, extraction temperature are 40-70 DEG C, extraction time 1-1.5h.
Embodiment 3
The other conditions of recovery test are identical as embodiment in the present embodiment, use the difference is that it extracts stirred tank
Normal agitation slot, extracts mixing time 3-4h, and mixture separation uses multiple tracks cylinder super-screenout, sifts out shedding material and black respectively
Powder.
Embodiment 4
The other conditions of recovery test are identical as embodiment in the present embodiment, the difference is that the separation of black powder uses certainly
Dynamic discharging plate and frame filter press, is directly dried after black slurry material filters pressing.
The invention patent is not limited to the above embodiment, using stream same as or similar to the above embodiments of the present invention
Journey, and other obtained techniques, within the scope of protection of the patent of the invention.
Claims (10)
1. a kind of technique of waste lithium cell solvent extraction processing electrolyte and binder, which comprises the following steps:
(1) it is crushed after pre-processing lithium ion battery;
(2) broken material is extracted using organic solvent;
(3) by material initial gross separation extracted, slurry and large granular materials are obtained;
(4) the slurry solid-liquor separation for obtaining step (3) obtains black powder product and organic liquid;
(5) the large granular materials solid-liquor separation for obtaining step (3), obtains solid bulky grain and organic liquid;
(6) organic liquid obtained step (4) and step (5) is fractionated, be separately recovered organic solvent, electrolyte, binder and
Lithium salts, organic solvent return step (2) are recycled.
2. technique as described in claim 1, which is characterized in that step (2) organic solvent be PC, EC, DMC, EMC,
One or more of NMP, DMAc, DMF, TEP and DMSO.
3. technique as claimed in claim 1 or 2, which is characterized in that being crushed for step (1) carries out in protective atmosphere, breaks
Broken point of coarse crushing and two steps fine crushing, coarse crushing make material size in 50mm hereinafter, fine crushing make material size in 15mm or less.
4. technique as claimed in claim 3, which is characterized in that the equipment that coarse crushing uses is selected from cyclopentane gas detector, single shaft is torn up
One or more of machine, rotary knife crusher and hammer mill, the equipment fine crushing used are selected from hammer knife crusher, heavy type granulating
One or more of machine, vertical roller pulverizer and vertical shaft crusher.
5. technique as claimed in claim 1 or 2, which is characterized in that the extraction series of step (2) is 1-20 grades.
6. technique as claimed in claim 1 or 2, which is characterized in that be initially separated into cyclone classification, shake described in step (3)
Dynamic screen fractionation or screw classifying.
7. technique as claimed in claim 1 or 2, which is characterized in that solid-liquor separation described in step (4) and step (5) includes
Centrifugation, filtering and negative pressure drying.
8. technique as claimed in claim 1 or 2, which is characterized in that further include:
The solid particle that step (7) obtains step (5) sorts, assorting room be magnetic separation, vortex magnetic separation, gravity treatment, in flotation
One or more obtain steel, stainless steel, plastics, diaphragm, copper and aluminium.
9. technique as claimed in claim 1 or 2, which is characterized in that further include:
The electrolyte and lithium salt component that step (8) analytical procedure (6) obtains are electrolysed according to lithium-ion battery electrolytes composition proportion
Electrolysis liquid product is made in liquid and lithium salts.
10. technique as claimed in claim 1 or 2, which is characterized in that pretreatment described in step (1) includes first by lithium electricity
0.5-4h is impregnated in pond in conducting solution, and the conducting solution is sodium chloride, potassium chloride, sodium sulphate, potassium sulfate or sodium nitrate
Aqueous solution, concentration of polymer solution 5%-15%.
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Cited By (8)
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CN110635191A (en) * | 2019-09-12 | 2019-12-31 | 金川集团股份有限公司 | Method for cleanly recovering all components of waste power lithium battery |
CN110649344A (en) * | 2019-09-12 | 2020-01-03 | 金川集团股份有限公司 | Method for separating and recycling electrolyte in waste power lithium battery by using ultrasonic enhanced extraction method |
CN111525209A (en) * | 2020-04-30 | 2020-08-11 | 北矿机电科技有限责任公司 | Recovery method of power lithium battery |
CN112604800A (en) * | 2020-11-29 | 2021-04-06 | 连云港中再钢铁炉料有限公司 | Processing technology of scrap steel shredder |
CN112845515A (en) * | 2020-12-30 | 2021-05-28 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Method for treating pyrolysis flue gas of solid waste |
CN113690501A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Recycling process of battery pole piece without pickling |
CN117650306A (en) * | 2024-01-30 | 2024-03-05 | 河南工学院 | Metal extraction and separation device in waste lithium iron phosphate battery |
CN117650306B (en) * | 2024-01-30 | 2024-04-12 | 河南工学院 | Metal extraction and separation device in waste lithium iron phosphate battery |
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CN110635191A (en) * | 2019-09-12 | 2019-12-31 | 金川集团股份有限公司 | Method for cleanly recovering all components of waste power lithium battery |
CN110649344A (en) * | 2019-09-12 | 2020-01-03 | 金川集团股份有限公司 | Method for separating and recycling electrolyte in waste power lithium battery by using ultrasonic enhanced extraction method |
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CN112845515A (en) * | 2020-12-30 | 2021-05-28 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Method for treating pyrolysis flue gas of solid waste |
CN113690501A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Recycling process of battery pole piece without pickling |
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CN117650306A (en) * | 2024-01-30 | 2024-03-05 | 河南工学院 | Metal extraction and separation device in waste lithium iron phosphate battery |
CN117650306B (en) * | 2024-01-30 | 2024-04-12 | 河南工学院 | Metal extraction and separation device in waste lithium iron phosphate battery |
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Application publication date: 20190528 |