CN108550942A - A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent - Google Patents
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent Download PDFInfo
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- CN108550942A CN108550942A CN201810489125.3A CN201810489125A CN108550942A CN 108550942 A CN108550942 A CN 108550942A CN 201810489125 A CN201810489125 A CN 201810489125A CN 108550942 A CN108550942 A CN 108550942A
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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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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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
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Abstract
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent, the pre-burning in resistance furnace by waste and old lithium ion battery first, waste and old lithium ion battery after pre-burning obtains positive and negative anodes pole piece through Mechanical Crushing, sorting, wet method stripping is carried out, achievees the purpose that positive-active material, carbon dust and aluminium, copper foil efficiently separate.The rate of recovery of nickel cobalt manganese lithium is all higher than 99% in positive-active material after separation, contains aluminium in positive-active material, copper is respectively less than 0.05%.The method of the present invention is simple and practicable, and the process of pre-burning carries out two sections of innoxious absorptions to the electrolyte and organic substance of hardly possible recycling and handles, and solves the problems, such as waste and old lithium ion battery electrolyte volatilization pollution environment in shattering process.Effectively waste lithium ion cell anode active material is completely separated with aluminium foil using wet method stripping, nickeliferous, cobalt, manganese, lithium positive-active material are through hydrometallurgic recovery process high efficiente callback valuable metal therein.This method technological process is short, and production cost is low, environmental-friendly, is easy to industrialize.
Description
Technical field
The invention belongs to secondary resources to recycle and circular economy technical field, and in particular to a kind of to utilize two sections of absorptions
Innoxious absorption processing is carried out to the electrolyte and organic substance that volatilize in waste and old lithium ion battery burn-in process, while utilizing leaching
The method of bubble carries out efficiently positive-active material, carbon dust and copper, aluminium foil in broken waste and old lithium ion battery positive/negative plate
The innoxious recovery and treatment method of waste and old lithium ion battery full constituent of separation and recovery.
Background technology
China has become largest production, consumption and the big export country of lithium ion battery at present.According to national statistics office data
Display, it is contemplated that will be more than 2,000,000 to the year two thousand twenty pure electric automobile and plug-in hybrid-power automobile volume of production and marketing.According to power
The service life of battery 5-8, the newly-increased power battery scrapped in China in 2018 are up to 11.8Gwh, corresponding recoverable
Metal be：1.8 ten thousand tons of nickel, 0.3 ten thousand tons of cobalt, 1.12 ten thousand tons of manganese, 0.34 ten thousand tons of lithium；The newly-increased power battery scrapped will within 2023
Reach 101Gwh, the metal of corresponding recoverable is：11.9 ten thousand tons of nickel, 2.3 ten thousand tons of cobalt, 7.1 ten thousand tons of manganese, 20,000 tons of lithium.Accordingly
Measuring and calculating, the overall market scale that the metals such as Call Provision, nickel, manganese, lithium are created from waste and old dynamic lithium battery in 2023 will be more than 300
Hundred million yuan.As lithium ion battery shipment amount and learies rapidly increase, thing followed environmental problem and resource reclaim recycle
Problem has aroused widespread concern in all circles of society.Therefore carry out to waste and old lithium ion battery and its generate the Resource recovery of waste material,
It will produce good economic benefit, social benefit and environmental benefit.
How electrode activity material in waste and old lithium ion battery to be kept completely separate with copper aluminium foil, in waste and old lithium ion battery
Nickel, cobalt, manganese, lithium metal element carry out high efficiente callback, while waste and old lithium ion battery pre-process shattering process in realize electricity
The harmless treatment of liquid and organic substance is solved, the two-win of environmental protection and economic development is really realized, makes lithium ion battery industry
Benign sustainable development is obtained, the emphasis and difficult point of waste and old lithium ion battery recycling are become.At present to waste and old lithium ion battery
It recycles research and is concentrated mainly on valuable metal recovery use aspects, recycling or harmless treatment are carried out to electrolyte therein
Research it is less, the problems such as that there are mechanization degrees when large-scale production is low, environmental pollution.Recycle the main method of valuable metal
There are the techniques such as pyrogenic process recycling, hydrometallurgic recovery, studies more using wet recycling process that the metalliferous material in anode pole piece is sour
Leaching recycling obtains the metallic solution containing cobalt, aluminium, lithium, is then recycling cobalt and lithium therein by the methods of extraction, ion exchange,
Metallic aluminium is removed generally as impurity.
Japan Patent CN1402376 disclose it is a kind of by used waste lithium ion in high temperature kiln roasting, point
Solution removes organic bath, is sieved after crushing, and oversize is handled with magnetic separation and eddy current separation again, isolate size degradation iron-clad,
Copper foil and aluminium foil etc..
Chinese patent CN105870529A discloses a kind of battery core is placed in DMC and impregnates, cleaning；It takes out in battery core
Positive/negative plate is respectively placed in NMP, distilled water and impregnates, is ultrasonically treated, obtains positive and negative anodes collector and positive and negative by positive and negative plate
Pole powder solution.Positive and negative electrode powder solution is centrifuged, positive and negative electrode powder is collected, is recycled after dry.
Chinese patent CN101942569A discloses a kind of side recycling lithium from waste and old lithium ion battery and waste pole piece
Method is mainly characterized by waste and old lithium ion battery or waste pole piece crusher in crushing, then is placed in thermally treated in high temperature furnace
Removal binder obtains powder.The aluminium in removal powder is dissolved with sodium hydroxide solution, with acid and reducing agent by electrode activity thing
Material leaches, and chemical method removes the impurity such as iron, copper, the aluminium in leachate.
Chinese patent CN103985920 and patent CN103367839 disclose it is a kind of directly from scrap lithium ion battery just
The separation method of cobalt acid lithium and aluminium foil on pole piece is mainly characterized by used Li ion cell carrying out discharge treatment, then just
Pole piece is put into the roasting of resistance furnace high temperature, and the positive plate after roasting is put into the container of water and stirs, finally by the object in container
Matter is sieved to obtain aluminium foil and positive-active material with sieve.
Chinese patent CN102517448A discloses one kind and adopting the immersion of n-methyl-2-pyrrolidone liquid organic acid, ultrasound
Treatment of battery pole piece obtains positive-active material.Positive-active material through 500 ~ 800 DEG C of 2 ~ 6h of calcining, obtains LiCoO again2Production
Product.
Chinese patent CN104157926 discloses a kind of method being crushed using physical impact, effectively by waste mobile phone
The broken dissociation of lithium ion battery, realizes selective broken, and broken material obtains aluminium by varigrained sieve, recycling
Foil.
It is had the following problems in the patent of above-mentioned separation and recovery Metal Values From Spent Lithium-ion Batteries：1, waste and old lithium from
Sub- battery pretreatment stage does not carry out recycling to the electrolyte to volatilize in shattering process or innoxious absorption is handled.2, pyrogenic process and
Physical separates and recovers electrode activity material and copper aluminium foil, although this method is simple, high energy consumption, and there are copper aluminium foils and electricity
Pole active material detaches halfway problem, and preprocessing process valuable metal yield is low.3, using the method for organic acid soak point
From recycling electrode activity material and copper aluminium foil, the organic acid used in this method causes serious pollution to the environment, and has certain wound to human body
The problem of evil, equally exists positive-active material and is detached with aluminium foil not exclusively, separative efficiency bottom.3, the side leached using Whote-wet method
Copper aluminium in waste and old lithium ion battery is leached into solution by method, then chemically by copper alum recovery, there are techniques for the method
Long flow path, reagent consumption is big, it is high there are cost recovery the problems such as.
Invention content
The technical problem to be solved by the present invention is to be directed to valuable gold in current waste and old lithium ion battery electrode active material
Belong to what the method recycled can not be completely separated the defect and electrode active material of environment generation secondary pollution with copper aluminium foil
Problem, and propose a kind of electrolyte to volatilize in shattering process to waste and old lithium ion battery and organic substance carry out two sections it is harmless
Change absorption processing, broken positive and negative anodes pole piece is realized into efficiently separating for electrode activity material and copper aluminium foil, the anode of recycling
Nickel in active material, cobalt, manganese, lithium yield reach 99% or more.
Technical problem to solve the present invention adopts the following technical scheme that：
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent, steps of the method are：
A, the waste and old lithium ion battery for collecting various models is placed in the sodium chloride solution that mass fraction is 5-10% and impregnates, makes
It discharges completely；
B, the waste and old lithium ion battery after electric discharge is placed in resistance furnace and carries out innoxious pre-burning, the electrolysis that burn-in process generates
Liquid and organic substance carry out two sections of absorptions；
C, the waste and old lithium ion battery after pre-burning is subjected to Mechanical Crushing, sorting obtains positive and negative anodes pole piece；
D, the sulfuric acid solution of 1.0-3.0mol/L is prepared, the positive and negative anodes pole piece immersion being crushed is put into after heating sulfuric acid solution to be made just
Pole active material and carbon dust are completely exfoliated from aluminium foil, copper foil；
E, it is rinsed with water 1-2 times after pulling aluminium foil, the copper foil after stripping with sieve out, naturally dry obtains aluminium foil, copper foil, containing just
The acid solution of pole active material is separated by solid-liquid separation, and positive-active material and toner mixture are obtained after the washed drying of filter residue,
Positive electrode active material material is subjected to the valuable metals such as wet-leaching recycling nickel therein, cobalt, manganese, lithium.
Calcined temperature is 200-600 DEG C in the step b, burn-in time 0.5-5h.
Using two sections of absorptions, one section is absorbed electrolyte and organic substance in the step b using activated carbon, two sections of uses
Alkali spray-absorption, alkali used are sodium hydroxide or calcium hydroxide.
Waste and old lithium ion battery Mechanical Crushing in the step c is at 3cm × 4cm-3cm × 5cm positive and negative anodes pole pieces.
Sulfuric acid solution heating temperature is 30-60 DEG C in the step d, soaking time 2-10min.
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent of the present invention realizes waste and old lithium ion battery
The innoxious recovery processing of whole process and valuable metal comprehensive utilization, make lithium ion battery industry obtain benign sustainable development.
This method is simple and practicable, and electrolyte and the innoxious absorption of organic substance, the method removal process are realized in preprocessing process
It is more environmentally-friendly, it avoids the waste and old lithium ion battery secondary pollution caused by environment, removal process in shattering process and does not generate
Toxic and harmful gas.The separative efficiency of electrode activity material and copper aluminium foil is high, nickel in isolated electrode activity material, cobalt,
Manganese, lithium yield reach 99% or more, wherein be respectively less than 0.05% containing aluminium, copper, can further hydrometallurgic recovery valuable metal therein,
The copper aluminium foil of recycling, which is 3cm × 4cm-3cm × 5cm small pieces, directly to be recycled, and easily realize large-scale industrial production.
Compared with the existing technology, the beneficial effects of the present invention are：
1, waste and old lithium ion battery electrolyte and the innoxious absorption of organic substance in removal process are realized to handle, is solved useless
Old lithium ion battery problem of environmental pollution caused by electrolyte volatilization in shattering process.
2, the difficulty that electrode activity material can not be efficiently separated with copper aluminium foil in waste and old lithium ion battery removal process is solved
Topic, realization electrode activity material are completely separated with copper aluminium foil, nickel, cobalt, manganese, lithium valuable metal in the positive-active material of recycling
Yield respectively reaches 99% or more, and 0.05% is respectively less than containing aluminium, copper in obtained electrodeposition active material.
3, this method is simple, and cost recovery is low, and removal process does not generate secondary pollution, no matter from the angle of environmental protection also
It is from the perspective of resource reclaim recycling, the present invention both provides advantageous guarantee.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific implementation mode
Embodiment 1
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent, steps of the method are：Collect nickel cobalt manganese 5:2:3
Ternary waste and old lithium ion battery is placed in the sodium chloride solution that mass fraction is 5% and impregnates, it is made to discharge completely.It will discharge
Full applying waste lithium ionic, which is put into resistance furnace, carries out pre-burning, and 600 DEG C of calcined temperature, burn-in time 0.5h, the process of pre-burning is to difficulty
The electrolyte and organic substance of recycling carry out two sections of innoxious absorption processing, and one section is absorbed using activated carbon, and two sections use alkali hydrogen
Sodium oxide molybdena spray-absorption.Waste and old lithium ion battery Mechanical Crushing after pre-burning is collected at 3cm × 5cm small pieces, after sorting and is obtained altogether
Positive and negative anodes pole piece 5Kg prepares 3.0 mol/L sulfuric acid 10L, is placed in the bucket of 25L, bath temperature rises to 30 DEG C, is put into and is crushed
Positive and negative anodes pole piece impregnate 10 min, pull copper aluminium foil out and be rinsed with water 2 times, solution Bush's funnel mistake of the material containing electrode activity
Filter, residue washing are dried to obtain electrode activity material.Copper aluminium foil 0.91Kg is obtained, electrode activity material 4.08Kg is recycled
To electrode activity material enter wet-leaching process and recycle nickel cobalt manganese lithium therein.
1 electrode activity material ingredient of table
Embodiment 2
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent, steps of the method are：Collect various models
Waste and old lithium ion battery is placed in the sodium chloride solution that mass fraction is 8% and impregnates progress discharge treatment, will discharge complete
Waste and old lithium ion battery, which is put into resistance furnace, carries out pre-burning, and the process of 200 DEG C, burn-in time 6h of calcined temperature, pre-burning returns hardly possible
The electrolyte and organic substance of receipts carry out two sections of innoxious absorption processing, and one section is absorbed using activated carbon, and two sections use alkali hydrogen-oxygen
Change calcium spray-absorption.Waste and old lithium ion battery after pre-burning is broken into 3cm × 3cm small pieces, after sorting altogether collect obtain it is positive and negative
Pole pole piece 10Kg prepares 2 .0mol/L sulfuric acid 20L, is placed in the stainless steel sink of 50L, bath temperature rises to 50 DEG C, is put into cutting
Good positive and negative anodes pole piece impregnates 5 min, and pulling aluminium foil out is rinsed with water 2 times, solution Bush's funnel mistake of the material containing electrode activity
Filter, residue washing are dried to obtain electrode activity material.Copper aluminium foil 1.78Kg, electrode activity material 8.18Kg, the electrode is obtained
Active material enters wet-leaching process and further recycles valuable metal therein.
2 electrode activity material ingredient of table
Embodiment 3
A kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent, steps of the method are：Collect various models
Waste and old lithium ion battery is placed in the sodium chloride solution that mass fraction is 10% and impregnates progress discharge treatment, will discharge complete
Applying waste lithium ionic, which is put into resistance furnace, carries out pre-burning, 400 DEG C, burn-in time 2h of calcined temperature, and the process of pre-burning is to hardly possible recycling
Electrolyte and organic substance carry out two sections of innoxious absorption processing, and one section is absorbed using activated carbon, and two sections use alkali sodium hydroxide
Spray-absorption.Waste and old lithium ion battery after pre-burning is broken into 3cm × 4cm small pieces, is collected altogether after sorting and obtains positive and negative anodes pole
Piece 50Kg configures the total 100L of 1.0mol/L sulfuric acid solutions, is placed in the stainless steel sink of 500L, bath temperature rises to 60 DEG C, is put into
The positive and negative anodes pole piece cut impregnates 2 min, pulls copper aluminium foil out and is rinsed with water 1 time, the solution of the material containing electrode activity uses Bush
Funnel filters, and residue washing is dried to obtain electrode activity material.Copper aluminium foil 9.08g, electrode activity material 40.87g is obtained, it should
Electrode activity material enters wet-leaching process and further recycles valuable metal therein.
3 electrode activity material ingredient of table
As described above, the electrolyte progress the present invention provides a kind of waste and old lithium ion battery in the pretreatment pre-burning stage to volatilization
Two sections of innoxious absorption processing, are fast and efficiently detached back from broken positive and negative anodes pole piece by the method for wet dip
The method for receiving electrode activity material and copper aluminium foil, nickel, cobalt, manganese, lithium metal yield reach in isolated electrode activity material
To 99% or more.The method of the present invention is simple, low for equipment requirements, and secondary pollution is not generated to environment, easily operated, can be to useless
Old lithium ion battery carries out large-scale industrial production.
The basic principles and main features and advantages of the present invention of the present invention, the technology of the industry has been shown and described above
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention.All foundations
The technical spirit of the present invention does any type of simple modification, equivalent change and modification to above example, each falls within the present invention
Protection domain.
Claims (5)
1. a kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent, it is characterised in that steps of the method are：
A, the waste and old lithium ion battery for collecting various models is placed in the sodium chloride solution that mass fraction is 5-10% and impregnates, makes
It discharges completely；
B, the waste and old lithium ion battery after electric discharge is placed in resistance furnace and carries out innoxious pre-burning, the electrolysis that burn-in process generates
Liquid and organic substance carry out two sections of absorptions；
C, the waste and old lithium ion battery after pre-burning is subjected to Mechanical Crushing, sorting obtains positive and negative anodes pole piece；
D, the sulfuric acid solution of 1.0-3.0mol/L is prepared, the positive and negative anodes pole piece immersion being crushed is put into after heating sulfuric acid solution to be made just
Pole active material and carbon dust are completely exfoliated from aluminium foil, copper foil；
E, it is rinsed with water 1-2 times after pulling aluminium foil, the copper foil after stripping with sieve out, naturally dry obtains aluminium foil, copper foil, containing just
The acid solution of pole active material is separated by solid-liquid separation, and positive-active material and toner mixture are obtained after the washed drying of filter residue,
Positive electrode active material material is subjected to the valuable metals such as wet-leaching recycling nickel therein, cobalt, manganese, lithium.
2. a kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent according to claim 1, feature exist
In：Calcined temperature is 200-600 DEG C in the step b, burn-in time 0.5-5h.
3. a kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent according to claim 1 or 2, feature
It is：Using two sections of absorptions, one section is absorbed electrolyte and organic substance in the step b using activated carbon, and two sections use alkali
Spray-absorption, alkali used are sodium hydroxide or calcium hydroxide.
4. a kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent according to claim 3, feature exist
In：Waste and old lithium ion battery Mechanical Crushing in the step c is at 3cm × 4cm-3cm × 5cm positive and negative anodes pole pieces.
5. a kind of innoxious recovery and treatment method of waste and old lithium ion battery full constituent according to claim 1 or 4, feature
It is：Sulfuric acid solution heating temperature is 30-60 DEG C in the step d, soaking time 2-10min.
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Cited By (13)
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| CN110144461A (en) * | 2019-05-08 | 2019-08-20 | 株洲冶炼集团股份有限公司 | A kind of comprehensive recovering process of waste lithium cell positive plate |
| CN110541077A (en) * | 2019-09-30 | 2019-12-06 | 中国矿业大学 | Method for recovering valuable components from waste lithium cobaltate battery positive plates |
| CN111085334A (en) * | 2019-12-10 | 2020-05-01 | 银隆新能源股份有限公司 | Method for recycling waste power batteries by reselection method and jigging equipment |
| CN112397801A (en) * | 2020-10-30 | 2021-02-23 | 北京佰利格瑞资源科技有限公司 | Lithium battery material recycling method |
| CN112510281A (en) * | 2020-11-26 | 2021-03-16 | 中国科学院过程工程研究所 | Method for recovering all components of waste lithium ion battery |
| CN112742843A (en) * | 2020-12-07 | 2021-05-04 | 中南大学 | Method for recycling waste lithium manganate battery through flotation and solid phase sintering |
| CN112786989A (en) * | 2021-03-17 | 2021-05-11 | 中南大学 | Method for separating active material layer and current collector of battery electrode plate |
| CN113165031A (en) * | 2019-03-04 | 2021-07-23 | 川崎重工业株式会社 | Treatment system and treatment method for waste lithium ion battery |
| CN113908977A (en) * | 2021-11-08 | 2022-01-11 | 湖南江冶机电科技股份有限公司 | Recovery process of waste lithium battery |
| CN114188626A (en) * | 2021-11-05 | 2022-03-15 | 华中科技大学 | Method for comprehensively separating and recycling materials in retired battery |
| CN114345539A (en) * | 2021-12-31 | 2022-04-15 | 湖南江冶新能源科技股份有限公司 | Method for separating anode powder and cathode powder of waste lithium battery |
| CN115156243A (en) * | 2022-07-18 | 2022-10-11 | 中国地质科学院郑州矿产综合利用研究所 | Recovery process of anode and cathode materials of waste battery |
| US20230041348A1 (en) * | 2020-06-29 | 2023-02-09 | Lg Energy Solution, Ltd. | Method for reusing active material by using positive electrode scrap |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113165031A (en) * | 2019-03-04 | 2021-07-23 | 川崎重工业株式会社 | Treatment system and treatment method for waste lithium ion battery |
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Application publication date: 20180918 |