CN109652655A - A kind of method that recovery processing lithium battery recycles lithium in the process - Google Patents
A kind of method that recovery processing lithium battery recycles lithium in the process Download PDFInfo
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- CN109652655A CN109652655A CN201811648635.7A CN201811648635A CN109652655A CN 109652655 A CN109652655 A CN 109652655A CN 201811648635 A CN201811648635 A CN 201811648635A CN 109652655 A CN109652655 A CN 109652655A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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
The present invention relates to a kind of methods that lithium is recycled during recovery processing lithium battery.It by waste lithium cell battery core by Mechanical Crushing, is impregnated after broken, the filtered filter cake fragment pyrolysis of water logging obtains pyrolysis material water logging under stirring condition, and filter screen gets copper aluminium foil mixing fragment, positive and negative anodes blending filter cake and rich lithium solution while hot；Filtrate water logging repeatedly after gained richness lithium solution to be pyrolyzed to the stirring water logging filtering of material again, rich lithium solution is then heated up, lithium carbonate is precipitated using poor solubility, filters to obtain lithium carbonate crude product；Crude product is prepared into lithium carbonate slurry through water again and filters out precipitating then in pumping liquid injection circulation reactor, the lithium solution refined；Lithium solution heating to above-mentioned purification, is filtered, then water washing filter cake, filter cake after heat preservation, dry, obtains lithium carbonate product.Using the recovery method of lithium in waste lithium cell of the invention, 99.5% or more the lithium carbonate purity of recycling, and impurity index can reach the professional standard that battery-level lithium carbonate uses.
Description
Technical field
The present invention relates to the recycling of lithium battery, lithium is recycled during specifically a kind of recovery processing lithium battery
Method.
Background technique
With the development of science and technology, electronic product has penetrated into the every nook and cranny of people's life.Due to lithium ion battery with
Ickel-cadmium cell, Ni-H cell are compared, and have high small in size, light weight, operating voltage, volume and specific energy high, memoryless
Effect, the advantages that self discharge is small, operating temperature range is wide, the service life is long, have dominated small-sized portable electronic product market, example
Such as: being applied to portable phone, video camera, portable notebook.As society continues to develop, weather, the energy and environment are asked
The appearance of topic, lithium ion battery are also widely used to electric car field.
With the fast development of lithium ion battery technology, the yield and learies of lithium ion battery, which is all presented, to be quicklyd increase
Trend, patent and the registration for studying waste and old lithium ion battery renewable resources are also more, mainly there is hydrometallurgic recovery and Dry recovery.Its
Middle hydrometallurgic recovery is current main recovery method.In hydrometallurgic recovery technology, mainstream technology route uses cracking and sorting, high temperature
Roasting, acidleach removal of impurities, heavy presoma, the recycling processes such as sulfate and lithium carbonate recycle the active part in lithium battery.
The method that wherein recycling lithium step mainly uses carries out mentioning lithium to handle heavy presoma mother liquor.But due to mother liquor complicated composition and sulphur
Hydrochlorate concentration is high, causes elemental lithium recovery difficult big and the lithium product quality of recycling is low.Accordingly, it is considered to the economy of lithium recycling
Property, it all selects the recycling for abandoning lithium mostly using the lithium battery returned enterprise of conventional wet recovery technology, causes lithium resource
Significant wastage.How to promote the economy of elemental lithium recycling and the quality for improving recycling lithium product is the great of lithium electricity recycling industry
Problem.
Summary of the invention
It is an object of that present invention to provide a kind of methods that lithium is recycled during recovery processing lithium battery.
To achieve the above object, the invention adopts a technical scheme as:
A kind of method that recovery processing lithium battery recycles lithium in the process:
1) waste lithium cell battery core is impregnated into 0.1-1h in water, the filtered filter of water logging after broken by Mechanical Crushing
Cake fragment is in CO2Or contain CO2Under mixed gas and oxygen free condition, heat up pyrolysis, obtains pyrolysis material water logging under stirring condition
1-5h, filter screen gets copper aluminium foil mixing fragment, positive and negative anodes blending filter cake and rich lithium solution while hot；Wherein, during water logging
The additional amount of water is 2-20 times of quality of material；
It is described by waste lithium cell battery core by Mechanical Crushing, impregnated after broken in water 0.1-1h as a water logging；
Be pyrolyzed material under stirring condition water logging 1-5h as secondary water logging；The separation of the realization elemental lithium of water logging twice.
2) by above-mentioned gained richness lithium solution, water logging is straight repeatedly for filtrate after the stirring water logging filtering of step 1) pyrolysis material again
Into rich lithium solution, lithium carbonate mass concentration is 1.1-1.3wt% (obtaining saturated concentration under the room temperature of lithium carbonate), then will
Rich lithium solution is warming up to 80-100 DEG C, and lithium carbonate is precipitated (i.e. by the saturation of lithium carbonate under high temperature and low temperature using poor solubility
Concentration is different), filter to obtain lithium carbonate crude product；
3) crude product is prepared to the lithium carbonate slurry of 2wt%-8wt% through water again, then pumping liquid injection circulation reactor
In, lead to CO at normal temperatures and pressures2It is reacted, the pH=7-9 to reaction solution (is passed through CO in system2It is reacted, reaction is formed
The pH value of carbonic acid adjustment system), precipitating is filtered out, the lithium solution refined；
4) 80-100 DEG C is heated to the lithium solution of above-mentioned purification, is filtered after keeping the temperature 0.5-2h, then washed through 90-100 DEG C
Filter cake is washed, filter cake is in CO2100-200 DEG C of drying under atmosphere, obtains lithium carbonate product.
Contain CO in the step 1)2Mixed gas is N2And CO2Or CO and CO2Mixed gas.Wherein, N2Or CO and CO2
Volume ratio be 1:10-10:1.
Waste power lithium battery carries out water logging after break process in the step 1), and mixed material is obtained by filtration after water logging and exists
CO2Or contain CO2Under mixed gas and oxygen free condition, 5-15 DEG C/min of heating rate is controlled, 400-800 DEG C of heat preservation 0.5- is warming up to
4h。
In the step 2) after filtering during water logging of the filtrate set for material after step 1) pyrolysis；In the step 4)
Filtrate set is for during step 3) lithium carbonate crude product slurry preparation after filtering.
Advantage for present invention:
Using the recovery method of lithium in waste lithium cell of the invention, 99.5% or more the lithium carbonate purity of recycling is waste and old
Lithium overall recovery in lithium battery can reach 95% or more, and impurity index can reach the industry that battery-level lithium carbonate uses
Standard, while lithium recovery process water recycled, non-wastewater discharge.Using liquid jet loop reactor, it is anti-to enhance gas-liquid
Answer efficiency, substantially emission-free discharge in lithium recovery process.
Simultaneously using Soaking treatment twice in removal process of the present invention, using in a water logging process removal battery fragment
Most impurity that electrolyte generates, then pass through CO2Or contain CO2The atmosphere of mixed gas is pyrolyzed, and swims cell active materials
The elemental lithium separated out is generated in the form of lithium carbonate, and lithium carbonate is dissolved out to Ni, Co, Mn isoreactivity substance completely by secondary water logging
The separation not soluble in water for realizing elemental lithium.The technique for extracting lithium carbonate using the poor solubility of lithium carbonate at different temperatures simultaneously
Lithium salts is recycled, compared with being concentrated by evaporation Lithium carbonate solution and extracting lithium carbonate technique, energy consumption is greatly reduced, and obtained lithium carbonate
Content in crude product height (98.5%-99.2%).Then by carbonizatin method prepared calcium carbonate lithium crude product, the carbonic acid lithium content of recycling reaches electricity
99.5% or more of pond level lithium carbonate requirement.
Detailed description of the invention
Fig. 1 is recycling lithium process during recovery processing lithium battery provided in an embodiment of the present invention.
Specific embodiment:
With reference to the accompanying drawing and embodiment the present invention will be further explained explanation.
Embodiment 1
18650 dynamic lithium battery decladding of waste and old nickel-cobalt-manganese ternary after the electric discharge of 30 sections is obtained into battery core, battery core is put into shearing
Mechanical Crushing selection by winnowing is carried out in formula crusher and obtains battery mixing particle 1.01kg, is then immersed in 6.00kg water
0.5h, the filter cake filtered after immersion are put into pyrolysis oven, lead to CO2It is pyrolyzed, 8 DEG C of heating rate of control/per minute, it is warming up to
650 DEG C, 1 hour is kept the temperature, pyrolysis material taking-up is put into stirring in 12.00kg water and is impregnated 3 hours, screening is filtered while hot, is recycled
Copper aluminium foil 0.14kg, positive and negative anodes mixed material 0.62kg and rich lithium solution 12.05kg.
Water logging makes the lithium carbonate mass concentration of rich lithium solution in filtrate reach 1.2wt% after pyrolysis, directly by above-mentioned institute
It obtains rich lithium solution and is warming up to 95 DEG C, according to the difference of lithium carbonate saturated concentration under different temperatures, lithium carbonate is precipitated with poor solubility,
Filtration drying obtains lithium carbonate crude product (content 98.80%) 48g, and filtrate 12.00kg is down to water of the room temperature set for material after being pyrolyzed
Leaching；
The lithium carbonate slurry that crude product is prepared through water to 5wt% again, then in pumping liquid injection circulation reactor, and is passed through
CO2It is reacted, the pH=7.8 to reaction solution (is passed through CO in system2It is reacted, reaction forms the pH of carbonic acid adjustment system
Value), purification lithium solution 0.98kg is obtained by filtration.
90 DEG C are heated to above-mentioned purification lithium solution, keeps the temperature 1h, filtering, then through 90 DEG C of water washings, obtain lithium carbonate wet product,
Wet product is in CO2The lower 150 DEG C of dryings of atmosphere obtain 40.0 grams of lithium carbonate, carbonic acid lithium content 99.58% to constant weight.Filtrated stock
0.9kg cools down rear enclosure for lithium carbonate crude product slurry preparation process.
The present embodiment process water is to obtain to extract lithium carbonate with poor solubility in subsequent embodiment based on fresh water
Stabilization technique data provide raw material place mat.
Embodiment 2
18650 dynamic lithium battery decladding of waste and old nickel-cobalt-manganese ternary after the electric discharge of 10 sections is obtained into battery core, battery core is put into shearing
Mechanical Crushing selection by winnowing is carried out in formula crusher and obtains battery mixing particle 0.34kg, is then immersed in 1h in 2.00kg water,
In the filter cake investment pyrolysis oven filtered after immersion, lead to CO2And N2Mixed gas (volume ratio 1:1) be pyrolyzed, control heating speed
12 DEG C of degree/per minute, 600 DEG C are warming up to, keeps the temperature 2 hours, pyrolysis material taking-up is put into 12.00kg and (applies in embodiment 1 and mentions
Filtrate after taking lithium carbonate crude product) in water stirring impregnate 2 hours, screening is filtered while hot, and recycling copper aluminium foil 0.05kg, positive and negative anodes are mixed
Close material 0.21kg and rich lithium solution 12.06kg.
Water logging makes the lithium carbonate mass concentration of rich lithium solution in filtrate reach 1.2wt% after pyrolysis, directly by above-mentioned institute
It obtains rich lithium solution and is warming up to 95 DEG C, according to the difference of lithium carbonate saturated concentration under different temperatures, carbonic acid is precipitated by poor solubility
Lithium, filtration drying obtain lithium carbonate crude product (content 99.10%) 55g, and filtrate 12.00kg is down to room temperature set for material after being pyrolyzed
Water logging；
Crude product is added water into the lithium carbonate slurry that (filtrate for applying prepared calcium carbonate lithium in embodiment 1) prepares 5wt%, then
In pumping liquid injection circulation reactor, and it is passed through CO2It is reacted, the pH=7.2 to reaction solution (is passed through CO in system2It carries out
Reaction, reaction form the pH value of carbonic acid adjustment system), purification lithium solution 1.00kg is obtained by filtration.
90 DEG C are heated to above-mentioned purification lithium solution, keeps the temperature 0.5h, filtering, then through 95 DEG C of water washings, it is wet to obtain lithium carbonate
Product, wet product is in CO2The lower 120 DEG C of dryings of atmosphere obtain 48.0 grams of lithium carbonate to constant weight, carbonic acid lithium content 99.62%, elemental lithium
The rate of recovery 95.6%.Filtrated stock 0.92kg cools down rear enclosure for lithium carbonate crude product slurry preparation process.
Embodiment 3
18650 dynamic lithium battery decladding of waste and old nickel-cobalt-manganese ternary after the electric discharge of 10 sections is obtained into battery core, battery core is put into shearing
Mechanical Crushing selection by winnowing is carried out in formula crusher and obtains battery mixing particle 0.35kg, is then immersed in 2.00kg water
0.2h, the filter cake filtered after immersion are put into pyrolysis oven, lead to CO2It is pyrolyzed, is controlled with the mixed gas (volume ratio 1:1) of CO
10 DEG C of heating rate/per minute, 620 DEG C are warming up to, keeps the temperature 1.5 hours, pyrolysis material taking-up is put into 12.00kg and (applies reality
Apply and extract the filtrate after lithium carbonate crude product in example 2) in water stirring impregnate 3 hours, screening is filtered while hot, recycles copper aluminium foil
0.05kg, positive and negative anodes mixed material 0.21kg and rich lithium solution 12.06kg.
Water logging makes the lithium carbonate mass concentration of rich lithium solution in filtrate reach 1.2wt% after pyrolysis, directly by above-mentioned institute
It obtains rich lithium solution and is warming up to 95 DEG C, according to the difference of lithium carbonate saturated concentration under different temperatures, carbonic acid is precipitated by poor solubility
Lithium, filtration drying obtain lithium carbonate crude product (content 99.00%) 57g, and filtrate 12.00kg is down to room temperature set for material after being pyrolyzed
Water logging；
Crude product is added water into the lithium carbonate slurry that (filtrate for applying prepared calcium carbonate lithium in embodiment 2) prepares 5wt%, then
In pumping liquid injection circulation reactor, and it is passed through CO2It is reacted, the pH=7.5 to reaction solution (is passed through CO in system2It carries out
Reaction, reaction form the pH value of carbonic acid adjustment system), purification lithium solution 1.02kg is obtained by filtration.
90 DEG C are heated to above-mentioned purification lithium solution, keeps the temperature 0.5h, filtering, then through 95 DEG C of water washings, it is wet to obtain lithium carbonate
Product, wet product is in CO2The lower 110 DEG C of dryings of atmosphere obtain 49.0 grams of lithium carbonate to constant weight, carbonic acid lithium content 99.50%, elemental lithium
The rate of recovery 97.5%.Filtrated stock 0.91kg cools down rear enclosure for lithium carbonate crude product slurry preparation process.
Embodiment 4
18650 dynamic lithium battery decladding of waste and old nickel-cobalt-manganese ternary after the electric discharge of 10 sections is obtained into battery core, battery core is put into shearing
Mechanical Crushing selection by winnowing is carried out in formula crusher and obtains battery mixing particle 0.35kg, is then immersed in 2.00kg water
0.5h, the filter cake filtered after immersion are put into pyrolysis oven, lead to CO2It is pyrolyzed, 10 DEG C of heating rate of control/per minute, heating
To 620 DEG C, 1.5 hours are kept the temperature, pyrolysis material taking-up is put into 12.00kg and (is applied after extracting lithium carbonate crude product in embodiment 3
Filtrate) in water stirring impregnate 2 hours, screening is filtered while hot, recycling copper aluminium foil 0.05kg, positive and negative anodes mixed material 0.21kg and richness
Lithium solution 12.06kg.
Water logging makes the lithium carbonate mass concentration of rich lithium solution in filtrate reach 1.2wt% after pyrolysis, directly by above-mentioned institute
It obtains rich lithium solution and is warming up to 95 DEG C, according to the difference of lithium carbonate saturated concentration under different temperatures, carbonic acid is precipitated by poor solubility
Lithium, filtration drying obtain lithium carbonate crude product (content 99.20%) 56g, and filtrate 12.00kg is down to room temperature set for material after being pyrolyzed
Water logging；
Crude product is added water into the lithium carbonate slurry that (filtrate for applying prepared calcium carbonate lithium in embodiment 3) prepares 5wt%, then
In pumping liquid injection circulation reactor, and it is passed through CO2It is reacted, the pH=7.5 to reaction solution (is passed through CO in system2It carries out
Reaction, reaction form the pH value of carbonic acid adjustment system), purification lithium solution 1.02kg is obtained by filtration.
90 DEG C are heated to above-mentioned purification lithium solution, keeps the temperature 0.5h, filtering, then through 95 DEG C of water washings, it is wet to obtain lithium carbonate
Product, wet product is in CO2The lower 110 DEG C of dryings of atmosphere obtain 48.6 grams of lithium carbonate to constant weight, carbonic acid lithium content 99.65%, elemental lithium
The rate of recovery 96.9%.Filtrated stock 0.91kg cools down rear enclosure for lithium carbonate crude product slurry preparation process.
Claims (4)
1. recycling the method for lithium during a kind of recovery processing lithium battery, it is characterised in that:
1) waste lithium cell battery core is impregnated into 0.1-1h in water after broken, the filtered filter cake of water logging is broken by Mechanical Crushing
Piece is in CO2Or contain CO2Under mixed gas and oxygen free condition, heat up pyrolysis, obtains pyrolysis material water logging 1- under stirring condition
5h, filter screen gets copper aluminium foil mixing fragment, positive and negative anodes blending filter cake and rich lithium solution while hot；Wherein, water during water logging
Additional amount be 2-20 times of quality of material；
2) by above-mentioned gained richness lithium solution again after the stirring water logging filtering of step 1) pyrolysis material filtrate repeatedly water logging until rich
Lithium carbonate mass concentration is 1.1-1.3wt% in lithium solution, and rich lithium solution is then warming up to 80-100 DEG C, utilizes poor solubility
Lithium carbonate is precipitated, filters to obtain lithium carbonate crude product；
3) the lithium carbonate slurry that crude product is prepared through water to 2wt%-8wt% again, then in pumping liquid injection circulation reactor,
Lead to CO under normal temperature and pressure2It is reacted, to the pH=7-9 of reaction solution, filters out precipitating, the lithium solution refined；
4) 80-100 DEG C is heated to the lithium solution of above-mentioned purification, is filtered after keeping the temperature 0.5-2h, then filtered through 90-100 DEG C of water washing
Cake, filter cake is in CO2100-200 DEG C of drying under atmosphere, obtains lithium carbonate product.
2. recycling the method for lithium during recovery processing lithium battery according to claim 1, it is characterised in that: the step 1)
In contain CO2Mixed gas is N2And CO2Or CO and CO2Mixed gas；Wherein, N2Or CO and CO2Volume ratio be 1:10-10:
1。
3. recycling the method for lithium during recovery processing lithium battery according to claim 1, it is characterised in that: the step 1)
Waste power lithium battery carries out water logging after middle break process, and mixed material is obtained by filtration after water logging in CO2Or contain CO2Mixed gas
And under oxygen free condition, 5-15 DEG C/min of heating rate is controlled, 400-800 DEG C of heat preservation 0.5-4h is warming up to.
4. recycling the method for lithium during recovery processing lithium battery according to claim 1, it is characterised in that: the step 2)
After middle filtering during water logging of the filtrate set for material after step 1) pyrolysis；Filtrate covers for walking after filtering in the step 4)
During rapid 3) lithium carbonate crude product slurry preparation.
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| US11873228B2 (en) * | 2022-04-08 | 2024-01-16 | Uong CHON | Method of extracting lithium, method of preparing lithium carbonate and method of preparing lithium hydroxide |
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| WO2022268792A1 (en) | 2021-06-23 | 2022-12-29 | H.C. Starck Tungsten Gmbh | Process for recycling battery materials by way of reductive, pyrometallurgical treatment |
| US11873228B2 (en) * | 2022-04-08 | 2024-01-16 | Uong CHON | Method of extracting lithium, method of preparing lithium carbonate and method of preparing lithium hydroxide |
| CN114951225A (en) * | 2022-06-02 | 2022-08-30 | 安徽南都华铂新材料科技有限公司 | Diaphragm sorting equipment for disassembling waste lithium batteries and sorting operation method thereof |
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