CN107623152B - Applying waste lithium ionic power battery resource recycle method - Google Patents
Applying waste lithium ionic power battery resource recycle method Download PDFInfo
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- CN107623152B CN107623152B CN201711017436.1A CN201711017436A CN107623152B CN 107623152 B CN107623152 B CN 107623152B CN 201711017436 A CN201711017436 A CN 201711017436A CN 107623152 B CN107623152 B CN 107623152B
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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 invention discloses a kind of applying waste lithium ionic power battery resource recycle method, processing step includes: the processes such as applying waste lithium ionic power battery discharge treatment, dismantling processing, burning disposal, more metal charge pulverization process, the molten leaching process of more metal charges acid, extraction processing, precipitation process, flue gas secondary combustion processing, flue gas quenching, flue gas alkali spray process, flue gas urea spray process, flue gas adsorption treatment.The present invention can sufficiently recycle the valuable metal in applying waste lithium ionic power battery, farthest improve metal recovery utilization rate, realize recycling for metal resource；Flue gas is after the process such as second-time burning, chilling, alkali spray, urea spray, absorption, can direct emission, improve applying waste lithium ionic power battery resource utilization process environmental protection index, do not generate secondary pollution, realize clean manufacturing, economic benefit, obvious environment benefit.
Description
Technical field
The present invention relates to waste and old power battery recycling fields, and in particular to a kind of applying waste lithium ionic power battery recycling time
Receiving method.
Background technique
With the fast development of new-energy automobile market, the learies of lithium-ion-power cell will be significantly increased.Lithium ion
Power battery is mainly made of anode, cathode, diaphragm, electrolyte.In typical lithium-ion-power cell containing cobalt, lithium, copper,
The valuable metals such as aluminium, nickel, iron, wherein copper, lithium, cobalt, nickel are primarily present in positive electrode, great recovery value.Waste and old lithium from
If sub- power battery recovery processing is improper, not only the metal resource rate of recovery is not high, causes the waste of resource, will also cause environment dirty
Dye, wherein the resource utilization of waste and old lithium ion battery utilizes and has become one of the key technology that recycling of WEEE utilizes.
Applying waste lithium ionic power battery recovery process is mainly by three kinds of pretreatment, hydrometallurgy, pyrometallurgical smelting technical combinations
It forms.Preconditioning technique is mainly disassembled, is broken, and waste and old lithium ion battery is carried out physical separation.Hydrometallurgy mainly into
Row leaching, extraction, precipitating etc., realize the separation and recycling of metal.Pyrometallurgical smelting is to pass through battery material and reducing agent, slag former
Enter in smelting furnace together after ingredient and carry out reduction melting, enters back into subsequent metal recovery process.
Currently, the recycling of applying waste lithium ionic power battery, which generallys use a variety of method joints, carries out resource utilization, there is place
The problems such as reason long flow path, metal recovery rate is not high.
Patent CN106025417A discloses a kind of applying waste lithium ionic power battery particle sorting unit, sorting unit master
It to include high-pressure water nozzle, vibrating screen panel, tilting stirring slurry, diaphragm casing particle discharge port, collector particle discharge port, electricity
The devices such as pole material discharge port, electrode material holding vessel, diaphragm casing output band, it is broken to may be implemented applying waste lithium ionic power battery
The sorting of each substance in material.The device that the device includes is more, and metal and nonmetallic, metal and metal are easy folder in assorting room
Miscellaneous, metal, which easily loses, causes the rate of recovery not high.
Patent CN106252778A discloses a kind of new-energy automobile applying waste lithium ionic power battery tertiary cathode material
Recovery method includes following processing step: the mixture of positive and negative anodes powder, binder is isolated after waste and old power battery is broken,
By the negative pole graphite powder in mixture, binder burning removal, dust recycles to obtain tertiary cathode material waste material, useless by detecting
The constituent content of lithium, nickel, cobalt, manganese in material, and benefit lithium is carried out, then be sintered-be crushed classification, finally obtain tertiary cathode material
Expect certified products.This method it is poor for applicability, applying waste lithium ionic power battery material ingredient is different, is also easy to during cracking and sorting
It is mingled with the metals such as copper, aluminium, iron in positive and negative anodes powder, after sintering, shadow is caused for subsequent tertiary cathode material product quality
It rings, causes industrialization production process stability poor, be unfavorable for scale application.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of solution applying waste lithium ionic power battery resource
Change removal process metal recovery rate is not high and is also easy to produce secondary pollution problem, realizes the efficient, clear of applying waste lithium ionic power battery
Clean resource utilization.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows: applying waste lithium ionic power battery recycling is returned
Receiving method includes the following steps.
(1) applying waste lithium ionic power battery electric discharge pretreatment: is subjected to discharge treatment.
(2) it disassembles: the obtained waste and old power battery without electricity of step (1) being subjected to shell and disassembles isolated plating
Gold, iron-clad or aluminum hull, battery core, are respectively used to the recycling of subsequent gold, iron, aluminium, and battery core is used for subsequent processing.
(3) it burns: the obtained battery core of step (2) being subjected to burning disposal, obtains more metal charges and flue gas.
(4) it crushes: the obtained more metal charges of step (3) is ground into more metal powder materials.
(5) leach: it is molten that the obtained more metal powder materials of step (4) are carried out acid.
(6) it extracts: the obtained solution of step (5) is subjected to extraction and separation, respectively obtain cobalt, nickel, copper, lithium metal separation
Liquid.
(7) precipitate: the obtained metal separating liquid of step (6) precipitated, to metal be separately recovered to obtain cobalt,
Nickel, copper, lithium metal product.
(8) second-time burning: carrying out second-time burning processing for the obtained flue gas of step (3), will be remaining organic in flue gas
Object full combustion obtains the flue gas without organic matter.
(9) chilling: the obtained flue gas without organic matter of step (8) is subjected to quenching, is cooled down to flue gas
And recuperation of heat.
(10) alkali sprays: the obtained flue gas of step (9) being carried out alkali spray process, is carried out at de- acidic materials to flue gas
Reason obtains the flue gas without acid.
(11) urea sprays: the obtained flue gas of step (10) being carried out urea spray process, carries out denitrogenation oxygen to flue gas
Compound processing, obtains the flue gas of not nitrogen-containing oxide.
(12) it adsorbs: the obtained flue gas of step (11) being subjected to adsorption treatment, adsorbs minimal amount of solid cigarette in flue gas
Dirt, obtain can qualified discharge flue gas.
Preferably, in the step (1), discharge treatment is carried out to applying waste lithium ionic power battery using salt water, when electric discharge
Between 2-4 hour.
Preferably, in the step (2), shell is carried out using dedicated waste and old power battery disassembling apparatus and gold-plated is torn open
Solution and classification recycling.
Preferably, in the step (3), burning disposal is carried out to battery core using converter, incineration temperature control is 400-
800 DEG C, burn time maintenance 30-60 minutes.
Preferably, in the step (4), more metal charges will be obtained in step (3) using pulverizer and crushed, crushed
Granularity is 40-80 mesh.
Preferably, in the step (5), the acid is molten to be dissolved more metal powder materials using sulfuric acid, described
Sulfuric acid concentration is 180-200 g/L, liquid-solid ratio 5-6.
Preferably, in the step (6), the extraction and separation use extractant to extract more metal acid solutions
Separation, removal of impurities are taken, the extractant can be P204, P507, at least one of Cyanex272, respectively obtain cobalt, nickel, copper, lithium
Metal separating liquid.
Preferably, in the step (7), the precipitating uses chemical precipitation method to obtain respectively to step (6)
Metal separating liquid precipitated, precipitating reagent can be oxalic acid, NH4F, at least one of sodium carbonate, respectively obtain copper, cobalt, nickel,
Lithium metal product.
Preferably, in the step (8), the second-time burning temperature control is 1100-1250 DEG C.
Preferably, in the step (9), flue-gas temperature is down to by the chilling using waste heat boiler chilling
Lower than 200 DEG C.
Preferably, in the step (10), the alkali spray is mainly using sodium bicarbonate to the acid in flue gas
Matter is removed, and spray liquid sodium bicarbonate concentration is 10-25wt.%.
Preferably, in the step (11), the urea spray process is using urea to the nitrogen oxides in flue gas
It is removed, spray liquid urea concentration is 5-20wt.%.
Preferably, in the step (12), the absorption mainly use active carbon to impurity remaining in flue gas into
Row absorption, finally makes flue gas qualified discharge.
Preferably, the battery core of the applying waste lithium ionic power battery is after burning disposal in obtained more metal powder materials
Without diaphragm paper, metal recovery rate is up to 99.9% or more.
Compared with the prior art, the advantages of the present invention are as follows: applying waste lithium ionic power battery resource utilization of the invention
Method, clean and effective are crushed-leaching-extraction and separation-by setting electric discharge pretreatment-more metal charges of dismantling-burning-
Precipitating-flue gas secondary combustion-flue gas quenching-flue gas alkali spray process-flue gas urea spray process-flue gas absorption
The process flows such as processing, are finally separately recovered to obtain metallic cobalt, copper, nickel, lithium.It has the advantage that 1 and other waste and old lithiums
Ion battery recovery method is compared, and can sufficiently recycle the valuable metal in applying waste lithium ionic power battery, farthest
Metal recovery utilization rate is improved, realizes recycling for metal resource；2, flue gas is through flue gas secondary combustion, chilling, alkali spray, urine
Element spray, absorption etc. is after process, can direct emission, improve the environmental protection of applying waste lithium ionic power battery resource utilization process
Index does not generate secondary pollution, realizes clean manufacturing, economic benefit, obvious environment benefit.
Detailed description of the invention
Fig. 1 is the process flow chart of applying waste lithium ionic power battery resource recycle method of the present invention.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
As shown in Figure 1, a kind of processing step of applying waste lithium ionic power battery resource recycle method include: waste and old lithium from
Sub- power battery discharge treatment, dismantling processing, burning disposal, more metal charge break process, the molten processing of more metal charges acid, more metals
Expect extraction processing, more metal charge precipitation process, flue gas secondary combustion processing, flue gas quenching, flue gas alkali spray process, flue gas
The valuable metal in applying waste lithium ionic power battery can be finally separately recovered in the processes such as urea spray process, flue gas adsorption treatment,
Realize that metal resource recycles.Flue gas can make to shut out through techniques such as second-time burning, chilling, alkali spray, urea spray, absorption
The secondary pollution that exhausted flue gas generates, improves environmental protection index, realizes resource circulation utilization and the cleaning of applying waste lithium ionic power battery
Production.
Specifically: applying waste lithium ionic power battery being subjected to punching processing using reserve battery puncher, average each electricity
3-4 hole is beaten in pond, can significantly improve the discharging efficiency of applying waste lithium ionic power battery.It will be impregnated through punching treated battery
Discharge treatment, 2-4 hour of discharge time are carried out in salt water.Again by the applying waste lithium ionic power battery after discharge treatment
Dismantling processing is carried out, by the shell of battery and gold-plated dismantling and subsequent classification is used for and recycles, recyclable iron, aluminium and gold-plated.It will
The battery core that dismantling is handled, which is sent into incinerator, carries out burning disposal, and incinerator selects converter, and burning process is maintained at 400-
It is carried out at a temperature of 800 DEG C, burns time maintenance 30-60 minutes, with this condition available applying waste lithium ionic power battery
The optimum efficiency of burning.More metal charges that burning disposal obtains enter pulverization process, are crushed to granularity 40-80 mesh.After crushing
The more metal charges arrived carry out the molten processing of acid, and acid dissolution mainly uses sulfuric acid leaching, and the leachate obtained after the molten processing of acid enters
Subsequent extraction and separation are carried out extraction and separation, removal of impurities to more metal acid solutions using extractant, are produced with the metal classified
Product, then chemical precipitation method is used to handle metal product of the liquid to be classified after extraction and separation.The flue gas that burning process generates
First through second-time burning, i.e., by the organic matter completely burned in flue gas, obtain the flue gas without organic matter, the control of second-time burning temperature
At 1100-1250 DEG C；Flue gas without organic matter enters quenching through pipeline, recuperation of heat is carried out using waste heat boiler, through urgency
After cold treatment, flue-gas temperature is brought down below 200 DEG C.Flue gas after quenching is subjected to alkali spray process, using bicarbonate
Sodium is sprayed, to obtain the flue gas without acidic materials.Flue gas after alkali sprays is subjected to urea spray, to be free of
The flue gas of nitrogen oxides.Flue gas after urea spray process is subjected to adsorption treatment, is adsorbed using active carbon.Waste and old lithium
The battery core of ion battery is free of diaphragm paper after burning disposal in obtained more metal powder materials, metal recovery rate reaches
99.9% or more.
Applying waste lithium ionic power battery after discharge treatment goes electric rate 100%, ensure that the safety of dismantling process, together
When can be recycled for the salt water of electric discharge.The shell that handles through dismantling, gold-plated and battery core can be recycled respectively,
Improve the recovery utilization rate of metal resource.Flue gas after second-time burning, the content of organics through quenching, in flue gas
Lower than 0.1%；Flue gas after alkali spray, urea spray process, flue gas middle acid substance and nitrogen oxides index meet discharge mark
It is quasi-.Meet discharge standard through the indices in activated carbon adsorption treated flue gas.
Embodiment 1
(1) electric discharge pretreatment: carrying out punching processing to applying waste lithium ionic power battery using reserve battery puncher first,
Average each battery beats 3-4 hole, and then battery is soaked in salt water and carries out discharge treatment, 4 hours of discharge time.
(2) it disassembles: using the dedicated waste and old power battery disassembling apparatus waste and old power without electricity obtained to step (1)
Battery carries out shell and gold-plated dismantling, isolated gold-plated, iron-clad or aluminum hull, battery core, is respectively used to subsequent gold, iron, aluminium
Recycling, battery core be used for subsequent recovery processing.
(3) it burns: burning disposal being carried out using battery core of the converter to applying waste lithium ionic power battery, incineration temperature control is
600 DEG C, time maintenance 60 minutes is burned, more metal charges and flue gas are obtained.
(4) it crushes: more metal charges will be obtained in step (3) using pulverizer and crushed, obtaining granularity is that 80 purposes are more
Metal powder material.
(5) it leaches: concentration being used to dissolve for the sulfuric acid solution of 190 g/L to more metal powder materials, control liquid-solid ratio is
5。
(6) it extracts: extraction and separation being carried out to more metal acid solutions using extractant, using P204 extracting copper, using P507
Cobalt is extracted, liquid uses P204 extraction of nickel after extracting cobalt, and lithium in liquid, respectively obtains copper, cobalt, nickel, lithium metal separating liquid after extracting nickel.
(7) precipitate: liquid precipitates after the metal separation obtained respectively to step (6) using chemical precipitation method, uses
Oxalic acid precipitation cobalt, using sodium carbonate coprecipitated nickel hydroxide, using sodium carbonate cement copper, using NH4F precipitates lithium, is separately recovered to obtain oxalic acid
Cobalt, nickelous carbonate, copper carbonate, lithium fluoride product.
(8) second-time burning: carrying out second-time burning processing for the obtained flue gas of step (3), and controlling is 1200 DEG C or so, will
Remaining organic matter full combustion in flue gas obtains the flue gas without organic matter.
(9) chilling chilling: is carried out using the waste heat boiler quick cooling method flue gas without organic matter obtained to step (8)
Processing, is down to 150 DEG C or so for flue-gas temperature.
(10) alkali sprays: concentration being used to carry out alkali to the obtained flue gas of step (9) for the sodium bicarbonate solution of 20wt.%
Spray process carries out de- acidic materials processing to flue gas, obtains the flue gas without acid.
(11) urea sprays: concentration being used to carry out urea spray to (10) obtained flue gas for the urea liquid of 15wt.%
Processing carries out denitrifying oxide processing to flue gas, obtains the flue gas of not nitrogen-containing oxide.
(12) it adsorbs: adsorption treatment will be carried out to the obtained flue gas of step (11) using active carbon, and adsorb pole in flue gas
A small amount of solid flue dust, obtain can qualified discharge flue gas.
Claims (7)
1. a kind of waste and old lithium ion battery resource recycle method, which comprises the following steps:
(1) applying waste lithium ionic power battery electric discharge pretreatment: is subjected to discharge treatment；
(2) it disassembles: the obtained waste and old power battery without electricity of step (1) being subjected to shell and disassembles isolated gold-plated, iron
Shell or aluminum hull, battery core, are respectively used to the recycling of subsequent gold, iron, aluminium, and battery core is used for subsequent recovery processing；
(3) it burns: the obtained battery core of step (2) being subjected to burning disposal, obtains more metal charges and flue gas；
(4) it crushes: the obtained more metal charges of step (3) is ground into more metal powder materials；
(5) leach: it is molten that the obtained more metal powder materials of step (4) are carried out acid；
(6) it extracts: the obtained solution of step (5) being subjected to extraction and separation, respectively obtains cobalt, nickel, copper, lithium metal separating liquid；
(7) it precipitates: the obtained metal separating liquid of step (6) is precipitated, be separately recovered to obtain cobalt, nickel, copper, lithium metal production
Product；
(8) second-time burning: the obtained flue gas of step (3) is subjected to second-time burning processing, organic matter remaining in flue gas is filled
Divided combustion obtains the flue gas without organic matter；
(9) chilling: the obtained flue gas without organic matter of step (8) is subjected to quenching, cooling and heat are carried out to flue gas
Recycling；The chilling is brought down below 200 DEG C using waste heat boiler chilling, by flue-gas temperature；
(10) alkali sprays: the obtained flue gas of step (9) is subjected to alkali spray process, de- acidic materials processing is carried out to flue gas,
Obtain the flue gas without acid；The alkali spray mainly removes the acidic materials in flue gas using sodium bicarbonate, sprays
Liquid sodium bicarbonate concentration is 10-25wt.%；
(11) urea sprays: the obtained flue gas of step (10) being carried out urea spray process, carries out denitrifying oxide to flue gas
Processing, obtains the flue gas of not nitrogen-containing oxide；The urea spray process carries out the nitrogen oxides in flue gas using urea
Removing, spray liquid urea concentration are 5-20wt.%；
(12) it adsorbs: the obtained flue gas of step (11) being subjected to adsorption treatment, minimal amount of solid flue dust in flue gas is adsorbed, obtains
To can qualified discharge flue gas.
2. waste and old lithium ion battery resource recycle method according to claim 1, which is characterized in that the step
(3) in, burning disposal is carried out to battery core using converter, incineration temperature control is 400-800 DEG C, burns 30-60 points of time maintenance
Clock.
3. waste and old lithium ion battery resource recycle method according to claim 1, which is characterized in that the step
(4) in, more metal charges will be obtained in step (3) using pulverizer and crushed, grinding particle size is 40-80 mesh.
4. waste and old lithium ion battery resource recycle method according to claim 1, which is characterized in that the step
(5) in, the acid is molten to be dissolved more metal powder materials using sulfuric acid, and the sulfuric acid concentration is 180-200 g/L, and liquid is solid
Than for 5-6.
5. waste and old lithium ion battery resource recycle method according to claim 1, which is characterized in that the step
(6) in, the extraction and separation use extractant to carry out extraction and separation, removal of impurities to more metal acid solutions, and the extractant is
At least one of P204, P507, Cyanex272 respectively obtain cobalt, nickel, copper, lithium metal separating liquid.
6. waste and old lithium ion battery resource recycle method according to claim 1, which is characterized in that the step
(7) in, the precipitating is that the metal separating liquid for using chemical precipitation method to obtain respectively to step (6) precipitates, and is precipitated
Agent is oxalic acid, NH4F, at least one of sodium carbonate respectively obtain copper, cobalt, nickel, lithium metal product.
7. waste and old lithium ion battery resource recycle method according to claim 1, which is characterized in that the step
(8) in, the second-time burning temperature control is 1100-1250 DEG C.
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| CN109065996B (en) * | 2018-08-02 | 2020-02-04 | 中南大学 | Method for regenerating waste nickel cobalt lithium manganate ternary cathode material |
| CN110034349A (en) * | 2019-04-20 | 2019-07-19 | 湖南金源新材料股份有限公司 | A kind of pretreatment of waste lithium cell and dismantling recovery method |
| CN110061320A (en) * | 2019-04-23 | 2019-07-26 | 金川集团股份有限公司 | A method of utilizing active powder material in cracking process recycling waste power lithium battery |
| CN112086703B (en) * | 2020-09-10 | 2021-08-06 | 中南大学 | Resource treatment method for carbon residue of retired battery |
| CN112030002B (en) * | 2020-09-10 | 2022-12-30 | 江西理工大学 | Method for producing blister copper by directly carrying out oxygen-enriched smelting on waste circuit boards |
| CN112195343A (en) * | 2020-09-11 | 2021-01-08 | 湖南先导新材料科技有限公司 | Lithium battery recycling method and system |
| CN113745685B (en) * | 2021-09-07 | 2023-05-12 | 派尔森环保科技有限公司 | Waste battery recycling system and process |
| CN116315232A (en) * | 2023-03-29 | 2023-06-23 | 盐城工学院 | Environment-friendly recycling method for waste power batteries |
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| CN105728434B (en) * | 2016-02-29 | 2017-05-17 | 中南大学 | Resourceful treatment method for waste circuit board |
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