CN106229577A - The method that the mixing of a kind of waste nickel hydrogen battery both positive and negative polarity material is leached - Google Patents
The method that the mixing of a kind of waste nickel hydrogen battery both positive and negative polarity material is leached Download PDFInfo
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- CN106229577A CN106229577A CN201610709333.0A CN201610709333A CN106229577A CN 106229577 A CN106229577 A CN 106229577A CN 201610709333 A CN201610709333 A CN 201610709333A CN 106229577 A CN106229577 A CN 106229577A
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- sulphuric acid
- concentrated sulphuric
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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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- 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
- C22B7/007—Wet processes by acid leaching
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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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- General Chemical & Material Sciences (AREA)
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Abstract
The method that the mixing of a kind of waste nickel hydrogen battery both positive and negative polarity material is leached, described method bag: A battery pretreatment, B electrode debris slurry, C-acid leaching process, D solid-liquid separation add up to 4 steps.Through pretreated waste nickel hydrogen battery both positive and negative polarity mixed material, by controlling hydrogen peroxide and the addition speed of concentrated sulphuric acid, the heat of dilution of acid and the heat of reaction self is effectively utilized to leach, it is to avoid external heat, improve leaching efficiency, valuable metal leaching rate is all higher than 99%.
Description
Technical field
The present invention relates to Ni-MH battery recovery technology field, specifically a kind of waste nickel hydrogen battery both positive and negative polarity material mixing leaching
The method gone out.
Background technology
Ni-MH battery is mainly used in consumption electronic products and hybrid vehicle, and the service life of Ni-MH battery is 3-8
Year, along with adding up year by year of Ni-MH battery usage amount, having resulted in many garbages, future also can continue to increase.Waste nickel-hydrogen electricity
Pond contains substantial amounts of nickel and a considerable amount of cobalt and rare earth, nickel and compound thereof are the most poisonous, be also confirmed to be environmental carcinogenesis
Material.It addition, nickel be a kind of rare, of many uses, be worth higher non-ferrous metal, cobalt resource especially is few, grade is low, price is high
Expensive metal.The electrode active material of every 100,000,000 Ni-MH battery 2000t to be expended, recycle substantial amounts of Ni in Ni-MH battery,
The valuable metal such as Co and rare earth, is possible not only to bring obvious environmental benefit, but also has certain economic benefit and society
Benefit, effectively utilization and the further production cost reducing battery to metals resources all have important value.
The recovery method of waste nickel-hydrogen battery is mainly reclaimed by pyrogenic process and hydrometallurgic recovery both at home and abroad, and pyrogenic process reclaims main utilization and gives up
In used batteries the boiling point difference of each element carry out separating, melting.By pretreated electrode waste material roasting at 600～800 DEG C,
Separating and purify different metals from the flue gas waste residue discharged, can obtain nickeliferous mass fraction is 50%～55%, containing irony
Amount mark is the Ni-Fe alloy of 30%～35%.The raw material that this dilval can produce with nickel-base alloy and rustless steel, current day
This Sumitomo Metal Industries, three moral metal Deng Ji companies use the method to recycle waste nickel hydrogen battery.Pyrogenic process reclaims
Process treatment process is simple, treating capacity is big, and available existing abandoned nickel and cadmium cell processing equipment processes；But there is recovery to obtain
Dilval added value of product low, recovery rate of valuable metals is low, and rare earth composition can not obtain efficient recovery, and processing procedure is to setting
Standby requirement is high, energy consumption is big, easily cause the drawbacks such as secondary pollution.
Hydrometallurgic recovery is by waste nickel hydrogen battery after pretreatment, isolates iron compound, then enters with finite concentration acid
Row dissolves and leaches, and filters insoluble matter and obtains containing metal salt solutions such as Ni, Co, Mn, Al, RE (rare-earth metal La, Ce, Pr, Nd),
Finally use various process for separation and purification, reclaim various valuable metal.During wet recycling process, the leaching of both positive and negative polarity material is
It is related to the committed step of metal yield, processing cost, how valuable metal is efficiently transferred in solution, it is achieved industrialized
Produce continuously, be the research emphasis of wet recycling process.
If Wu Wei et al. is at " rare metal " Vol.34NO.1,2010,70～84 to introduce waste nickel hydrogen battery both positive and negative polarity whole
Body carries out processing to reclaim nickel in battery, cobalt and the technique of rare earth (RE) metal, and determines nickel, cobalt, dilute by orthogonal test
Soil optimization leaching condition in dilute sulfuric acid.Optimizing sulfuric acid leaching condition is: extraction time is 3.8h, and liquid-solid ratio is 15:1, sulfur
Acid initial concentration is 1.8mol/L, extraction temperature 80 DEG C.Under optimizing leaching condition, the leaching rate of nickel reaches 96.8%, the leaching of cobalt
Going out rate and reach 97.3%, the leaching rate of rare earth reaches 94.6%.
In the wet processing process of waste nickel hydrogen battery positive electrode, negative material or anode and cathode mixed materials, acidleach
Time use acid solution mainly have hydrochloric acid, sulphuric acid and nitric acid.General sulphuric acid can effectively leach lanthanum, but other METAL EXTRACTION are the completeest
Entirely；Nitric acid system nickel cobalt leaches most effective, but ferrum leaching rate height is its major defect；And hydrochloric acid that to be Fe extraction efficiency minimum is optimal
Select.But nitric acid and hydrochloric acid are volatile, corrosive equipment during leaching, it evaporate in air and easily pollute environment.Therefore, sulfur is used at present
Between acid is as the concentration compared with polyacid general 1.5～3mol/L of pickle liquor, extraction temperature, typically between 80～95 DEG C, leaches
Between time 1～3h, in the majority between liquid-solid ratio 6～15.
About waste nickel hydrogen battery both positive and negative polarity material leach method, representative patent have CN101383440A,
CN101886178A, EP2597164A1 etc..
Chinese patent CN101383440A discloses one and directly reclaims from anode of nickel-metal hydride battery waste material, prepares ultra-fine nickel
The method of powder, it is mainly characterized by being disassembled by waste nickel hydrogen battery initially with machine of disassembling obtaining positive pole material and pulverizing, then
Using sulphuric acid and hydrogen peroxide system to leach, leachate with P204 abstraction impurity removal, P507 Separation of nickel and cobalt, finally uses hydration after except ferrum
Extra-fine nickel powder is prepared in hydrazine reduction.The method makes the response rate of nickel in anode waste be more than 98.5%, and gained nikel powder is that purity is more than
99.7%, average diameter grain be 400mm, the spherical ultra-fine nickel powder of face-centered cubic crystal formation.The sulphuric acid that in the method, leaching process uses
Initial concentration is 3.2mol/L, and hydrogen peroxide is directly allocated in sulphuric acid, and consumption is 3mL/g positive pole, and liquid-solid ratio is 4:1, extraction temperature
85 DEG C, extraction time 1h, leachate nickel content is about 100g/L, and leaching rate is more than 99%.
Chinese patent CN101886178A discloses the comprehensive recovering process of a kind of waste nickel hydrogen battery, waste nickel hydrogen battery
After broken, magnetic separation, sieving, siftage sulphuric acid and oxidant leach, and carry out the separation and recovery of rare earth after leachate regulation pH,
Carrying out abstraction impurity removal again, the nickel cobalt sulfate liquor finally given can be used for the life of nickel-hydrogen battery positive pole material ball-shape nickel hydroxide
Produce.The method leaching process leachate sulfur acid and oxidant (hydrogen peroxide, persulfuric acid alkali metal salt), sulphuric acid in liquid before leaching
Concentration be 1～5moL, concentration of hydrogen peroxide is 5～10%, and the concentration of alkali metal persulfates is 0.5～5mol/L, liquid-solid ratio
For 6:1, extraction temperature is 50～90 DEG C, and extraction time is 1～3h, and leaching rate is more than 99%.
European patent EP 2597164A1 discloses a kind of separation nickel, cobalt from waste nickel hydrogen battery positive and negative electrode active material
Method, the method by Ni-MH battery disintegrate and classification obtain positive and negative electrode active substance, after sulfuric acid leaching, utilize alkali gold
Belong to sulfate (sodium sulfate, potassium sulfate) rare-earth separating, then remove zinc with sulfide (hydrogen sulfide gas, sodium bisulfide, sodium sulfide)
And reclaim nickel, cobalt, the regenerant nickel cobalt mixed sulfides obtained.Can be directly as manufacturing nickel sulfate and cobaltous sulfate, cobalt metal
Deng known procedure in.In the method, sulfuric acid concentration used by leaching process is 64%, and liquid-solid ratio is about 6:1, extraction temperature 80 DEG C,
Extraction time 3h, leaching process passes through leachate and the neutralization repeatedly of positive and negative electrode active material, makes the pH of final leachate reach
2.0 left and right.
All there is problems with leaching process in patent in above-mentioned document, in (1) leachate, residual acid concentration is higher, follow-up
Also need when rare earth reclaims to add alkali regulation pH, increase acid-base reagent consumption；If utilizing material to be neutralized, neutralize in material used
Valuable metal leaching rate is relatively low, also needs to leach further, reduces the efficiency of leaching, also add equipment investment and workman simultaneously
Labor intensity.(2) generally utilizing the dilute sulfuric acid prepared to do leaching acid, hydrogen peroxide does oxidant, and leaching process needs extra
Heating, although extraction time is shorter, Steep cencentration is higher, but needs the preparation increasing independent complex acid operation and diluted acid with defeated
Send equipment, the most also have lost the heat during diluting concentrated sulfuric acid.
Summary of the invention
The technical problem to be solved is to provide the side that the mixing of a kind of waste nickel hydrogen battery both positive and negative polarity material is leached
Method, higher to solve residual acid concentration in prior art leachate, also need when follow-up rare earth reclaims to add alkali regulation pH, increase acid
Base reagent consumes；The problem that leaching process needs extra heating.
The present invention solves the technical scheme of technical problem: the side that the mixing of a kind of waste nickel hydrogen battery both positive and negative polarity material is leached
Method, described method bag: A battery pretreatment, B electrode debris slurry, C-acid leaching process, D solid-liquid separation add up to 4 steps.
A battery pretreatment: waste nickel hydrogen battery through broken shell, wash, disassemble, be cut into length and width and be about 0.1～about 1cm
Electrode debris.
B electrode debris is starched: add pure water in electrode debris, and electrode debris is 8～12:1 with the liquid-solid ratio of water.
C-acid leaching processes: add concentrated sulphuric acid in the electrode debris after pulp, controls concentrated sulphuric acid and adds speed, when solution temperature
When degree reaches more than 50 DEG C, while continuing to add concentrated sulphuric acid, add hydrogen peroxide, control the addition speed of concentrated sulphuric acid, hydrogen peroxide
Degree, makes solution temperature maintain 50～80 DEG C, and during adding concentrated sulphuric acid, hydrogen peroxide, pH, for maintaining 0.5～1, waits in solution solid
Liquid material proportion no longer changes, and when pH value reaches 1.3～1.5, stops adding concentrated sulphuric acid, hydrogen peroxide, wherein concentrated sulphuric acid consumption
Being 1.5～2.0g/g materials, hydrogen peroxide mass concentration is 30%, and consumption is 0.4～1.2mL/g material.
D solid-liquid separation: after acidleach process material interpolation terminates, uniform stirring 1～1.5h, afterwards solution is carried out solid-liquid and divide
From, obtaining leached mud and leachate, leached mud slag rate is 0.5～1%, and leachate nickel concentration is more than 50g/L.
The beneficial effects of the present invention is: through pretreated waste nickel hydrogen battery both positive and negative polarity mixed material, by control
The addition speed of producing hydrogen peroxide and concentrated sulphuric acid, effectively utilizes the heat of dilution of acid and the heat of reaction self to leach, it is to avoid
External heat, improves the efficiency once leached, and valuable metal leaching rate is all higher than 99%.Leachate after solid-liquid separation without
Regulation pH value can directly carry out rare earth recovery process, and leached mud can reclaim as nickle contained discarded material.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1.
A battery pretreatment: take 100g waste nickel hydrogen battery through broken shell, wash, disassemble, be cut into length and width and be about 0.1～1cm
The electrode debris of left and right.
B electrode debris is starched: add 1000mL pure water in electrode debris.
C-acid leaching processes: add concentrated sulphuric acid in the electrode debris after pulp, controls concentrated sulphuric acid and adds speed, when solution temperature
When degree reaches more than 50 DEG C, while continuing to add concentrated sulphuric acid, add hydrogen peroxide, control the addition speed of concentrated sulphuric acid, hydrogen peroxide
Degree, makes solution temperature maintain 50～80 DEG C, and during adding concentrated sulphuric acid, hydrogen peroxide, pH, for maintaining 0.5, waits solid-liquid in solution
Material proportion no longer changes, and now pH value is 1.5, amounts to and consumes 100mL concentrated sulphuric acid and the hydrogen peroxide of 40mL30%.
D solid-liquid separation: after acidleach process material interpolation terminates, uniform stirring 1h, afterwards solution is carried out solid-liquid separation,
To leached mud and leachate.
Leaching test the results are shown in Table 1.
Table 1 leaching test result
Embodiment 2.
A battery pretreatment: take 1000g waste nickel hydrogen battery through broken shell, wash, disassemble, be cut into length and width be about 0.1～
The electrode debris of about 1cm.
B electrode debris is starched: add 9800mL pure water in electrode debris.
C-acid leaching processes: add concentrated sulphuric acid in the electrode debris after pulp, controls concentrated sulphuric acid and adds speed, when solution temperature
When degree reaches more than 50 DEG C, while continuing to add concentrated sulphuric acid, add hydrogen peroxide, control the addition speed of concentrated sulphuric acid, hydrogen peroxide
Degree, makes solution temperature maintain 50～80 DEG C, and during adding concentrated sulphuric acid, hydrogen peroxide, pH, for maintaining 0.6, waits solid-liquid in solution
Material proportion no longer changes, and now pH value is 1.3, amounts to and consumes 900mL concentrated sulphuric acid and the hydrogen peroxide of 1000mL30%.
D solid-liquid separation: after acidleach process material interpolation terminates, uniform stirring 1.5h, afterwards solution is carried out solid-liquid separation,
Obtain leached mud and leachate.
Leaching test the results are shown in Table 2.
Table 2 leaching test result
Claims (1)
1. the method that a waste nickel hydrogen battery both positive and negative polarity material mixing is leached, it is characterised in that described method includes following technique
Step:
A battery pretreatment: waste nickel hydrogen battery through disassembling, broken shell, wash, be cut into the electrode that length and width are about about 0.1 ~ 1cm
Fragment；
B electrode debris is starched: add water in electrode debris, and electrode debris is 8 ~ 12:1 with the liquid-solid ratio of water；
C-acid leaching processes: add concentrated sulphuric acid in the electrode debris after pulp, controls concentrated sulphuric acid and adds speed, when solution temperature reaches
During to more than 50 DEG C, while continuing to add concentrated sulphuric acid, add hydrogen peroxide, control concentrated sulphuric acid, the addition speed of hydrogen peroxide, make
Solution temperature maintains 50 ~ 80 DEG C, and during adding concentrated sulphuric acid, hydrogen peroxide, system pH, for maintaining 0.5 ~ 1, waits solid-liquid in solution
Material proportion no longer changes, and when pH value reaches 1.3 ~ 1.5, stops adding concentrated sulphuric acid, hydrogen peroxide；Wherein concentrated sulphuric acid consumption is
1.5 ~ 2.0g/g material, hydrogen peroxide mass concentration is 30%, and consumption is 0.4 ~ 1.2mL/g material；
D solid-liquid separation: after acidleach process material interpolation terminates, uniform stirring 1 ~ 1.5h, afterwards solution is carried out solid-liquid separation,
To leached mud and leachate, leached mud slag rate is 0.5 ~ 1%, and leachate nickel concentration is more than 50g/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106935923A (en) * | 2017-03-31 | 2017-07-07 | 山东理工大学 | The method that valuable metal is reclaimed from waste nickel hydrogen battery |
| CN108767286A (en) * | 2018-06-26 | 2018-11-06 | 包头昊明稀土新电源科技有限公司 | Waste and old rare earth new power collector recovery method and device |
| CN109065999A (en) * | 2018-08-17 | 2018-12-21 | 湖南金凯循环科技有限公司 | A method of recycling waste and old lithium titanate battery |
| CN109616713A (en) * | 2018-11-06 | 2019-04-12 | 广西师范大学 | The method that aluminium foil is separated with positive active material in waste and old lithium ion battery |
| CN111689530A (en) * | 2020-05-25 | 2020-09-22 | 荆门市格林美新材料有限公司 | Method and device for producing nickel sulfate solution |
| CN113862474A (en) * | 2021-08-18 | 2021-12-31 | 池州西恩新材料科技有限公司 | Continuous acid leaching system and method adopting aeration to control reaction temperature |
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| CN105024106A (en) * | 2015-07-31 | 2015-11-04 | 合肥国轩高科动力能源股份公司 | Method for recovering ferric phosphate from waste lithium ion battery and scrapped anode piece |
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| JP2003041326A (en) * | 2001-07-27 | 2003-02-13 | Sumitomo Metal Mining Co Ltd | Method for recovering valuable metal from scrap of nickel metal hydride secondary battery |
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| CN108767286A (en) * | 2018-06-26 | 2018-11-06 | 包头昊明稀土新电源科技有限公司 | Waste and old rare earth new power collector recovery method and device |
| CN109065999A (en) * | 2018-08-17 | 2018-12-21 | 湖南金凯循环科技有限公司 | A method of recycling waste and old lithium titanate battery |
| CN109065999B (en) * | 2018-08-17 | 2020-06-19 | 湖南金凯循环科技有限公司 | Method for recycling waste lithium titanate batteries |
| CN109616713A (en) * | 2018-11-06 | 2019-04-12 | 广西师范大学 | The method that aluminium foil is separated with positive active material in waste and old lithium ion battery |
| CN111689530A (en) * | 2020-05-25 | 2020-09-22 | 荆门市格林美新材料有限公司 | Method and device for producing nickel sulfate solution |
| CN111689530B (en) * | 2020-05-25 | 2023-08-22 | 荆门市格林美新材料有限公司 | Nickel sulfate solution production method and device |
| CN113862474A (en) * | 2021-08-18 | 2021-12-31 | 池州西恩新材料科技有限公司 | Continuous acid leaching system and method adopting aeration to control reaction temperature |
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Application publication date: 20161214 |