CN107871912A - In a kind of used Li ion cell from recovery in leachate caused by valuable metal iron removaling aluminium method - Google Patents
In a kind of used Li ion cell from recovery in leachate caused by valuable metal iron removaling aluminium method Download PDFInfo
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- CN107871912A CN107871912A CN201710872175.5A CN201710872175A CN107871912A CN 107871912 A CN107871912 A CN 107871912A CN 201710872175 A CN201710872175 A CN 201710872175A CN 107871912 A CN107871912 A CN 107871912A
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- aluminium
- iron
- slag
- leachate
- valuable metal
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
Abstract
The invention belongs to solution purification field in hydrometallurgy, the method for disclosing iron removaling aluminium in leachate caused by valuable metal (sulfuric acid nickel cobalt manganese solution) in a kind of used Li ion cell from recovery.The inventive method comprises the following steps：(1) pH for adjusting leachate is 1.5~2.0, and addition oxidant makes ferrous oxidising into ferric iron；(2) regulation system pH is 2.5~3.5, is aged, and filtering, obtains filtrate and iron aluminum slag；(3) regulation system pH is 4.5~5.0 again, is aged, and filtering, is purified liquid and aluminium slag.The aluminium slag that step (3) obtains is used to be used for regulation system pH in step (2) as conditioning agent.The inventive method can not only make iron in solution, aluminium content be reduced to production requirement value, and caused slag strainability is good, the valuable metal carried secretly in slag is few, and gained aluminium slag can be repeated for iron removaling in system, the minimizing target of slag is realized, there is preferable economic benefit and environmental benefit.
Description
Technical field
It is valuable in more particularly to a kind of used Li ion cell from recovery the invention belongs to solution purification field in hydrometallurgy
The method of iron removaling aluminium in leachate caused by metal (sulfuric acid nickel cobalt manganese solution).
Background technology
Lithium ion battery since commercialization, because its have, small volume higher than energy, light weight, temperature limit it is wide,
Unique advantage such as have extended cycle life, have a safety feature, and is widely used in civilian and military domain, such as video camera, mobile electricity
Words, notebook computer and Portable Measurement Instrument etc., while lithium ion battery has turned into the light-duty of New-energy electric vehicle first choice
One of high-energy power battery.For lithium ion battery after 500~1500 charge and discharge cycles, its active material will lose work
Property, cause the capacity of battery to decline and scrap battery.Widely using for lithium ion battery certainly will bring substantial amounts of old and useless battery,
If its random discarding can not only be caused seriously to pollute to environment, the even more waste to resource.In lithium ion battery contain compared with
The metals resources such as more nickel (Ni), cobalt (Co), copper (Cu), lithium (Li), aluminium (Al), manganese (Mn), wherein cobalt, nickel, manganese and lithium contain
Amount is respectively up to 30%, 20%, 20% and 35%, even more high.Therefore it is the economic value in waste and old lithium ion battery is high
Metal is recycled, and no matter in terms of the environmental protection or from the aspects of the recycling of resource, is all significant.
The enterprise of recovery used Li ion cell will mainly be prepared into battery material, but electricity again at present after valuable metal recovery
Pond material requires very high to impurity content.Containing elements such as iron, aluminium, zinc, copper, carbon in used Li ion cell, therefore in recovery electricity
Need to purify leachate during valuable metal in pond, and how can make iron in leachate, aluminium remove it is clean and
The problems such as the amount of metal carried secretly in slag is few, slag yield is few, removal of impurities cost is low are always perplex battery recycling industry several big
Problem.Found by consulting substantial amounts of bibliography, domestic technical staff no so far was engaged in be carried out using two-step method
The research of iron removaling aluminium.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of simple, height
Effect from recovery used Li ion cell in leachate caused by valuable metal (sulfuric acid nickel cobalt manganese solution) iron removaling aluminium method,
For solving to reclaim the various problems that iron removaling aluminium runs into during valuable metal in used Li ion cell.
The purpose of the present invention is realized by following proposal：
A kind of simple, efficient leachate (the sulfuric acid nickel cobalt manganese caused by valuable metal from recovery used Li ion cell
Solution) in iron removaling aluminium method, comprise the following steps：
(1) pH for adjusting leachate is 1.5~2.0, and addition oxidant makes ferrous oxidising into ferric iron；
(2) regulation system pH is 2.5~3.5, is aged, and filtering, obtains filtrate and iron aluminum slag；
(3) regulation system pH is 4.5~5.0 again, is aged, and filtering, is purified liquid and aluminium slag.
The aluminium slag that step (3) obtains is used as conditioning agent and is used for regulation system pH in step (2).So as to be removed
Iron, obtain iron aluminum slag.
Above-mentioned aluminium slag, which is used to preferably add aluminium slag in step (2) system in step (2), first reacts 0.5h or more, followed by
Continuous regulation system pH；More preferably react 0.5~1h.
Leachate described in step (1) is preferably the nickel sulfate caused by valuable metal from recovery used Li ion cell
Sulfuric acid nickel cobalt manganese solution after cobalt manganese solution, more preferably copper removal.
Oxidant described in step (1) is oxidant commonly used in the art, such as hydrogen peroxide, sodium chlorate, height
Potassium manganate etc..
The amount of oxidant used is so that ferrous iron is fully oxidized to three-level iron and is defined in system.
Step (1)~step (3) regulation pH can use alkali or acid to be adjusted, and described alkali can be sodium carbonate, hydrogen
At least one of sodium oxide molybdena, calcium carbonate, calcium hydroxide, calcium oxide etc..
The time of ageing is preferably respectively 0.5h or more, preferably 0.5~1h in step (2) and step (3).
Iron aluminum slag obtained by step (2) can use water or diluted acid to be washed.
Iron aluminum slag obtained by step (2) can be used for selling outside.
Step (3) described scavenging solution is solution after target iron removaling aluminium, available for the processing of follow-up valuable metal recovery.
The inventive method, preferably include following steps：
(1) pH for adjusting leachate is 1.5~2.0, and addition oxidant makes ferrous oxidising into ferric iron；
(2) regulation system pH is 2.5~3.5, is aged, and filtering, obtains filtrate and iron aluminum slag；
(3) regulation system pH is 4.5~5.0 again, is aged, and filtering, is purified liquid and aluminium slag；
(4) regulation system pH in step (2) is added using the aluminium slag that step (3) obtains as pH adjusting agent, so as to iron removaling, obtained
To iron aluminum slag；
(5) circulation above-mentioned steps realize the lasting iron removaling of leachate, aluminium.
The present invention is using two-step method to the sulfuric acid nickel cobalt manganese solution caused by valuable metal from recovery used Li ion cell
Iron removaling aluminium is carried out, the iron in solution, aluminium content can not only be made to be reduced to production requirement value, and caused slag strainability is good,
The valuable metal carried secretly in slag is few, it is often more important that the quantity of slag significantly reduces than a step iron removaling aluminium method, realizes the minimizing mesh of slag
Mark, therefore there is preferable economic benefit and environmental benefit with two-step method iron removaling aluminium.
The present invention is had the following advantages and beneficial effect relative to prior art：
The inventive method using from recovery used Li ion cell during valuable metal caused sulfuric acid nickel cobalt manganese solution as
Raw material, the iron aluminium in the sulfuric acid nickel cobalt manganese solution after copper removal is removed totally with two step iron removaling aluminium methods.Present invention process is simple, behaviour
Make simplicity, caused iron aluminum slag amount is few, it is few to be mingled with the valuable metal amount such as nickel cobalt manganese in slag, and gained aluminium slag can be repeated for system
Middle iron removaling, the purification of iron in solution, aluminium is not only realized, also achieve the minimizing of slag, there is preferable environmental benefit and economy
Benefit.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
The material being related in the following example can obtain from commercial channel.
Embodiment 1
Fig. 1 is shown in technological process.The sulfuric acid nickel cobalt manganese solution after 500mL copper removals is taken, its pH is adjusted to 1.5 with sodium carbonate, so
The hydrogen peroxide that mass fraction is 20% is added in backward solution makes ferrous iron in system be fully oxidized to ferric iron, available iron cyaniding
Whether ferrous iron is oxidized completely in potassium sampling Detection system.Aluminium slag reaction 0.5h is added into the solution after oxidation, is added
Calcium carbonate soln makes pH be adjusted to 2.5, and (when first processing does not have aluminium slag, can be directly added into calcium carbonate soln makes pH be adjusted to 2.5), old
Filtered after changing 30min, filtered fluid, which flows into, removes reactive aluminum kettle, and iron aluminum slag is outer after washing to sell.With sodium carbonate liquor by filtered fluid
PH is aged 1h after being adjusted to 4.5, then filter, and is purified liquid and aluminium slag, and scavenging solution flows into next process, and aluminium slag returns again to previous
Step carries out iron removaling and obtains iron aluminum slag.After testing, the solution concentration of iron after purified is 5mg/L, aluminum concentration 75mg/L, is reached
Production requirement；Nickel content is 0.5wt% in iron aluminum slag (butt), cobalt content 0.2wt%, manganese content 0.8wt%, is met
Produce control standard.
Embodiment 2
The sulfuric acid nickel cobalt manganese solution after 500mL copper removals is taken, its pH is adjusted to 2.0 with sodium carbonate, then added into solution
The hydrogen peroxide that mass fraction is 20% makes ferrous iron be fully oxidized to ferric iron, can use divalence in potassium ferricyanide sampling Detection system
Whether iron is oxidized completely.Aluminium slag is added into the solution after oxidation, adding calcium carbonate soln after reaction 1h is adjusted to pH
3.5, filtered after being aged 30min, filtered fluid, which flows into, removes reactive aluminum kettle, and iron aluminum slag is outer after washing to sell.Be tod with sodium carbonate liquor
The pH of filtrate is aged 0.5h after being adjusted to 5.0, then filter, and is purified liquid and aluminium slag, and scavenging solution flows into next process, and aluminium slag is again
Return to previous step progress iron removaling and obtain iron aluminum slag.After testing, the solution concentration of iron after purified is 8mg/L, and aluminum concentration is
51mg/L, production requirement is reached；Nickel content is 0.36wt% in iron aluminum slag (butt), cobalt content 0.15wt%, manganese content
For 0.57wt%, meet production control standard.
Embodiment 3
The sulfuric acid nickel cobalt manganese solution after 500mL copper removals is taken, its pH is adjusted to 1.5 with sodium carbonate, then added into solution
Whether completely the hydrogen peroxide that mass fraction is 20% makes ferrous iron be fully oxidized to ferric iron, ferrous iron quilt is detected with the potassium ferricyanide
Oxidation.Aluminium slag is added into the solution after oxidation, calcium carbonate soln is added after reaction 40min makes pH be adjusted to 3.5, ageing
Filtered after 30min, filtered fluid, which flows into, removes reactive aluminum kettle, and iron aluminum slag is outer after washing to sell.With sodium carbonate liquor by the pH of filtered fluid
50min is aged after being adjusted to 4.8, is then filtered, is purified liquid and aluminium slag, scavenging solution flows into next process, before aluminium slag returns again to
One step carries out iron removaling and obtains iron aluminum slag.After testing, the solution concentration of iron after purified is 4mg/L, aluminum concentration 63mg/L, is reached
Production requirement is arrived；Nickel content is 0.40wt% in iron aluminum slag (butt), cobalt content 0.11wt%, and manganese content is
0.52wt%, meet production control standard.
Embodiment 4
The sulfuric acid nickel cobalt manganese solution after 500mL copper removals is taken, its pH is adjusted to 1.8 with sodium carbonate, then added into solution
Whether completely the hydrogen peroxide that mass fraction is 20% makes ferrous iron be fully oxidized to ferric iron, ferrous iron quilt is detected with the potassium ferricyanide
Oxidation.Aluminium slag is added into the solution after oxidation, adding calcium carbonate soln after reaction 0.5h makes pH be adjusted to 3.0, is aged 30min
After filter, filtered fluid is flowed into and remove reactive aluminum kettle, and iron aluminum slag is sold outside after washing.The pH of filtered fluid is adjusted to sodium carbonate liquor
0.5h is aged after 4.5, is then filtered, is purified liquid and aluminium slag, scavenging solution flows into next process, and aluminium slag returns again to previous step
Carry out iron removaling and obtain iron aluminum slag.After testing, the solution concentration of iron after purified is 4mg/L, aluminum concentration 72mg/L, has reached life
Production requires；Nickel content is 0.32wt% in iron aluminum slag (butt), cobalt content 0.11wt%, manganese content 0.48wt%, is met
Produce control standard.
Embodiment 5
The sulfuric acid nickel cobalt manganese solution after 500mL copper removals is taken, its pH is adjusted to 2.0 with sodium carbonate, then added into solution
Whether completely the hydrogen peroxide that mass fraction is 20% makes ferrous iron be fully oxidized to ferric iron, ferrous iron quilt is detected with the potassium ferricyanide
Oxidation.Aluminium slag is added into the solution after oxidation, adding calcium carbonate soln after reaction 0.5h makes pH be adjusted to 3.5, is aged 30min
After filter, filtered fluid is flowed into and remove reactive aluminum kettle, and iron aluminum slag is sold outside after washing.The pH of filtered fluid is adjusted to sodium carbonate liquor
45min is aged after 4.8, is then filtered, is purified liquid and aluminium slag, scavenging solution flows into next process, and aluminium slag returns again to back
The rapid iron removaling that carries out obtains iron aluminum slag.After testing, the solution concentration of iron after purified is 9mg/L, aluminum concentration 59mg/L, is reached
Production requirement；Nickel content is 0.45wt%, cobalt content 0.21wt%, manganese content 0.65wt% in iron aluminum slag (butt), is accorded with
Control standard is produced in symphysis.
Embodiment 6
The sulfuric acid nickel cobalt manganese solution after 500mL copper removals is taken, its pH is adjusted to 2.0 with sodium carbonate, then added into solution
Whether completely the hydrogen peroxide that mass fraction is 20% makes ferrous iron be fully oxidized to ferric iron, ferrous iron quilt is detected with the potassium ferricyanide
Oxidation.Aluminium slag is added into the solution after oxidation, calcium carbonate soln is added after reaction 45min makes pH be adjusted to 3.0, ageing
Filtered after 30min, filtered fluid, which flows into, removes reactive aluminum kettle, and iron aluminum slag is outer after washing to sell.With sodium carbonate liquor by the pH of filtered fluid
1h is aged after being adjusted to 4.6, is then filtered, is purified liquid and aluminium slag, scavenging solution flows into next process, and aluminium slag returns again to back
The rapid iron removaling that carries out obtains iron aluminum slag.After testing, the solution concentration of iron after purified is 6mg/L, aluminum concentration 76mg/L, is reached
Production requirement；Nickel content is 0.43wt%, cobalt content 0.16wt%, manganese content 0.71wt% in iron aluminum slag (butt), is accorded with
Control standard is produced in symphysis.
The inventive method using from recovery used Li ion cell during valuable metal caused sulfuric acid nickel cobalt manganese solution as
Raw material, the iron aluminium in the sulfuric acid nickel cobalt manganese solution after copper removal is removed totally with two step iron removaling aluminium methods.The letter of the inventive method technique
Single, easy to operate, caused iron aluminum slag amount is few, it is few to be mingled with the valuable metal amount such as nickel cobalt manganese in slag, not only realize iron in solution,
The removal of aluminium, the minimizing of slag is also achieved, there is preferable environmental benefit and economic benefit.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
- It is 1. a kind of from the method for reclaiming iron removaling aluminium in leachate caused by valuable metal in used Li ion cell, it is characterised in that Comprise the following steps：(1) pH for adjusting leachate is 1.5~2.0, and addition oxidant makes ferrous oxidising into ferric iron；(2) regulation system pH is 2.5~3.5, is aged, and filtering, obtains filtrate and iron aluminum slag；(3) regulation system pH is 4.5~5.0 again, is aged, and filtering, is purified liquid and aluminium slag.
- 2. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that：The aluminium slag that step (3) obtains is used to be used for regulation system pH in step (2) as conditioning agent.
- 3. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 2 from recovery Method, it is characterised in that：The aluminium slag be used for step (2) in for will aluminium slag add step (2) system in first react 0.5h or with On, it is further continued for regulation system pH.
- 4. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that：Leachate described in step (1) is the sulphur caused by valuable metal from recovery used Li ion cell Sour nickel cobalt manganese solution.
- 5. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that：Oxidant described in step (1) is at least one of hydrogen peroxide, sodium chlorate and potassium permanganate.
- 6. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that：Step (1)~step (3) regulation pH is adjusted using alkali or acid.
- 7. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 6 from recovery Method, it is characterised in that：Described alkali is at least one in sodium carbonate, sodium hydroxide, calcium carbonate, calcium hydroxide and calcium oxide Kind.
- 8. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that：The time of ageing is respectively 0.5h or more in step (2) and step (3).
- 9. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that：The time of ageing is respectively 0.5~1h in step (2) and step (3).
- 10. iron removaling aluminium in leachate caused by valuable metal in the used Li ion cell according to claim 1 from recovery Method, it is characterised in that comprise the following steps：(1) pH for adjusting leachate is 1.5~2.0, and addition oxidant makes ferrous oxidising into ferric iron；(2) regulation system pH is 2.5~3.5, is aged, and filtering, obtains filtrate and iron aluminum slag；(3) regulation system pH is 4.5~5.0 again, is aged, and filtering, is purified liquid and aluminium slag；(4) regulation system pH in step (2) is added using the aluminium slag that step (3) obtains as pH adjusting agent, so as to iron removaling, obtains iron Aluminium slag；(5) circulation above-mentioned steps realize the lasting iron removaling of leachate, aluminium.
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| CN201710872175.5A CN107871912B (en) | 2017-09-25 | 2017-09-25 | Method for removing iron and aluminum from leachate generated during recovery of valuable metals in waste lithium ion batteries |
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| EP4194572A4 (en) * | 2020-08-25 | 2024-01-24 | Hunan Brunp Recycling Tech Co Ltd | Method for recycling iron and aluminum in nickel-cobalt-manganese solution |
| CN112126783B (en) * | 2020-08-25 | 2022-06-14 | 湖南邦普循环科技有限公司 | Recycling method of iron and aluminum in nickel-cobalt-manganese solution |
| US11760655B2 (en) | 2020-08-25 | 2023-09-19 | Hunan Brunp Recycling Technology Co., Ltd. | Method for recycling iron and aluminum in nickel-cobalt-manganese solution |
| CN112126783A (en) * | 2020-08-25 | 2020-12-25 | 湖南邦普循环科技有限公司 | Recycling method of iron and aluminum in nickel-cobalt-manganese solution |
| CN114853078A (en) * | 2022-05-12 | 2022-08-05 | 中国科学院过程工程研究所 | Method for removing iron and aluminum from iron and aluminum-containing solution and recycling aluminum |
| CN114853078B (en) * | 2022-05-12 | 2023-09-29 | 中国科学院过程工程研究所 | Method for removing iron and aluminum from iron-aluminum-containing solution and recycling aluminum |
| CN115180661A (en) * | 2022-07-22 | 2022-10-14 | 余姚市鑫和电池材料有限公司 | Method for recovering nickel-cobalt-copper mixed sulfate from iron-aluminum waste residues |
| CN115180661B (en) * | 2022-07-22 | 2024-02-13 | 余姚市鑫和电池材料有限公司 | Method for recovering nickel-cobalt-copper mixed sulfate from iron-aluminum waste residues |
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