CN110396600A - The lithium recovery process of waste and old lithium ion battery - Google Patents
The lithium recovery process of waste and old lithium ion battery Download PDFInfo
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- CN110396600A CN110396600A CN201910689453.2A CN201910689453A CN110396600A CN 110396600 A CN110396600 A CN 110396600A CN 201910689453 A CN201910689453 A CN 201910689453A CN 110396600 A CN110396600 A CN 110396600A
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- lithium
- waste
- ion battery
- lithium ion
- roasting
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
- C22B3/1608—Leaching with acyclic or carbocyclic agents
- C22B3/1616—Leaching with acyclic or carbocyclic agents of a single type
- C22B3/165—Leaching with acyclic or carbocyclic agents of a single type with organic acids
-
- 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
-
- 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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- 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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- Chemical & Material Sciences (AREA)
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- Mechanical Engineering (AREA)
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- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Primary Cells (AREA)
Abstract
The present invention provides a kind of lithium recovery process of waste and old lithium ion battery, waste and old lithium ion battery is crushed first and sorts to obtain positive and negative anodes active material powder and diaphragm, positive and negative anodes active material powder and diaphragm that sorting obtains are placed in the roasting kiln roasting certain time that temperature is 600~650 DEG C with certain mass ratio later, then product of roasting is leached using oxalic acid solution, nickel cobalt manganese slag and lithium oxalate solution is obtained by filtration, calcium hydroxide is finally added into lithium oxalate solution to be reacted, lithium hydroxide solution and calcium oxalate is obtained by filtration, obtained calcium oxalate is added in sulfuric acid and carries out acidification, oxalic acid solution is obtained by filtration.The method of the present invention, simple process, novelty, the lithium hydroxide solution purity is high recycled, the rate of recovery are high.
Description
Technical field
The present invention relates to a kind of lithium recovery process of waste and old lithium ion battery.
Background technique
With the development of new-energy automobile, a large amount of lithium ion batteries enter market, but lithium ion battery has certain make
With the service life, need replacing after a period of use, so that more waste and old lithium ion battery is generated, and in waste and old lithium ion battery
Containing more precious metals, if do not handled, a large amount of waste will cause, while pollution will also result in environment, therefore useless
The recycling and reuse problem of old lithium ion battery also becomes industry significant challenge.Lithium returns in traditional waste and old lithium ion battery
Receive, substantially by acidleach, removal of impurities, extraction and separation and etc. progress, have that long flow path, investment is big, lithium is mingled with so that the rate of recovery
It is low, be difficult to the problems such as purification process.
Summary of the invention
The present invention is intended to provide a kind of simple process, novelty, product recovery rate are high, the biggish waste and old lithium ion battery of value
Lithium recovery process.
The present invention is realized by the following scheme:
A kind of lithium recovery process of waste and old lithium ion battery, carries out according to the following steps,
(a) waste and old lithium ion battery is crushed and sorts to obtain positive and negative anodes active material powder and diaphragm；It is broken to include
Rough and torn, two steps of thin broken；Sorting the nickel mass content in obtained positive and negative anodes active material powder is that 15~20%, cobalt quality contains
Amount is 7~12%, manganese mass content is 14~18%, lithium mass content is 3~7%, and the diaphragm ingredient sorted is poly- second
One or both of alkene, polypropylene；
(b) sorting obtains in step (a) positive and negative anodes active material powder and diaphragm are placed in temperature with certain mass ratio
For 600~650 DEG C of roasting kiln roasting certain time；
(c) product of roasting for obtaining step (b) is leached using oxalic acid solution, and nickel cobalt manganese slag is obtained by filtration and lithium oxalate is molten
Liquid；
(d) calcium hydroxide is added into the lithium oxalate solution that step (c) obtains to be reacted, it is molten that lithium hydroxide is obtained by filtration
Obtained calcium oxalate is added in sulfuric acid and carries out acidification, oxalic acid solution and calcium sulphate solid is obtained by filtration by liquid and calcium oxalate,
Oxalic acid solution can be recycled.
Further, in the step (b), the addition quality of diaphragm be positive negative electrode active material powder be added quality 10~
20%, reduction roasting atmosphere is formed in roaster.The effect of diaphragm not only can provide fuel, but also can to form reduction in roaster
Atmosphere is roasted, ternary material in lithium ion battery is restored in reduction atmosphere, makes elemental lithium and ternary metal element connecting key
It interrupts, in favor of subsequent leaching.
Further, in the step (b), calcining time control is 3~5h.
In order to enable leaching efficiency maximizes, in the step (c), the solid-to-liquid ratio of product of roasting and oxalic acid solution is 15~
15~50g product of roasting can be added in 50g:1L, that is, 1L oxalic acid solution, the molar concentration of oxalic acid is 0.2~2mol/l, is leached anti-
Answering temperature control control is 50~95 DEG C, and the control of Leach reaction time is 0.2~4h.
Further, in the step (d), the molar ratio of lithium oxalate solution and calcium hydroxide is 1:1.15~1.2, reaction
Time control is 4~6h, at room temperature.
Further, in the step (d), the molar ratio of calcium oxalate and sulfuric acid is 1:1.25~1.3, and the quality of sulfuric acid is dense
Degree is 30~40%, and the control of acidification temperature is 70~80 DEG C, and the control of acidification time is 1~3h.
The lithium recovery process of waste and old lithium ion battery of the invention, simple process, novelty directly utilize applying waste lithium ionic electricity
The positive and negative anodes active material powder and diaphragm that pond is handled carry out oxalic acid leaching and calcium hydroxide processing, directly make after being fired
Standby to obtain lithium hydroxide product, lithium hydroxide product purity is high, the rate of recovery is high, and no nickel cobalt manganese is mingled with, and oxalic acid solution is recyclable
It uses, realizes low cost, the efficient lithium resource recycled in waste and old lithium ion battery.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited to the statements of embodiment.
Embodiment 1
A kind of lithium recovery process of waste and old lithium ion battery, carries out according to the following steps,
(a) waste and old lithium ion battery is crushed and sorts to obtain positive and negative anodes active material powder and diaphragm；It is broken to include
Rough and torn, two steps of thin broken；It is detected, the nickel mass content in positive and negative anodes active material powder sorted is 16%, cobalt matter
Amount content is 10%, manganese mass content is 15%, lithium mass content is 7%, and the diaphragm ingredient sorted is polyethylene；
(b) sorting obtains in step (a) positive and negative anodes active material powder and diaphragm are placed in the roaster that temperature is 600 DEG C
Middle roasting 3h, the addition quality of septation be positive negative electrode active material powder be added quality 11%；
(c) product of roasting for obtaining step (b) is leached using oxalic acid solution, and nickel cobalt manganese slag is obtained by filtration and lithium oxalate is molten
Liquid, wherein the solid-to-liquid ratio of product of roasting and oxalic acid solution is 25g:1L, and the molar concentration of oxalic acid is 0.5mol/l, Leach reaction temperature
Control control is 65 DEG C, and the control of Leach reaction time is 1.5h；It is chemically examined lithium leaching rate and reaches 90%；
(d) calcium hydroxide is added into the lithium oxalate solution that step (c) obtains to be reacted, lithium oxalate solution and hydroxide
The molar ratio of calcium is 1:1.15, and reaction time control at room temperature is 4h, and lithium hydroxide solution and calcium oxalate are obtained by filtration later, will
Obtained calcium oxalate, which is added in sulfuric acid, carries out acidification, and the molar ratio of calcium oxalate and sulfuric acid is 1:1.25, and the quality of sulfuric acid is dense
Degree is 30%, and the control of acidification temperature is 70 DEG C, and the control of acidification time is 1h, and oxalic acid is obtained by filtration and calcium sulfate is solid
Body, oxalic acid solution can be recycled.
Embodiment 2
A kind of lithium of waste and old lithium ion battery in the lithium recovery process of waste and old lithium ion battery, step and embodiment 1
The step of recovery process, is essentially identical, the difference is that:
1, in step (a), through detecting, in step (a), the nickel mass content in positive and negative anodes active material powder that sorts
For 19%, cobalt mass content be 8%, manganese mass content is 18%, lithium mass content is 5%, and the diaphragm ingredient sorted is
Polyethylene and polypropylene；
2, in step (b), calciner temperature control is 650 DEG C, and the addition quality of the diaphragm negative electrode active material powder that is positive adds
Enter the 20% of quality, calcining time control is 5h；
3, in step (c), the solid-to-liquid ratio of product of roasting and oxalic acid solution is 15g:1L, and the molar concentration of oxalic acid is
1.5mol/l, Leach reaction temperature control control are 50 DEG C, and the control of Leach reaction time is 4h, are chemically examined lithium leaching rate and reach 95%；
4, in step (d), the molar ratio of lithium oxalate solution and calcium hydroxide is 1:1.2, and reaction time control at room temperature is
The molar ratio of 6h, calcium oxalate and sulfuric acid is 1:1.3, and the mass concentration of sulfuric acid is 40%, and the control of acidification temperature is 80 DEG C, acid
Changing the control of processing time is 2h.
Embodiment 3
A kind of lithium of waste and old lithium ion battery in the lithium recovery process of waste and old lithium ion battery, step and embodiment 1
The step of recovery process, is essentially identical, the difference is that:
1, in step (a), through detecting, in step (a), the nickel mass content in positive and negative anodes active material powder that sorts
For 17%, cobalt mass content be 7%, manganese mass content is 15.5%, lithium mass content is 6%, the diaphragm ingredient sorted
For polyethylene and polypropylene；
2, in step (b), calciner temperature control is 625 DEG C, and the addition quality of the diaphragm negative electrode active material powder that is positive adds
Enter the 18% of quality, calcining time control is 4h；
3, in step (c), the solid-to-liquid ratio of product of roasting and oxalic acid solution is 45g:1L, and the molar concentration of oxalic acid is 2mol/
L, Leach reaction temperature control control are 90 DEG C, and the control of Leach reaction time is 0.5h, are chemically examined lithium leaching rate and reach 93%；
4, in step (d), the molar ratio of lithium oxalate solution and calcium hydroxide is 1:1.2, and reaction time control at room temperature is
The molar ratio of 5h, calcium oxalate and sulfuric acid is 1:1.28, and the mass concentration of sulfuric acid is 35%, and the control of acidification temperature is 75 DEG C,
The control of acidification time is 3h.
Claims (6)
1. a kind of lithium recovery process of waste and old lithium ion battery, it is characterised in that: it carries out according to the following steps,
(a) waste and old lithium ion battery is crushed and sorts to obtain positive and negative anodes active material powder and diaphragm；
(b) sorting obtains in step (a) positive and negative anodes active material powder and diaphragm are placed in temperature with certain mass ratio as 600
~650 DEG C of roasting kiln roasting certain time；
(c) product of roasting for obtaining step (b) is leached using oxalic acid solution, and nickel cobalt manganese slag and lithium oxalate solution is obtained by filtration；
(d) into the lithium oxalate solution that step (c) obtains be added calcium hydroxide reacted, be obtained by filtration lithium hydroxide solution and
Obtained calcium oxalate is added in sulfuric acid and carries out acidification, oxalic acid solution and calcium sulphate solid is obtained by filtration by calcium oxalate.
2. the lithium recovery process of waste and old lithium ion battery as described in claim 1, it is characterised in that: in the step (b), every
The addition quality of the film negative electrode active material powder that is positive is added the 10~20% of quality, and reduction roasting atmosphere is formed in roaster.
3. the lithium recovery process of waste and old lithium ion battery as claimed in claim 2, it is characterised in that: in the step (b), roasting
Burning time control is 3~5h.
4. the lithium recovery process of waste and old lithium ion battery as described in claim 1, it is characterised in that: in the step (c), roasting
The solid-to-liquid ratio for burning product and oxalic acid solution is 15~50g:1L, and the molar concentration of oxalic acid is 0.2~2mol/l, Leach reaction temperature control
Control is 50~95 DEG C, and the control of Leach reaction time is 0.2~4h.
5. the lithium recovery process of waste and old lithium ion battery as described in claim 1, it is characterised in that: in the step (d), grass
The molar ratio of sour lithium solution and calcium hydroxide is 1:1.15~1.2, and reaction time control is 4~6h.
6. the lithium recovery process of the waste and old lithium ion battery as described in Claims 1 to 5 is any, it is characterised in that: the step
(d) in, the molar ratio of calcium oxalate and sulfuric acid is 1:1.25~1.3, and the mass concentration of sulfuric acid is 30~40%, acidification temperature
Control is 70~80 DEG C, and the control of acidification time is 1~3h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760686A (en) * | 2019-12-13 | 2020-02-07 | 九江天赐高新材料有限公司 | Method for recovering lithium from waste lithium ion battery |
| CN110964927A (en) * | 2019-12-26 | 2020-04-07 | 甘肃睿思科新材料有限公司 | Neutralization treatment method for liquid after nickel and cobalt precipitation |
| CN113871744A (en) * | 2021-09-06 | 2021-12-31 | 北京科技大学 | Method for recycling waste lithium ion battery anode active material |
| CN114085999A (en) * | 2021-11-24 | 2022-02-25 | 昆明理工大学 | Method for recovering valuable metals from lithium battery anode leaching waste liquid |
| CN114335781A (en) * | 2021-12-27 | 2022-04-12 | 上海电力大学 | Method for extracting precious metal from waste lithium battery |
| CN114752769A (en) * | 2022-04-08 | 2022-07-15 | 中国矿业大学 | Method for recovering valuable metals of waste lithium battery materials by aid of pyrolysis of diaphragms |
| CN115566307A (en) * | 2022-11-15 | 2023-01-03 | 湖南五创循环科技有限公司 | Method for recovering high-purity lithium oxalate and high-purity lithium hydroxide from disassembled black powder of waste lithium battery and/or waste cathode powder of lithium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110760686A (en) * | 2019-12-13 | 2020-02-07 | 九江天赐高新材料有限公司 | Method for recovering lithium from waste lithium ion battery |
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| CN114752769A (en) * | 2022-04-08 | 2022-07-15 | 中国矿业大学 | Method for recovering valuable metals of waste lithium battery materials by aid of pyrolysis of diaphragms |
| CN114752769B (en) * | 2022-04-08 | 2023-09-22 | 中国矿业大学 | Method for recycling valuable metals of waste lithium battery materials assisted by diaphragm pyrolysis |
| CN115566307A (en) * | 2022-11-15 | 2023-01-03 | 湖南五创循环科技有限公司 | Method for recovering high-purity lithium oxalate and high-purity lithium hydroxide from disassembled black powder of waste lithium battery and/or waste cathode powder of lithium battery |
| CN115566307B (en) * | 2022-11-15 | 2023-03-24 | 湖南五创循环科技有限公司 | Method for recovering high-purity lithium oxalate and high-purity lithium hydroxide from waste lithium battery |
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Application publication date: 20191101 |