CN109881008A - A kind of method that reduction roasting-water quenching recycles lithium in waste and old lithium ion battery - Google Patents
A kind of method that reduction roasting-water quenching recycles lithium in waste and old lithium ion battery Download PDFInfo
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- CN109881008A CN109881008A CN201910143935.8A CN201910143935A CN109881008A CN 109881008 A CN109881008 A CN 109881008A CN 201910143935 A CN201910143935 A CN 201910143935A CN 109881008 A CN109881008 A CN 109881008A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The present invention relates to the methods of lithium in a kind of reduction roasting-water quenching recycling waste and old lithium ion battery, belong to old and useless battery recovery technology field.The present invention after waste and old lithium ion battery is discharged using Mechanical Crushing the following steps are included: sieve to obtain anode waste powder；Anode waste powder is uniformly mixed with reducing agent, obtains mixture；Mixture is subjected to reduction roasting；Mixture after reduction roasting is put into rapidly and carries out water quenching in water, lithium, which enters in water, in mixture obtains rich lithium solution, and the rate of recovery of lithium is 92%-98% in waste and old lithium ion battery.Efficient, the Selective Separation of lithium in waste and old lithium ion battery can be achieved in the present invention, and process flow is simple and convenient to operate, and solves the problems such as previous complex technical process, investment cost are big, cost recovery is high.
Description
Technical field
The invention belongs to old and useless battery recovery technology fields, and in particular to a kind of reduction roasting-waste and old lithium of water quenching recycling
The method of lithium in ion battery.
Background technique
Lithium ion battery is because having that voltage is high, specific capacity is big, the service life is long and the remarkable advantages such as memory-less effect, from its business
Just the power source market of walkie electronic apparatus equipment has quickly been captured since change.Since 2010, new-energy automobile industry
Increase and advance swiftly unhindered, lithium-ion-power cell yield increases year by year.And the service life of power lithium-ion battery is in 5-8, often
Year, there are about the power batteries for accounting for total amount 15% to scrap.It is shown according to industry related data, arrives the year two thousand twenty China power lithium-ion battery
Learies are up to about 500,000 tons；By 2023, learies were up to about 1,160,000 tons.Contain lithium, cobalt, nickel in lithium ion battery
Etc. national strategies metal, arbitrarily abandon the not only wasting of resources, but also pollute environment.According to China's future power lithium-ion battery
Learies speculate that by 2023, the market value of recyclable valuable metal be can achieve: 14,600,000,000 yuan of lithium, 8,400,000,000 yuan of nickel, cobalt
7300000000 yuan, 8.5 hundred million yuan of manganese realize that the clean and effective recycling of metal in lithium ion battery is of great significance.Currently, discarded lithium from
The recycling of sub- battery is concentrated mainly on nickel, cobalt, copper, manganese, aluminium valuable metal, and the process of recycling is mainly waste lithium ion
Electric discharge, physics dismantling, acid or alkali leach metal ion, solvent extraction and separation metallic element.With the increase to lithium resource demand,
The recycling of lithium in waste battery becomes more and more concerned, also more and more important.Currently, in waste and old lithium ion battery lithium recycling
Method is mainly sulfuric acid leaching technique.Sulfuric acid leaching technique basic process is that waste lithium ion cell anode material is molten in sulfuric acid
Solution then adjusts pH of leaching solution to alkalinity with sodium carbonate, the lithium ion in leachate is made to form lithium carbonate precipitating.Due to sulfuric acid
Lixiviation process is selectively weak, and the metals such as aluminium, copper, iron, nickel, cobalt, manganese for coexisting in positive electrode with lithium will be synchronized to leach, in and
Shi Wufa depth removes, and to obtain qualified lithium carbonate product, need to realize the simultaneous removing of above-mentioned several metals, difficulty is very big.
There are some methods for recycling lithium from waste and old lithium ion battery at present, but is had the following disadvantages in these methods.
(1) patent CN 201611186511.2 joined the auxiliary material of chlorine-containing polymer, polyvinyl chloride and poly- third during recycling lithium
Then ethylene etc. carries out ball mill mixing, so that process flow is complicated.(2) patent CN201711355295.4 uses sulfuric acid solution
Electrode material after impregnation-calcination, obtains acid leaching liquor, with the Li of PC-88A extraction and separation leachate, will add in water phase after extraction
Enter carbonate, is separated by filtration to obtain Li2CO3Product, the method process flow is complicated, and the period is long.(3) patent CN
201810265725.1, which are added oxidant first into waste lithium ion cell anode material, carries out oxidation reaction, will by auxiliary agent
Lithium is converted into water-soluble lithium salts, then leaches obtained water-soluble lithium salts in water or acid solution, rich lithium is obtained after filtering
Solution and leach residue, the method needs to be added the auxiliary agents such as sodium sulphate, potassium sulfate, ammonium sulfate, while need in acid solution into
Row leaches, complex process, increases cost.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of efficient and Selective Separation lithium, work
The method that skill process was simple and convenient to operate, reduced lithium in reduction roasting-water quenching recycling waste and old lithium ion battery of cost.
The invention is realized by the following technical scheme:
A kind of method that reduction roasting-water quenching recycles lithium in waste and old lithium ion battery, which is characterized in that the method packet
Include following steps:
(1) anode waste powder is obtained using Mechanical Crushing after waste and old lithium ion battery being discharged；
(2) anode waste powder is uniformly mixed with reducing agent, obtains mixture；
(3) mixture is subjected to reduction roasting；
(4) mixture after reduction roasting is put into rapidly and carries out water quenching in water, lithium, which enters, in mixture obtains richness in water
Lithium solution.
According to above-mentioned method, which is characterized in that waste and old lithium ion battery is waste lithium manganese oxide battery, waste and old cobalt acid lithium electricity
One of pond, waste and old nickle cobalt lithium manganate battery, waste and old nickel cobalt lithium aluminate battery are a variety of.
According to above-mentioned method, which is characterized in that reducing agent is graphite cathode powder, charcoal, active carbon, contains in step (2)
Carbon negative pole material, H2, one of CO or a variety of.
According to above-mentioned method, which is characterized in that the additional amount of reducing agent is positive waste powder quality in step (2)
30%~50%.
According to above-mentioned method, which is characterized in that it is 800 DEG C that mixture is carried out to the temperature of reduction roasting in step (3)
~1200 DEG C.
According to above-mentioned method, which is characterized in that mixture is carried out to the time of reduction roasting for 30min in step (3)
~180min.
According to above-mentioned method, which is characterized in that the water quenching time is 5min~30min in step (4).
According to above-mentioned method, which is characterized in that the rate of recovery of lithium is 92%-98% in step (4) mixture.
Advantageous effects of the invention: compared with prior art, reducing agent used in (1) present invention may be derived from old and useless battery
Itself or common marketable material, cost is relatively low；(2) only the relatively low reducing agent of a certain amount of cost need to be added in the present invention, by also
Efficiently separating for lithium and unclassified stores in waste and old lithium ion battery can be realized in former calcining-water quenching；(3) the method for the present invention makes waste and old
The rate of recovery of lithium is 92%-98% in lithium ion battery, and is free of other metal impurities in rich lithium solution；Rich lithium solution can root
According to market demand direct preparation of high-purity lithium salts product, such as battery-level lithium carbonate or LITHIUM BATTERY lithium hydroxide, solid material after water quenching
Hydrometallurgic recovery can be used in the metallic elements such as the cobalt, nickel, the manganese that are rich in, prepares corresponding high-purity salt product.(4) present invention process stream
Journey is simple, easy to operate, solves the problems such as previous complex technical process, investment cost are big, cost recovery is high, is conducive to industry
Change.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the invention will be further described.
Referring to Fig. 1, the method for lithium in a kind of reduction roasting of the invention-water quenching recycling waste and old lithium ion battery, including
Following steps: (1) anode waste powder is obtained using Mechanical Crushing after waste and old lithium ion battery being discharged；Applying waste lithium ionic
Battery is waste lithium manganese oxide battery, in waste and old cobalt acid lithium battery, waste and old nickle cobalt lithium manganate battery, waste and old nickel cobalt lithium aluminate battery
It is one or more.(2) anode waste powder is uniformly mixed with reducing agent, obtains mixture；Reducing agent is graphite cathode powder, wood
Charcoal, contains carbon negative pole material, H at active carbon2, one of CO or a variety of.The additional amount of reducing agent is positive waste powder quality
30%~50%.(3) mixture is subjected to reduction roasting；The temperature that mixture carries out reduction roasting is 800 DEG C~1200 DEG C.It is mixed
It closes object and carries out the time of reduction roasting as 30min~180min.(4) mixture after reduction roasting is put into rapidly in water and is carried out
Water quenching 5min~30min, lithium, which enters in water, in mixture obtains rich lithium solution, and rest materials are separated by filtration into slag, make lithium
It is efficiently separated with unclassified stores.The rate of recovery of lithium is 92%-98% in mixture, and is free of other gold in rich lithium solution
Belong to impurity.
Embodiment 1
It sorts to obtain anode waste powder using Mechanical Crushing after waste lithium manganese oxide battery is discharged；By anode waste
Powder and graphite cathode powder are uniformly mixed to get mixture, and the additional amount of graphite cathode powder is the 30% of positive waste powder quality；It will
Mixture, which is put into Muffle furnace, carries out reduction roasting；Maturing temperature is 800 DEG C, calcining time 30min；After reduction roasting
Mixture puts into carry out water quenching in water rapidly, and the water quenching time is 5min, and lithium, which enters in water, in mixture obtains rich lithium solution, passes through
Filtering efficiently separates lithium with unclassified stores.The rate of recovery of lithium is 93% in waste lithium manganese oxide battery.
Embodiment 2
It sieves to obtain anode waste powder using Mechanical Crushing after waste and old cobalt acid lithium battery is discharged；By anode waste
Powder and charcoal are uniformly mixed to get mixture, and the additional amount of charcoal is the 40% of positive waste powder quality；Mixture is put into horse
Reduction roasting is not carried out in furnace；Maturing temperature is 1000 DEG C, calcining time 60min；Mixture after reduction roasting is rapid
Water quenching is carried out in investment water, the water quenching time is 20min, and lithium, which enters in water, in mixture obtains rich lithium solution, makes lithium by filtering
It is efficiently separated with unclassified stores.The rate of recovery of lithium is 96% in waste and old cobalt acid lithium battery.
Embodiment 3
It sieves to obtain anode waste powder using Mechanical Crushing after waste and old nickle cobalt lithium manganate ternary battery is discharged；It will
Anode waste powder and active carbon are uniformly mixed to get mixture, and the additional amount of active carbon is the 50% of positive waste powder quality；It will
Mixture, which is put into Muffle furnace, carries out reduction roasting；Maturing temperature is 1200 DEG C, calcining time 180min；After reduction roasting
Mixture put into carry out water quenching in water rapidly, the water quenching time is 30min, and lithium, which enters in water, in mixture obtains rich lithium solution,
Lithium is efficiently separated with unclassified stores by filtering.The rate of recovery of lithium is 98% in waste and old nickle cobalt lithium manganate ternary battery.
The embodiment of the present invention is explained in detail for above-mentioned combination attached drawing, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be in the premise for not departing from present inventive concept
Lower various changes can be made, belongs to technical scope of the invention.
Claims (8)
1. the method for lithium in a kind of reduction roasting-water quenching recycling waste and old lithium ion battery, which is characterized in that the method includes
Following steps:
(1) it sieves to obtain anode waste powder using Mechanical Crushing after waste and old lithium ion battery being discharged；
(2) anode waste powder is uniformly mixed with reducing agent, obtains mixture；
(3) mixture is subjected to reduction roasting；
(4) mixture after reduction roasting is put into rapidly and carries out water quenching in water, lithium enters in water that obtain rich lithium molten in mixture
Liquid.
2. the method according to claim 1, wherein waste and old lithium ion battery is waste lithium manganese oxide battery, waste and old
One of cobalt acid lithium battery, waste and old nickle cobalt lithium manganate ternary battery, waste and old nickel cobalt lithium aluminate ternary battery are a variety of.
3. the method according to claim 1, wherein reducing agent is graphite cathode powder, charcoal, work in step (2)
Property charcoal, contain carbon negative pole material, H2, one of CO or a variety of.
4. the method according to claim 1, wherein the additional amount of reducing agent is positive waste powder in step (2)
The 30%~50% of quality.
5. the method according to claim 1, wherein mixture to be carried out to the temperature of reduction roasting in step (3)
It is 800 DEG C~1200 DEG C.
6. according to the method described in claim 5, it is characterized in that, mixture to be carried out to the time of reduction roasting in step (3)
For 30min~180min.
7. the method according to claim 1, wherein the water quenching time is 5min~30min in step (4).
8. the method according to claim 1, wherein the rate of recovery of lithium is in step (4) waste and old lithium ion battery
92%-98%.
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| CN201910143935.8A CN109881008A (en) | 2019-02-27 | 2019-02-27 | A kind of method that reduction roasting-water quenching recycles lithium in waste and old lithium ion battery |
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| CN201910143935.8A CN109881008A (en) | 2019-02-27 | 2019-02-27 | A kind of method that reduction roasting-water quenching recycles lithium in waste and old lithium ion battery |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110165324A (en) * | 2019-06-24 | 2019-08-23 | 中国科学院青海盐湖研究所 | A kind of method and system recycling anode and Regeneration and Repair from waste lithium cell |
| CN110265742A (en) * | 2019-06-24 | 2019-09-20 | 中国科学院青海盐湖研究所 | Recycling prepares the method and system of composite positive pole from leftover bits and substandard products |
| CN110828927A (en) * | 2019-10-18 | 2020-02-21 | 广西银亿新材料有限公司 | Method for comprehensively recovering waste lithium ion batteries |
| CN111009699A (en) * | 2019-11-26 | 2020-04-14 | 宁夏百川新材料有限公司 | Method for recycling lithium manganate waste battery |
| CN111118294A (en) * | 2020-01-15 | 2020-05-08 | 北京矿冶科技集团有限公司 | Method for recycling valuable metals from waste lithium ion battery materials step by step |
| CN111430829A (en) * | 2020-03-11 | 2020-07-17 | 中南大学 | Method for recycling and regenerating waste lithium battery anode material under assistance of biomass waste |
| CN111979415A (en) * | 2020-07-01 | 2020-11-24 | 湖南雅城新材料有限公司 | Method for recovering waste lithium cobaltate positive electrode material without strong acid leaching |
| CN112575203A (en) * | 2020-12-07 | 2021-03-30 | 金川集团股份有限公司 | Method for recycling lithium in waste power lithium battery |
| CN112680598A (en) * | 2020-12-15 | 2021-04-20 | 中南大学 | Method for low-cost clean treatment of waste lithium ion battery anode material |
| CN113117637A (en) * | 2021-04-19 | 2021-07-16 | 重庆大学 | Method for preparing carbon dioxide adsorbing material by using waste lithium cobaltate battery as raw material |
| WO2021218510A1 (en) * | 2020-05-01 | 2021-11-04 | XProEM Ltd. | Process for recovering lithium and transition metals from waste cathode of spent lithium ion battery |
| CN113999967A (en) * | 2021-11-02 | 2022-02-01 | 赣州有色冶金研究所有限公司 | Method for recovering lithium in lithium ion battery anode material |
| US20220194806A1 (en) * | 2020-12-22 | 2022-06-23 | Pukyong National University Industry-University Cooperation Foundation | Lithium oxide recovery method from lithium manganese oxide (lmo) |
| CN115072747A (en) * | 2022-05-31 | 2022-09-20 | 湖南力合厚浦科技有限公司 | Lithium carbonate recovery method and device |
| WO2022193781A1 (en) * | 2021-03-17 | 2022-09-22 | 广东邦普循环科技有限公司 | Regeneration method for waste ternary positive electrode material, and use thereof |
| CN115354161A (en) * | 2022-08-29 | 2022-11-18 | 通化建新科技有限公司 | Method for recycling lithium from waste power batteries by rotary hearth furnace |
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| CN110165324A (en) * | 2019-06-24 | 2019-08-23 | 中国科学院青海盐湖研究所 | A kind of method and system recycling anode and Regeneration and Repair from waste lithium cell |
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| CN111009699A (en) * | 2019-11-26 | 2020-04-14 | 宁夏百川新材料有限公司 | Method for recycling lithium manganate waste battery |
| CN111118294A (en) * | 2020-01-15 | 2020-05-08 | 北京矿冶科技集团有限公司 | Method for recycling valuable metals from waste lithium ion battery materials step by step |
| CN111430829A (en) * | 2020-03-11 | 2020-07-17 | 中南大学 | Method for recycling and regenerating waste lithium battery anode material under assistance of biomass waste |
| WO2021218510A1 (en) * | 2020-05-01 | 2021-11-04 | XProEM Ltd. | Process for recovering lithium and transition metals from waste cathode of spent lithium ion battery |
| CN111979415B (en) * | 2020-07-01 | 2022-06-17 | 湖南雅城新材料有限公司 | Method for recovering waste lithium cobaltate positive electrode material without strong acid leaching |
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| CN112575203A (en) * | 2020-12-07 | 2021-03-30 | 金川集团股份有限公司 | Method for recycling lithium in waste power lithium battery |
| CN112680598A (en) * | 2020-12-15 | 2021-04-20 | 中南大学 | Method for low-cost clean treatment of waste lithium ion battery anode material |
| US20220194806A1 (en) * | 2020-12-22 | 2022-06-23 | Pukyong National University Industry-University Cooperation Foundation | Lithium oxide recovery method from lithium manganese oxide (lmo) |
| WO2022193781A1 (en) * | 2021-03-17 | 2022-09-22 | 广东邦普循环科技有限公司 | Regeneration method for waste ternary positive electrode material, and use thereof |
| GB2618688A (en) * | 2021-03-17 | 2023-11-15 | Guangdong Brunp Recycling Technology Co Ltd | Regeneration method for waste ternary positive electrode material, and use thereof |
| ES2962915A1 (en) * | 2021-03-17 | 2024-03-21 | Guangdong Brunp Recycling Technology Co Ltd | Regeneration method for waste ternary positive electrode material, and use thereof |
| CN113117637A (en) * | 2021-04-19 | 2021-07-16 | 重庆大学 | Method for preparing carbon dioxide adsorbing material by using waste lithium cobaltate battery as raw material |
| CN113999967A (en) * | 2021-11-02 | 2022-02-01 | 赣州有色冶金研究所有限公司 | Method for recovering lithium in lithium ion battery anode material |
| CN115072747A (en) * | 2022-05-31 | 2022-09-20 | 湖南力合厚浦科技有限公司 | Lithium carbonate recovery method and device |
| CN115354161A (en) * | 2022-08-29 | 2022-11-18 | 通化建新科技有限公司 | Method for recycling lithium from waste power batteries by rotary hearth furnace |
| CN115354161B (en) * | 2022-08-29 | 2024-02-02 | 通化建新科技有限公司 | Method for recycling lithium in waste power battery by rotary hearth furnace |
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Effective date of registration: 20191023 Address after: 537624 Longtan Industrial Park, Bobai County, Yulin City, Guangxi Zhuang Autonomous Region Applicant after: Guangxi Silver billion new material Co., Ltd. Applicant after: Guangxi Yinyi high tech R & D Co., Ltd. Address before: 537624 Yulin Longtan Industrial Park, Yulin City, Guangxi Zhuang Autonomous Region Applicant before: Guangxi Silver billion new material Co., Ltd. |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190614 |