CN107180991A - A kind of method of waste lithium cell recycling - Google Patents
A kind of method of waste lithium cell recycling Download PDFInfo
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- CN107180991A CN107180991A CN201710311098.6A CN201710311098A CN107180991A CN 107180991 A CN107180991 A CN 107180991A CN 201710311098 A CN201710311098 A CN 201710311098A CN 107180991 A CN107180991 A CN 107180991A
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- Prior art keywords
- lithium cell
- waste lithium
- positive electrode
- aniline
- cell recycling
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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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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Primary Cells (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a kind of method of waste lithium cell recycling, waste lithium cell is placed in protection gas and disassembled by (1), obtains active positive electrode material；(2) active positive electrode material is collected, then is cleaned with deionized water and ethanol；(3) the material dried recovered after cleaning is utilized；(4) under room temperature condition, material after appropriate drying is taken, is added in aniline solution, add a certain amount of ammonium persulfate-sodium bisulfate, produce SO4 -Oxidative degradation aniline.Compared with prior art, timeliness of the present invention is short, simple to operate, on the one hand solves the problems, such as the secondary pollution that waste lithium cell pollution environment and METAL EXTRACTION are caused；On the other hand the processing of difficult degradation sewage is used it for, processing cost has been saved, has created environmental benefit.
Description
Technical field
The invention belongs to field of environment protection, more particularly, to a kind of method of waste lithium cell recycling.
Background technology
Battery is widely present in various electronic products and electric automobile as a kind of power storage devices, with the public
Increase to electronic product demand, the consumption figure of battery also gradually increases.In US and European, it is estimated that 8,000,000,000 can be consumed every year
Battery；In Japan, only 2004,6,000,000,000 batteries with regard to production and consumption.In China, the learies of battery are even more surprising,
Scrap about 10,000,000,000 refuse batteries, about 300,000 tons of weight every year；, will if these batteries are not added with any processing and concentrate landfill
Make 10,000,000,000 m3Water body polluted, make nearly 4000k m3Soil lose use function.In waste and old lithium ion battery containing cobalt,
The high value metals such as iron, aluminium, copper, take certain processing means to carry out recycling to old and useless battery, can not only mitigate
Influence to environment, can also realize recycling for resource.
Based on potentiometric titrations (SO4-) high-level oxidation technology (AOPs-SRs) be the drop grown up in recent years
The new and effective water technology of persistent organic pollutants in Xie Shui.Research shows, SO4-Not only in wider pH value (3
~8) in the range of show higher oxidation activity, and SO4 in neutral conditions-Oxidation-reduction potential close in addition it is high
In the OH that oxidisability is extremely strong.Transition metal ion catalyst PMS produces SO4-It is a kind of most widely used method.Meanwhile, it is many
Plant transition metal Cu2+、Co2+、Mn2+、Ni2+、Fe2+、Fe3+、Ru3+、Ce3+And V3+PMS can be catalyzed and produce SO4-·。
Metal in positive active material is focused primarily upon in battery to the recycling of waste and old lithium ion battery research at present
Extraction, but secondary pollution is easily caused in extraction process.Chinese patent CN106129513A discloses a kind of from waste lithium cell
The middle recovery method for reclaiming various materials, is splitted as positive plate, barrier film, negative plate including waste lithium cell, then
Electrode material, adhesive and collector recycling in positive/negative pole piece.The patent removal process is complicated, more use N,
N- dimethylpropionamide equal solvents, and it is related to high-temperature stirring and mixed solvent recovery rectifying, it is also easy to produce toxic and harmful gas, high temperature
Energy consumption increases cost, finally simply isolated electrode material, without further innovative utilization electrode material.In order to more
Plus simple, safe efficient, inexpensive and high benefit recycling waste lithium cell, we propose one kind in the present invention
Innovative recycling technique.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of waste lithium cell is returned
The method recycled is received, technology is simple, effective, the problem of waste lithium cell is handled on the one hand is solved, on the other hand by positive pole
Material is used as catalyst, generates great environmental benefit.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method of waste lithium cell recycling, using following steps：
(1) waste lithium cell is placed in protection gas and disassembled, obtain active positive electrode material；
(2) active positive electrode material is collected, then is cleaned with deionized water and ethanol；
(3) the material dried recovered after cleaning is utilized；
(4) under room temperature condition, material after appropriate drying is taken, is added in aniline solution, add a certain amount of hydrogen persulfate
Potassium complex salt, produces SO4 -Oxidative degradation aniline.
Protection gas described in step (1) is nitrogen or inert gas, and active positive electrode material is based on manganese dioxide.
Step (2) is broken uniform by the positive electrode of collection, with washes of absolute alcohol 3~5 times, then is cleaned with water to solution
Stirred in neutrallty condition, cleaning process, quiescent setting 2~10 minutes, remove supernatant afterwards.
Positive electrode after cleaning is dried in vacuo 12~24h by step (3) at a temperature of 50~70 DEG C.
The amount of the positive electrode added in step (4) is 2~10mg/100ml aniline solutions, and the potassium hydrogen persulfate of addition is answered
The amount for closing salt is 5~20mg/100ml aniline solutions, and the pH value of aniline solution is 6~8, and the concentration of aniline solution is 10-
30ppm。
The present invention carries out safety, simple recovery to waste lithium cell, and removal process is to be effectively utilized waste and scrap again
Environmental protection, is used as catalyst by positive electrode, has saved the material and cost of production catalyst again.Utilize the waste and old lithium of the present invention
The positive electrode of battery is as heterogeneous catalysis, for the high-level oxidation technology aniline degradation waste water based on potentiometric titrations
Catalytic oxidation, under certain conditions, 100% aniline degradation is only needed 60 minutes.This effect close under the same terms,
The material synthesized by the use of prior art is degraded benzene for being catalyzed the class Fenton technology of potentiometric titrations as heterogeneous catalysis
The catalytic oxidation time of amine waste water.The present invention, relative to existing waste lithium cell recovery and utilization technology, simple, direct,
Green, and combine high-level oxidation technology catalysis generation SO4-Pollution degradation waste water, achieves environmental benefit again.
The benefit of the present invention is relative to existing lithium battery recovery and utilization technology, with advantages below：
(1) removal process cost is very cheap, can obtain part benefit by the copper and iron reclaimed in lithium battery, and avoid
The secondary liquid waste pollution that the medicament of METAL EXTRACTION process spends and caused.
(2) positive electrode in lithium battery is used as heterogeneous catalysis, it is possible to recycled for multiple times, has saved catalyst
Production cost.
(3) combine high-level oxidation technology catalysis and produce SO4 -Oxidative degradation waste water, obtains benefit in sewage disposal.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of waste lithium cell positive electrode.
Fig. 2 is the scanning electron microscope (SEM) photograph that waste lithium cell positive electrode is used as before and after catalyst reaction.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.Following examples will be helpful to this area
Technical staff further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the general of this area
For logical technical staff, without departing from the inventive concept of the premise, various modifications and improvements can be made.These are belonged to
Protection scope of the present invention.
Embodiment 1
A kind of method of new waste lithium cell recycling, specifically includes following steps：
(1) waste lithium cell is placed in protection gas, it disassembled with demountor, by the material after disassembling by material
Classified, positive electrode is collected, based on manganese dioxide.
(2) positive electrode collected is broken into fine particle, with washes of absolute alcohol 3 times, then is cleaned with water to solution and be in
Stirred in neutrallty condition, cleaning process, quiescent setting, removes supernatant afterwards.
(3) positive electrode after cleaning, 24h is dried in vacuo at a temperature of 60 DEG C.
(4) manganese bioxide material 3mg is taken, in the aniline solution for being added to the 20ppm that volume 100mlpH is 7, is added
10mg ammonium persulfate-sodium bisulfate.
Fig. 1 is the X-ray diffractogram of the positive electrode based on manganese dioxide, and as can be seen from Figure 1 main component is
Simultaneously there is carbon in manganese dioxide, due to the insertion and abjection of lithium ion during lithium battery use, waste and old anode material of lithium battery
The impurity contained is more, and the crystallinity of manganese dioxide is without so good.
Fig. 2 is the scanning electron microscope (SEM) photograph that positive electrode is used as before and after catalyst reaction, from figure 2 it can be seen that before and after reaction,
It is smooth that catalyst surface becomes, and this is due to rock friction in course of reaction to cause, and front and rear pattern does not have significant change, and explanation is urged
Agent has certain stability.
Embodiment 2
Positive electrode based on manganese dioxide is as heterogeneous catalysis, for the senior oxygen based on potentiometric titrations
The catalytic oxidation of change technology aniline degradation waste water, its detailed process is as follows：
The aniline waste water that 100ml concentration is 20ppm is taken in 250ml conical flask, the potassium hydrogen persulfate for adding 10mg is answered
Salt is closed, 5mg catalyst is subsequently added into.PH value of solution is adjusted into 185mg disodium hydrogen phosphate and 152mg sodium dihydrogen phosphate
Property.Stirring reaction is carried out on the water bath with thermostatic control shaking table that conical flask is placed in 25 DEG C, to add oxidant as time zero, Mei Geyi
The section time takes a sample, and isometric methanol is added immediately and is quenched, after 0.22um membrane filtration, high performance liquid chromatography is used
Instrument (HPLC) is determined, and the degradation efficiency of aniline degradation is calculated according to the relation of the concentration of aniline in solution and absorbance：100% drop
Solving aniline needs 60 minutes, and the recyclable rear recycled for multiple times of catalyst.
Reference examples
α-the MnO synthesized using prior art2As heterogeneous catalysis, for being catalyzed the height based on potentiometric titrations
The catalytic oxidation of level oxidation technology aniline degradation, its detailed process is as follows：
The aniline waste water that 100ml concentration is 20ppm is taken in 250ml conical flask, the potassium hydrogen persulfate for adding 10mg is answered
Salt is closed, 5mg catalyst is subsequently added into.PH value of solution is adjusted into 185mg disodium hydrogen phosphate and 152mg sodium dihydrogen phosphate
Property.Stirring reaction is carried out on the water bath with thermostatic control shaking table that conical flask is placed in 25 DEG C, to add oxidant as time zero, Mei Geyi
The section time takes a sample, and isometric methanol is added immediately and is quenched, after 0.22um membrane filtration, high performance liquid chromatography is used
Instrument (HPLC) is determined, and the degradation efficiency of aniline degradation is calculated according to the relation of the concentration of aniline in solution and absorbance：100% drop
Solving aniline needs 60 minutes.This is basically identical with manganese dioxide catalytic effect in waste lithium cell.
Contrasted by above-described embodiment 2 and using reference examples, with waste lithium cell positive electrode as catalyst and
α-the MnO of synthesis2Catalytic effect is basically identical.This illustrates that the method for the present invention has an actual effect, and has saved synthesis and urge
The cost of agent, has reached recycling, and generate economy and environmental benefit.
Embodiment 3
A kind of method of waste lithium cell recycling, using following steps：
(1) waste lithium cell is placed in nitrogen and disassembled, active positive electrode material is obtained, based on manganese dioxide；
(2) it is the positive electrode of collection is broken uniform, cleaned with washes of absolute alcohol 3 times, then with water to solution neutral bar
Stirred in part, cleaning process, quiescent setting minute, removes supernatant afterwards；
(3) by the positive electrode after cleaning, 24h is dried in vacuo at a temperature of 50 DEG C；
(4) under room temperature condition, material 2mg after drying is taken, is added in 100ml aniline solutions, the pH value of aniline solution is 6,
Concentration is 10ppm, adds 5mg ammonium persulfate-sodium bisulfate, produces SO4 -Oxidative degradation aniline.
Embodiment 4
A kind of method of waste lithium cell recycling, using following steps：
(1) waste lithium cell is placed in nitrogen and disassembled, active positive electrode material is obtained, based on manganese dioxide；
(2) it is the positive electrode of collection is broken uniform, cleaned with washes of absolute alcohol 4 times, then with water to solution neutral bar
Stirred in part, cleaning process, quiescent setting minute, removes supernatant afterwards；
(3) by the positive electrode after cleaning, 24h is dried in vacuo at a temperature of 60 DEG C；
(4) under room temperature condition, material 10mg after drying is taken, is added in 100ml aniline solutions, the pH value of aniline solution is 7,
Concentration is 20ppm, adds 5mg ammonium persulfate-sodium bisulfate, produces SO4 -Oxidative degradation aniline.
Embodiment 5
A kind of method of waste lithium cell recycling, using following steps：
(1) waste lithium cell is placed in inert gas and disassembled, obtain active positive electrode material, using manganese dioxide as
It is main；
(2) it is the positive electrode of collection is broken uniform, cleaned with washes of absolute alcohol 5 times, then with water to solution neutral bar
Stirred in part, cleaning process, quiescent setting minute, removes supernatant afterwards；
(3) by the positive electrode after cleaning, 12h is dried in vacuo at a temperature of 70 DEG C；
(4) under room temperature condition, material 10mg after drying is taken, is added in 100ml aniline solutions, the pH value of aniline solution is 8,
Concentration is 30ppm, adds 20mg ammonium persulfate-sodium bisulfate, produces SO4 -Oxidative degradation aniline.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (9)
1. a kind of method of waste lithium cell recycling, it is characterised in that this method uses following steps：
(1) waste lithium cell is placed in protection gas and disassembled, obtain active positive electrode material；
(2) active positive electrode material is collected, then is cleaned with deionized water and ethanol；
(3) the material dried recovered after cleaning is utilized；
(4) under room temperature condition, material after appropriate drying is taken, is added in aniline solution, added a certain amount of potassium hydrogen persulfate and answer
Salt is closed, SO is produced4 -Oxidative degradation aniline.
2. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that in step (1)
Described protection gas is nitrogen or inert gas.
3. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that in step (1)
Described active positive electrode material is based on manganese dioxide.
4. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that step (2) will
The positive electrode of collection is broken uniform, with washes of absolute alcohol 3~5 times, then is cleaned with water to solution neutral condition, cleaning process
Middle stirring, quiescent setting 2~10 minutes, remove supernatant afterwards.
5. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that step (3) will
Positive electrode after cleaning, is dried in vacuo 12~24h at a temperature of 50~70 DEG C.
6. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that in step (4)
The amount of the positive electrode of addition is 2~10mg/100ml aniline solutions.
7. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that in step (4)
The amount of the ammonium persulfate-sodium bisulfate of addition is 5~20mg/100ml aniline solutions.
8. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that in step (4)
The pH value of aniline solution is 6~8.
9. the method for a kind of waste lithium cell recycling according to claim 1, it is characterised in that in step (4)
The concentration of aniline solution is 10-30ppm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108147566A (en) * | 2017-12-22 | 2018-06-12 | 上海第二工业大学 | A kind of method using waste lithium ion cell anode material catalytic degradation organic wastewater |
| CN109244498A (en) * | 2018-09-19 | 2019-01-18 | 上海电力学院 | A kind of recycling and reusing method of waste and old lithium ion battery |
| CN113555615A (en) * | 2021-06-29 | 2021-10-26 | 昆明理工大学 | Method for preparing high-efficiency PMS activator from waste lithium ion battery and application |
| WO2021227213A1 (en) * | 2020-05-11 | 2021-11-18 | 湖南大学 | Catalyst for use in removing antibiotics in water body by activating peroxymonosulfate, preparation method therefor, and application thereof |
| CN114335781A (en) * | 2021-12-27 | 2022-04-12 | 上海电力大学 | Method for extracting precious metal from waste lithium battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109244498A (en) * | 2018-09-19 | 2019-01-18 | 上海电力学院 | A kind of recycling and reusing method of waste and old lithium ion battery |
| WO2021227213A1 (en) * | 2020-05-11 | 2021-11-18 | 湖南大学 | Catalyst for use in removing antibiotics in water body by activating peroxymonosulfate, preparation method therefor, and application thereof |
| CN113555615A (en) * | 2021-06-29 | 2021-10-26 | 昆明理工大学 | Method for preparing high-efficiency PMS activator from waste lithium ion battery and application |
| CN114335781A (en) * | 2021-12-27 | 2022-04-12 | 上海电力大学 | Method for extracting precious metal from waste lithium battery |
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| Publication number | Publication date |
|---|---|
| CN107180991B (en) | 2020-10-23 |
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