CN107986335A - A kind of method that manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode - Google Patents
A kind of method that manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode Download PDFInfo
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- CN107986335A CN107986335A CN201711339851.9A CN201711339851A CN107986335A CN 107986335 A CN107986335 A CN 107986335A CN 201711339851 A CN201711339851 A CN 201711339851A CN 107986335 A CN107986335 A CN 107986335A
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- positive electrode
- manganese dioxide
- lithium battery
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- General Chemical & Material Sciences (AREA)
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Abstract
The present invention provides a kind of method for preparing manganese dioxide particle using waste and old ternary dynamic lithium battery positive electrode, include the following steps；(1) positive electrode is heat-treated；Complete electric discharge dismounting and broken waste and old ternary dynamic lithium battery positive electrode are put into Muffle furnace and are heated to 400 DEG C~700 DEG C, 30min~60min is kept, for removing PVDF and acetylene black；(2) coordinated using dilute sulfuric acid, hydrogen peroxide and be cleaned by ultrasonic positive electrode；Positive electrode after heat treatment in step (1) is used into 0.5~1.5mol.L‑1Dilute sulfuric acid, 10%~30% hydrogen peroxide, coordinate be cleaned by ultrasonic 5~20 minutes；Positive electrode after ultrasonic cleaning is used into 0.5~1.5mol.L‑1Dilute sulfuric acid cleaning aluminium foil and recycle；(3) preparation of manganese dioxide particle by two parts liquid in step (2) collect one be in 75 DEG C~95 DEG C under the conditions of react 50~60min；The potassium peroxydisulfate solid stirring 80~120min of reaction added, filtration washing, prepares α type manganese dioxide particles and leaches nickel cobalt elemental lithium completely.The present invention can realize the preparation of α type manganese dioxide particles and effectively leach nickel cobalt elemental lithium.
Description
Technical field
It is more particularly to a kind of to use waste and old ternary power lithium battery the present invention relates to a kind of method for preparing manganese dioxide particle
The method that pond positive electrode prepares manganese dioxide particle.
Background technology
With economic development and the requirement of environmental protection, promote the consumption structure of the energy to change, reduce disappearing for fossil fuel
Take, increase the consumption proportion of clean energy resource；The implementation of national policy also promotes the generation of this transformation, such as：National " 863 " meter
Delineating has electric automobile special, promotes the development of electric automobile, reduces the consumption of the fossil fuel of petroleum-type；Also promote at the same time
The rapid development of power battery industry；Vehicular dynamic battery species have cobalt acid lithium battery, ternary lithium battery, lithium manganate battery with
And ferric phosphate lithium cell etc., and ferric phosphate lithium cell and ternary lithium battery occupy consumption market mainstream at present；Ternary lithium battery by
It is big, small and be subject to market to favor in its capacity, it is mostly used for small passenger car；Ferric phosphate lithium cell is reviewed, due to it just
The heat endurance of pole material is better than ternary anode material of lithium battery, so the battery that Large Electric car uses at present is ferric phosphate
Lithium battery；At present, the new energy that Beijing new-energy automobile, Jianghuai Automobile, Jiangling automobile, Chery Automobiles, many safe automobiles etc. have listed
In the passenger car of source, most vehicles have started to use ternary lithium battery；Understood according to automobile industry latest data statistics：Three
First lithium battery is used for passenger car and the ratio of pure electric vehicle special-purpose vehicle is incrementally increasing, it was demonstrated that has more waste and old ternary power in the future
Lithium battery needs to recycle.
The preparation of manganese dioxide is mainly derived from natural minerals pyrolusite at the same time, generally using high-temperature sulfuric acid manganese solution electrolysis
Produce, manganese carbonate ore and pyrolusite can be used as raw material；The preparation of manganese sulfate solution include leaching, iron removaling, neutralization, except with much money
Belong to, filtering, stand the process such as removing calcium and magnesium, be made crude product after high-temperature electrolysis, it is treated include peeling off, crush, wash, in
It is made qualified brilliant with processes such as dryings；Also manganese carbonate, manganese nitrate pyrolysismethod, by low price manganese oxide and oxidant such as chloric acid
Composite reaction direct oxidation is made respectively for sodium, chlorine, oxygen etc..
The content of the invention
The technical problem to be solved in the present invention is to provide it is a kind of effective, simple, quickly use waste and old ternary power
The method that anode material of lithium battery prepares α type manganese dioxide particles, the present invention, which can greatly reduce, prepares manganese dioxide particle
Cost, while realize the recycling of waste and old ternary dynamic lithium battery positive electrode.
To reach above-mentioned purpose, technical scheme is as follows：
A kind of method that manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode, the described method includes
Following steps；
(1) positive electrode is heat-treated
Complete electric discharge dismounting and broken waste and old ternary dynamic lithium battery positive electrode are put into Muffle furnace and are heated to 400 DEG C
~700 DEG C, 30min~60min is kept, for removing PVDF and acetylene black；
(2) coordinated using dilute sulfuric acid, hydrogen peroxide and be cleaned by ultrasonic positive electrode；
By positive electrode after heat treatment in step (1) using 0.5~1.5mol.L-1 dilute sulfuric acid, 10%~30%
Hydrogen peroxide, which coordinates, to be cleaned by ultrasonic 5~20 minutes；Positive electrode after ultrasonic cleaning is used to the dilute sulfuric acid of 0.5~1.5mol.L-1
Cleaning aluminium foil simultaneously recycles；
(3) preparation of manganese dioxide particle
Two parts liquid in step (2) is collected one 50~60min is reacted under the conditions of 75 DEG C~95 DEG C；Add
Potassium peroxydisulfate solid stirring reaction 80~120min, filtration washing, prepares α type manganese dioxide particles, while realizes nickel cobalt
Effective leaching of elemental lithium.
In one embodiment of the invention, sulfuric acid dosage and positive electrode quality when being cleaned by ultrasonic in step (2)
Ratio be 5：1~15：1(L/kg).
In one embodiment of the invention, the dioxygen water consumption in step (2) and the ratio of positive electrode quality are 0.5：1
~1：1(L/kg).
In one embodiment of the invention, dilute sulfuric acid dosage and positive electrode matter after being cleaned by ultrasonic in step (2)
The ratio of amount is 10：1~5：1(L/kg).
In one embodiment of the invention, the dosage of potassium peroxydisulfate and the ratio of positive electrode quality are in step (3)
1.5：1~10：1(L/kg).
In one embodiment of the invention, mixing speed is 600r/min~1500r/min in step (3).
In the present invention, waste and old ternary dynamic lithium battery positive electrode prepare α type manganese dioxide particle mainly by manganese ion with
Over cure acid ion is acted on being completed under the conditions of sulfuric acid in nickel cobalt ionic catalysis；According to manganese ion and over cure acid ion and Gao Meng
Acid group decomposition reaction equation：
2MnSO4+5K2S2O8+8H2O=2KMnO4+4K2SO4+8H2SO4
4KMnO4+2H2SO4=3O2↑+2H2O+4MnO2↓+2K2SO4
2KMnO4+3MnSO4+2H2O=5MnO2↓+2H2SO4+K2SO4
Understand that waste and old ternary lithium dynamical battery positive electrode produces manganese ion, manganese ion warp after acidleach by above equation
Cross and α type manganese dioxide particles generated after series reaction, manganese ion is reacted with over cure acid ion in the present invention, during produce
Acid can continue to leach waste and old ternary dynamic lithium battery positive electrode, while cause more manganese elements in positive electrode
Into in solution, raw material is provided for manganese ion and the reaction of over cure acid ion, can also realize the leaching of lithium cobalt nickel element.
The present invention has the following advantages：
(1) present invention is suitable for the various waste and old ternary dynamic lithium battery positive electrode recycling leachings containing manganese nickel cobalt, just
When pole material leaches, α type manganese dioxide particles can be not only prepared, but also can realize the leaching of other metals resources.
(2) dilute sulfuric acid of the present invention, hydrogen peroxide, potassium peroxydisulfate, can effectively realize α type dioxies under the conditions of 75 DEG C~95 DEG C
Change the preparation of manganese particle and the leaching of other metals, there is preferable economic benefit.
(3) reaction time of the invention can be controlled in 3 it is small when it is interior, avoid shadow of the reaction time consumption to leachate subsequent operation
Ring.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the flow diagram that the present invention reacts；
Fig. 2 is the XRD diagram of manganese dioxide under the conditions of different rotating speeds；
α type manganese dioxide particles SEM schemes under the conditions of Fig. 3 is 900r/min；
Fig. 4 is the laser particle size measurement result figure of α type manganese dioxide particles under 900rad/min speed conditions.
Embodiment
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, tie below
Conjunction is specifically illustrating, and the present invention is further explained.
As shown in Fig. 1 first steps：Using Muffle furnace by complete electric discharge is disassembled and is crushed waste and old ternary dynamic lithium battery
Positive electrode be heat-treated at 530 DEG C 1 it is small when；Second step is by the cathode material for the waste and old ternary dynamic lithium battery for completing heat treatment
Material uses dilute sulfuric acid (dilute sulfuric acid dosage：Positive electrode dosage=10:1mL/g), hydrogen peroxide (dioxygen water consumption:Positive electrode dosage
=1：1mL/g) coordinate and be cleaned by ultrasonic positive electrode 10 minutes；3rd step is to use dilute sulfuric acid (dilute sulfuric acid dosage：Positive electrode is used
Amount=10:1mL/g) wash aluminium foil；4th step is that two parts cleaning solution is heated to 90 DEG C of reaction 50min；5th step is to add
Potassium peroxydisulfate solid (positive electrode dosage：Potassium peroxydisulfate dosage=1:8g/g) and with certain speed stirring reaction to 120min；
α type manganese dioxide particles are made in last filtration washing drying, while realize effective leaching of other metals in positive electrode.
Embodiment 1
Positive electrode is 3.1564g in embodiment, and rotating speed uses 900r/min.
Using Muffle furnace by the positive electrode of complete electric discharge is disassembled and is crushed waste and old ternary dynamic lithium battery at 530 DEG C
Be heat-treated 1 it is small when, then will complete heat treatment waste and old ternary dynamic lithium battery positive electrode 31.6mL1molL-1's
Dilute sulfuric acid, the hydrogen peroxide of 3.2mL30%, which coordinates, is cleaned by ultrasonic positive electrode 10 minutes, afterwards using 31.6mL1molL-1It is dilute
Sulfuric acid scrubbing aluminium foil；Two parts cleaning solution is heated to 90 DEG C of reaction 50min at the same time, the potassium peroxydisulfate for adding 25.2513g is consolidated
Body 900r/min stirrings are reacted to 120min；Yield is after measured：99.42%, grain diameter：Laser particle analyzer test result D
(3,2) and D (4,3) and d (0.5) are respectively 12.277 μm, 20.158 μm and 17.742 μm (see Fig. 4).As shown in Figure 2
Product is α type manganese dioxide；α type manganese dioxide particles SEM schemes under the conditions of Fig. 3 is 900r/min.
Embodiment 2
Positive electrode is 2.9723g in embodiment, and rotating speed uses 1200r/min.
Using Muffle furnace by the positive electrode of complete electric discharge is disassembled and is crushed waste and old ternary dynamic lithium battery at 530 DEG C
Be heat-treated 1 it is small when, then will complete heat treatment waste and old ternary dynamic lithium battery positive electrode 29.7mL1molL-1's
Dilute sulfuric acid, the hydrogen peroxide of 3.0mL30%, which coordinates, is cleaned by ultrasonic positive electrode 10 minutes, afterwards using 29.7mL1molL-1It is dilute
Sulfuric acid scrubbing aluminium foil；Two parts cleaning solution is heated to 90 DEG C of reaction 50min at the same time, the potassium peroxydisulfate for adding 23.7784g is consolidated
Body 1200r/min stirrings are reacted to 120min；Yield is after measured：99.47%, grain diameter：Laser particle analyzer test result D
(3,2) and D (4,3) and d (0.5) are respectively 15.502 μm, 26.568 μm and 24.915 μm.Product is α as shown in Figure 2
Type manganese dioxide.
Embodiment 3
Positive electrode is 3.0561g in embodiment, and rotating speed uses 1500r/min.
Using Muffle furnace by the positive electrode of complete electric discharge is disassembled and is crushed waste and old ternary dynamic lithium battery at 530 DEG C
Be heat-treated 1 it is small when, then will complete heat treatment waste and old ternary dynamic lithium battery positive electrode 30.6mL1molL-1's
Dilute sulfuric acid, the hydrogen peroxide of 3.1mL30%, which coordinates, is cleaned by ultrasonic positive electrode 10 minutes, afterwards using 30.6mL1molL-1It is dilute
Sulfuric acid scrubbing aluminium foil；Two parts cleaning solution is heated to 90 DEG C of reaction 50min at the same time, the potassium peroxydisulfate for adding 24.4488g is consolidated
Body 1500r/min stirrings are reacted to 120min；Yield is after measured：99.53%, grain diameter：Laser particle analyzer test result D
(3,2) and D (4,3) and d (0.5) are respectively 18.629 μm, 27.819 μm and 26.506 μm.Product is α as shown in Figure 2
Type manganese dioxide.
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
- A kind of 1. method that manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode, it is characterised in that institute The method of stating includes the following steps；(1) positive electrode is heat-treatedWill completely electric discharge dismounting and broken waste and old ternary dynamic lithium battery positive electrode be put into Muffle furnace be heated to 400 DEG C~ 700 DEG C, 30min~60min is kept, for removing PVDF and acetylene black；(2) coordinated using dilute sulfuric acid, hydrogen peroxide and be cleaned by ultrasonic positive electrode；Positive electrode after heat treatment in step (1) is used into 0.5~1.5mol.L-1Dilute sulfuric acid, 10%~30% dioxygen Water, which coordinates, to be cleaned by ultrasonic 5~20 minutes；Positive electrode after ultrasonic cleaning is used into 0.5~1.5mol.L-1Dilute sulfuric acid cleaning Aluminium foil simultaneously recycles；(3) preparation of manganese dioxide particleTwo parts liquid in step (2) is collected one 50~60min is reacted under the conditions of 75 DEG C~95 DEG C；Add over cure Sour potassium solid stirring 80~120min of reaction, filtration washing, prepares α type manganese dioxide particles, while realizes nickel cobalt elemental lithium Effective leaching.
- A kind of manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode 2. according to claim 1 Method, it is characterised in that the ratio of sulfuric acid dosage and positive electrode quality when being cleaned by ultrasonic in step (2) is 5：1~15：1 (L/kg)。
- A kind of manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode 3. according to claim 1 Method, it is characterised in that the ratio of dioxygen water consumption and positive electrode quality in step (2) is 0.5：1~1：1(L/kg).
- A kind of manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode 4. according to claim 1 Method, it is characterised in that the ratio of dilute sulfuric acid dosage and positive electrode quality after being cleaned by ultrasonic in step (2) is 10：1~5： 1(L/kg)。
- A kind of manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode 5. according to claim 1 Method, it is characterised in that the ratio of the dosage of potassium peroxydisulfate and positive electrode quality is 1.5 in step (3)：1~10：1(L/kg).
- A kind of manganese dioxide particle is prepared using waste and old ternary dynamic lithium battery positive electrode 6. according to claim 1 Method, it is characterised in that mixing speed is 600r/min~1500r/min in step (3).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108832216A (en) * | 2018-06-14 | 2018-11-16 | 合肥工业大学 | A kind of pre-treating method of waste power lithium battery recycling |
| CN109473748A (en) * | 2018-10-24 | 2019-03-15 | 北京工业大学 | A kind of stripping means of waste and old ternary dynamic lithium battery positive electrode and collector |
| CN110563046A (en) * | 2019-09-10 | 2019-12-13 | 广州大学 | method for recycling waste lithium ion battery anode material |
| CN113584309A (en) * | 2021-07-05 | 2021-11-02 | 广东佳纳能源科技有限公司 | Method for separating manganese in ternary lithium ion battery anode leachate |
| CN116168958A (en) * | 2023-01-09 | 2023-05-26 | 中国地质大学（武汉） | Preparation method of miniature super capacitor |
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| CN109473748A (en) * | 2018-10-24 | 2019-03-15 | 北京工业大学 | A kind of stripping means of waste and old ternary dynamic lithium battery positive electrode and collector |
| CN110563046A (en) * | 2019-09-10 | 2019-12-13 | 广州大学 | method for recycling waste lithium ion battery anode material |
| CN113584309A (en) * | 2021-07-05 | 2021-11-02 | 广东佳纳能源科技有限公司 | Method for separating manganese in ternary lithium ion battery anode leachate |
| CN116168958A (en) * | 2023-01-09 | 2023-05-26 | 中国地质大学（武汉） | Preparation method of miniature super capacitor |
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