CN110527837A - A kind of efficient leaching method of cell positive material - Google Patents
A kind of efficient leaching method of cell positive material Download PDFInfo
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- CN110527837A CN110527837A CN201910892860.3A CN201910892860A CN110527837A CN 110527837 A CN110527837 A CN 110527837A CN 201910892860 A CN201910892860 A CN 201910892860A CN 110527837 A CN110527837 A CN 110527837A
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- cell positive
- positive material
- filter residue
- sulfuric acid
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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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
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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
- C22B47/00—Obtaining manganese
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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
- 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
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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
- 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 Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of efficient leaching methods of cell positive material, belong to old and useless battery recycling field, solve the problem that existing method leaching rate is lower, and sulfuric acid utilization rate is low and neutralization reagent dosage is big.The technical scheme is that cell positive material is uniformly mixed with the ratio of liquid-solid ratio 5.5-7.5mL:1g with water, mixed liquor is obtained, the concentrated sulfuric acid is added, it is warming up to 80-95 DEG C, insulation reaction, dripping hydrogen peroxide to fully reacting are separated by filtration to obtain a filter residue and first-time filtrate；First-time filtrate is mixed with cell positive material, is warming up to 80-95 DEG C, insulation reaction 1-2h, is separated by filtration to obtain unreacted completely secondary filter residue and secondary filtrate；Secondary filter residue return step one is continued to leach.The present invention improves leaching rate by two step solid-liquid circulating leachings；The acid concentration for reducing liquid after leaching, improves the utilization rate of sulfuric acid；The dosage for reducing alkaline reagent needed for neutralization reaction, reduces costs.
Description
Technical field
The invention belongs to old and useless battery recycling fields, and in particular to a kind of efficient leaching method of cell positive material.
Background technique
Leaching in relation to cell positive material, the prior art use one step leaching method of dioxysulfate aqueous systems, leaching rate
Reach 98%, need to be further increased, and its dioxygen water consumption is big, liquid acid concentration is higher thereafter, causes to be used in subsequent technique
The alkaline reagent dosage of neutralization reaction is big, higher cost.Also useful sulfuric acid or citric acid are mixed with hydrogen peroxide is soaked through ultrasound
Out, there is also the same problems, while more demanding to ultrasonic device and production environment.In addition, also useful microwave soaks to improve
The method of effect out, but effect is still undesirable, and liquid acid concentration is higher after gained leaching, and sulfuric acid utilization rate is lower, subsequent reactions
Dosis neutralisata is big, causes unnecessary reagent waste.
Summary of the invention
The object of the present invention is to provide a kind of efficient leaching methods of cell positive material, to solve existing method leaching rate
Problem lower, that sulfuric acid utilization rate is low and neutralization reagent dosage is big.
The technical scheme is that a kind of efficient leaching method of cell positive material, comprising the following steps:
Step 1: being first uniformly mixed cell positive material with water with the ratio of liquid-solid ratio 5.5-7.5mL:1g, mixed liquor is obtained,
The concentrated sulfuric acid is added, is warming up to 80-95 DEG C, insulation reaction, dripping hydrogen peroxide to fully reacting is separated by filtration to obtain a filter residue
And first-time filtrate；
Step 2: first-time filtrate obtained by step 1 is mixed with cell positive material, it is warming up to 80-95 DEG C, insulation reaction 1-2h,
It is separated by filtration to obtain unreacted completely secondary filter residue and secondary filtrate；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
As a further improvement of the present invention, in step 1, the volume fraction of sulfuric acid is 98%, and sulphuric acid is
0.4-0.7 times that volume is cell positive material quality is added in 250-350g/L mixed liquor, hydrogen peroxide.
As a further improvement of the present invention, in step 2, cell positive material additional amount is remaining in first-time filtrate
1.6-2 times of sour quality.
As a further improvement of the present invention, it is characterised in that: the cell positive material includes nickle cobalt lithium manganate, cobalt acid
Lithium or LiMn2O4.
Compared with prior art, the invention has the following advantages that
Leached 1. traditional step leaching is improved to two steps by the present invention, by first-time filtrate obtained by step 1 be used for step 2 after
Continuous reaction, a filter residue are final remaining carbon slag, and secondary filter residue return step one obtained by step 2 is continued to participate in leaching, two
Secondary filtrate is that the leachate of final gained element improves leaching rate in this, as two step solid-liquid circulating leachings；
2. the present invention is leached by two steps, reduce the dosage of hydrogen peroxide in Leach reaction；The acid for reducing liquid after leaching is dense
Degree, improves the utilization rate of sulfuric acid；The dosage of alkaline reagent needed for reducing subsequent neutralization reaction, reduces costs；
3. operation of the present invention is simple, solve existing problems.
Specific embodiment
The following examples can further illustrate the present invention, but the invention is not limited in any way.
Embodiment 1, nickle cobalt lithium manganate anode material efficient leaching method steps are as follows:
Step 1: being first uniformly mixed nickle cobalt lithium manganate cell positive material with water with the ratio of liquid-solid ratio 5.5ml:1g, obtain
Mixed liquor adds the concentrated sulfuric acid (volume fraction 98%), and additional amount is 350g/L mixed liquor, is warming up to 95 DEG C, insulation reaction, then
Hydrogen peroxide is added dropwise to fully reacting, 0.7 times (ml:g) that volume is positive quality of materials is added in hydrogen peroxide, is separated by filtration once
Filter residue and first-time filtrate, through detecting, first-time filtrate acid concentration is 120g/L, and remaining slag rate is 4%, total metal content 5%；
Step 2: first-time filtrate obtained by step 1 is mixed with nickle cobalt lithium manganate cell positive material, nickle cobalt lithium manganate battery is just
Pole material additional amount is 2 times of residual sulfuric acid quality in first-time filtrate, is warming up to 95 DEG C, insulation reaction 2h is separated by filtration not
The secondary filter residue of fully reacting and secondary filtrate, detect after reaction, and secondary filtrate acid concentration is 0g/L；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
In the present embodiment, metal leaching rate 99.2%.Acid concentration reaches in final gained sulfate liquor (secondary filtrate)
0g/L, sulfuric acid utilization rate reach 100%, save the dosage of hydrogen peroxide 13%, and the acid amount neutralized is needed to reduce 120g/ in subsequent technique
L saves lye dosage.
Embodiment 2, nickle cobalt lithium manganate anode material efficient leaching method steps are as follows:
Step 1: being first uniformly mixed nickle cobalt lithium manganate cell positive material with water with the ratio of liquid-solid ratio 7.5ml:1g, obtain
Mixed liquor adds the concentrated sulfuric acid (volume fraction 98%), and additional amount is 250g/L mixed liquor, is warming up to 80 DEG C, insulation reaction, then
Hydrogen peroxide is added dropwise to fully reacting, 0.4 times (ml:g) that volume is positive quality of materials is added in hydrogen peroxide, is separated by filtration once
Filter residue and first-time filtrate, through detecting, first-time filtrate acid concentration is 60g/L；
Step 2: first-time filtrate obtained by step 1 is mixed with nickle cobalt lithium manganate cell positive material, nickle cobalt lithium manganate battery is just
Pole material additional amount is 1.6 times of residual sulfuric acid quality in first-time filtrate, is warming up to 80 DEG C, insulation reaction 1h is separated by filtration
Unreacted completely secondary filter residue and secondary filtrate, detect after reaction, and secondary filtrate acid concentration is 5g/L；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
In the present embodiment, metal leaching rate 98%.Hydrogen peroxide additional amount is less, saves 50% dosage, metal leaching
Extracting rate also decreases, and acid concentration reaches 5g/L in final gained sulfate liquor (secondary filtrate), and sulfuric acid utilization rate reaches
98%, it needs in subsequent technique the acid amount neutralized to reduce 55g/L, reduces the dosage of lye.
Embodiment 3, nickle cobalt lithium manganate anode material efficient leaching method steps are as follows:
Step 1: being first uniformly mixed nickle cobalt lithium manganate cell positive material with water with the ratio of liquid-solid ratio 6ml:1g, mixed
Liquid to be closed, is added the concentrated sulfuric acid (volume fraction 98%), additional amount is 300g/L mixed liquor, it is warming up to 90 DEG C, insulation reaction, then drip
Add hydrogen peroxide to fully reacting, 0.5 times (ml:g) that volume is positive quality of materials is added in hydrogen peroxide, is separated by filtration once to filter
Slag and first-time filtrate, through detecting, first-time filtrate acid concentration is 80g/L；
Step 2: first-time filtrate obtained by step 1 is mixed with nickle cobalt lithium manganate cell positive material, nickle cobalt lithium manganate battery is just
Pole material additional amount is 1.8 times of residual sulfuric acid quality in first-time filtrate, is warming up to 90 DEG C, insulation reaction 1.5h is separated by filtration
Unreacted completely secondary filter residue and secondary filtrate are obtained, is detected after reaction, secondary filtrate acid concentration is 2g/L；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
In the present embodiment, metal leaching rate 99%.Hydrogen peroxide 37% is saved, first-time filtrate acid concentration is 80g/L, in
Reach 2g/L with, secondary filtrate acid concentration, sulfuric acid utilization rate reaches 99.3%, and reduces neutralizing acid amount 78g/L.
It can be seen that by embodiment 1-3, for nickle cobalt lithium manganate, carried out according to the material ratio of embodiment 1 and reaction time
Reaction, best leaching effect can be reached, after reaction, without extra acid in secondary filtrate, sulfuric acid obtain all of；Embodiment
3 leaching effect is preferable, after reaction, the complete sulfuric acid of remaining traces of unreacted in secondary filtrate.
Embodiment 4, cobalt acid lithium battery positive electrode efficient leaching method steps are as follows:
Step 1: being first uniformly mixed cobalt acid lithium battery positive electrode with water with the ratio of liquid-solid ratio 7.5mL:1g, mixed
Liquid adds the concentrated sulfuric acid (volume fraction 98%), and additional amount is 300g/L mixed liquor, is warming up to 95 DEG C, insulation reaction, then is added dropwise
For hydrogen peroxide to fully reacting, 0.6 times (mL:g) that volume is positive quality of materials is added in hydrogen peroxide, is separated by filtration to obtain a filter residue
And first-time filtrate, through detecting, first-time filtrate acid concentration is 100g/L；
Step 2: first-time filtrate obtained by step 1 is mixed with cobalt acid lithium battery positive electrode, cobalt acid lithium battery positive electrode adds
Entering amount is to be warming up to 90 DEG C, insulation reaction 2h 1.8 times of residual sulfuric acid quality in first-time filtrate, be separated by filtration unreacted is complete
Complete secondary filter residue and secondary filtrate, detect after reaction, and secondary filtrate acid concentration is 3g/L；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
In the present embodiment, cobalt acid lithium leaching effect is good, can be leached completely with this reagent additional proportion, leaching rate reaches
99.5%.Hydrogen peroxide saves dosage 14%, and acid concentration is 3g/L in the final secondary filtrate of gained, and sulfuric acid utilization rate reaches 99%.
Embodiment 5, lithium manganate cell positive electrode material efficient leaching method steps are as follows:
Step 1: being first uniformly mixed lithium manganate cell positive electrode material with water with the ratio of liquid-solid ratio 7.5mL:1g, mixed
Liquid adds the concentrated sulfuric acid (volume fraction 98%), and additional amount is 350g/L mixed liquor, is warming up to 95 DEG C, insulation reaction, then is added dropwise
For hydrogen peroxide to fully reacting, 0.7 times (mL:g) that volume is positive quality of materials is added in hydrogen peroxide, is separated by filtration to obtain a filter residue
And first-time filtrate, through detecting, first-time filtrate acid concentration is 120g/L；
Step 2: first-time filtrate obtained by step 1 is mixed with lithium manganate cell positive electrode material, lithium manganate cell positive electrode material adds
Entering amount is to be warming up to 95 DEG C, insulation reaction 2h 2 times of residual sulfuric acid quality in first-time filtrate, be separated by filtration unreacted is complete
Secondary filter residue and secondary filtrate, detected after reaction, secondary filtrate acid concentration be 5g/L；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
LiMn2O4 needs high temperature high acidic oils compared to the more difficult leaching of other positive electrodes, and dioxygen water consumption is slightly more, is thrown with this
Material ratio is leached, and metal leaching rate reaches 98%.Acid concentration is 5g/ in final gained sulfate liquor (secondary filtrate)
L, sulfuric acid utilization rate are 98.5%.
To sum up, the method for the present invention leaches the metallic element in positive electrode, and dioxygen water consumption is few, the final secondary filter of gained
Acid concentration is extremely low in liquid, and sulfuric acid utilization rate is 98% or more, and the lye of 60-120g/L acid need to be neutralized by saving post-processing, and metal soaks
Extracting rate at least can reach 98%, and carrying out reaction with optimal conditions can reach 99% or more.The present invention is leached by two steps, reaches efficient
The purpose for leaching and efficiently utilizing.
Claims (4)
1. a kind of efficient leaching method of cell positive material, it is characterised in that the following steps are included:
Step 1: being first uniformly mixed cell positive material with water with the ratio of liquid-solid ratio 5.5-7.5mL:1g, mixed liquor is obtained,
The concentrated sulfuric acid is added, is warming up to 80-95 DEG C, insulation reaction, dripping hydrogen peroxide to fully reacting is separated by filtration to obtain a filter residue
And first-time filtrate；
Step 2: first-time filtrate obtained by step 1 is mixed with cell positive material, it is warming up to 80-95 DEG C, insulation reaction 1-2h,
It is separated by filtration to obtain unreacted completely secondary filter residue and secondary filtrate；
Step 3: secondary filter residue return step one obtained by step 2 is continued to leach.
2. a kind of efficient leaching method of cell positive material according to claim 1, it is characterised in that: in step 1
In, the volume fraction of sulfuric acid is 98%, and sulphuric acid is 250-350g/L mixed liquor, and it is anode that volume, which is added, in hydrogen peroxide
0.4-0.7 times of quality of materials.
3. a kind of efficient leaching method of cell positive material according to claim 2, it is characterised in that: in step 2
In, cell positive material additional amount is 1.6-2 times of residual acid quality in first-time filtrate.
4. a kind of efficient leaching method of cell positive material according to any one of claim 1-3, it is characterised in that:
The cell positive material includes nickle cobalt lithium manganate, cobalt acid lithium or LiMn2O4.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111549229A (en) * | 2020-05-11 | 2020-08-18 | 赣州有色冶金研究所 | Method for extracting lithium from positive electrode material of waste lithium ion battery through pre-reduction preferential dissolution |
| CN113913606A (en) * | 2021-12-10 | 2022-01-11 | 矿冶科技集团有限公司 | Two-stage countercurrent leaching method for anode material of waste power battery |
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| CN113913606A (en) * | 2021-12-10 | 2022-01-11 | 矿冶科技集团有限公司 | Two-stage countercurrent leaching method for anode material of waste power battery |
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