CN108977665A - A method of recycling waste and old lithium manganese phosphate - Google Patents
A method of recycling waste and old lithium manganese phosphate Download PDFInfo
- Publication number
- CN108977665A CN108977665A CN201810942891.0A CN201810942891A CN108977665A CN 108977665 A CN108977665 A CN 108977665A CN 201810942891 A CN201810942891 A CN 201810942891A CN 108977665 A CN108977665 A CN 108977665A
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- China
- Prior art keywords
- manganese
- waste
- phosphate
- old lithium
- lithium manganese
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
- C22B47/00—Obtaining manganese
-
- 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
-
- 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
-
- 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
Abstract
A method of recycling waste and old lithium manganese phosphate, comprising the following steps: Step 1: waste and old lithium manganese phosphate is uniformly mixed with calcium oxide, 0.5-3.0h is then heat-treated under the conditions of 300-600 DEG C；Step 2: step 1 product is placed in container, it is that the first slurries are made in 1:5-1:2 addition water according to solid-to-liquid ratio, then filters；Step 3: filter residue obtained by step 2 is placed in container, it is that the second slurries are made in 1:7-1:2 addition water according to solid-to-liquid ratio, continuously adds sulfuric acid or salt acid for adjusting pH value is 0.5-1.5；Step 4: the content of manganese in the slag of slurry is detected to reducing agent is added obtained by step 3 after adjusting pH value is 0.5-1.0, stopping plus reducing agent when manganese content is already below 0.5wt%；Step 5: by filtering obtained by step 4 up to solution and calcium phosphate filter residue containing manganese compound.Recovery method provided in the present invention is relatively simple, realizes waste and old resource recycling, it is therefore prevented that waste and old lithium manganese phosphate powder pollutes the environment.
Description
Technical field
The present invention relates to old and useless battery recycling fields, are related specifically to a kind of method for recycling waste and old lithium manganese phosphate.
Background technique
Lithium manganese phosphate, chemical formula: LiMnPO4 is a kind of natural minerals or artificial synthesized ternary electrode of lithium cell material
Material.The substance has the crystal structure of olivine shape, and physicochemical properties are stablized when leading to it as electrode material.Lithium manganese phosphate
The discharge platform of specific capacity and 4.1 V or so with 171 mAh/g, this but also lithium manganese phosphate become lithium of new generation from
The ideal material of sub- power battery.
It deepens continuously currently, being studied in terms of the expenses such as lithium manganese phosphate material synthesis, modified and chemical property, but
Have no that the report in terms of lithium manganese phosphate battery recycling, the lithium manganese phosphate in a large amount of waste and old lithium ion batteries cause environment
It greatly destroys, how to provide a kind of method for recycling waste and old lithium manganese phosphate becomes today's society urgent problem to be solved.
Summary of the invention
The technical problem to be solved in the present invention is that a kind of method for recycling waste and old lithium manganese phosphate is provided, it can by this method
Effectively waste and old lithium ion battery anode material manganese lithium phosphate to be recycled, so that waste and old resource recycling is realized,
The lithium manganese phosphate powder in waste lithium ion cell anode material is prevented to pollute the environment.
To solve the above-mentioned problems, using following technical scheme: a method of waste and old lithium manganese phosphate being recycled, including following
Step:
Step 1: waste and old lithium manganese phosphate is uniformly mixed in mass ratio for 1:1.5-1:1 with calcium oxide, then in 300-600 DEG C
Under the conditions of be heat-treated 0.5-3.0h；
Step 2: the product after step 1 is heat-treated is placed in container, it is that 1:5-1:2 addition water is made first according to solid-to-liquid ratio
Then lithium hydroxide solution, the filter residue containing manganese and calcium phosphate is obtained by filtration in slurries；
It is that water is added in 1:7-1:2 according to solid-to-liquid ratio Step 3: the filter residue containing manganese and calcium phosphate obtained by step 2 is placed in container
The second slurries are made, continuously adds sulfuric acid or salt acid for adjusting pH value is 0.5-1.5；
Step 4: the content of manganese in the slag of slurry is detected to reducing agent is added obtained by step 3 after adjusting pH value is 0.5-1.0,
Stop adding reducing agent when manganese content is already below 0.5wt%, continues if manganese content is higher than 0.5wt% plus reducing agent is until manganese
Content is lower than 0.5wt%；
Step 5: the manganese compound is chlorine by filtering obtained by step 4 to get solution and calcium phosphate filter residue containing manganese compound
Change manganese or manganese sulfate.
The waste and old lithium manganese phosphate is obtained by following methods: disassembling waste and old lithium manganese phosphate battery to obtain positive electrode, so
By crushing, sieve to obtain the final product.
Preferably, the mass ratio between waste and old lithium manganese phosphate and calcium oxide described in step 1 is 1:1.25.
Preferably, the solid-to-liquid ratio between product and water after being heat-treated in step 2 is 1:3.5.
Preferably, the solid-to-liquid ratio between the filter residue and water containing manganese and calcium phosphate in step 3 is 1:5.
Wherein, reducing agent described in step 4 is sodium sulfite or hydrogen peroxide.
The present invention can obtain manganese compound crystal, the manganese compound after obtaining the solution containing manganese compound by evaporative crystallization
Crystal is manganese chloride crystal or manganese sulfate crystal.
Compared to the prior art, the invention has the following advantages: waste and old lithium manganese phosphate can be recycled to obtain by the present invention
Lithium hydroxide solution and solution containing manganese compound, can be obtained manganese for the further condensing crystallizing of solution containing manganese compound
Object crystal, technique is relatively simple, realizes waste and old resource recycling, is recycled using this method to the waste and old lithium manganese phosphate of 1kg
The lithium of available 40g or more and the manganese of 220g or more, the rate of recovery is higher, effectively prevents waste and old lithium manganese phosphate powder to environment
It pollutes, can be widely used for the waste and old lithium ion battery that recycling positive electrode is lithium manganese phosphate.
Specific embodiment
Embodiment is given below so that the present invention to be specifically described, it is necessary to which indicated herein is following embodiment
It is used to further illustrate the present invention, should not be understood as limiting the scope of the invention, the ordinary skill in the field
Personnel still fall within protection scope of the present invention to some nonessential improvement of the invention made or adjustment according to this embodiment.
Embodiment 1
A method of recycling waste and old lithium manganese phosphate, comprising the following steps:
Step 1: waste and old lithium manganese phosphate 1kg is uniformly mixed with calcium oxide 1.2kg, then it is heat-treated under the conditions of 600 DEG C
0.5h；
Step 2: the product after step 1 is heat-treated is placed in container, 5L water is added, the first slurries are made, be then obtained by filtration
Lithium hydroxide solution 3.2L and filter residue containing manganese and calcium phosphate, test to obtain lithium hydroxide by flame atomic absorption spectrometry
The amount containing lithium of solution is 12.5g/L；
Step 3: being placed in container containing manganese and calcium phosphate is added 3L water and the second slurries is made, continuously add salt acid for adjusting pH
Value is 0.5；
Step 4: adjusting after pH value is 0.5-1.0 and being examined by flame atomic absorption spectrometry to hydrogen peroxide is added obtained by step 3
The content of the manganese in the slag (butt) of slurry is surveyed, testing result is 0.3 wt%, i.e., manganese content is stood already below 0.5wt% at this time
Stop that hydrogen peroxide is added；
Step 5: four gained slurry of filtration step, obtains manganese chloride solution 4.5L and calcium phosphate filter residue, passes through Flame Atomic Absorption Spectrometry light
The manganese content that spectrometry is tested to obtain manganese chloride solution is 50g/L, and manganese chloride crystal can be obtained in manganese chloride solution condensing crystallizing.
In step 4, if after finding that the pH value of solution is greater than 1.5, then hydrochloric acid is added during hydrogen peroxide is added
It drops to pH in the range of 0.5-1.5 again, then proceedes to that hydrogen peroxide is added.
By Step 2: it is found that the present embodiment passes through the recycling waste and old lithium manganese phosphate of 1kg after test result calculations in step 4
Available lithium 40g and manganese 225g.
Embodiment 2
A method of recycling waste and old lithium manganese phosphate, comprising the following steps:
Step 1: waste and old lithium manganese phosphate 1kg is uniformly mixed with calcium oxide 1kg, 3h then is heat-treated under the conditions of 300 DEG C；
Step 2: the product after step 1 is heat-treated is placed in container, 5L water is added, the first slurries are made, be then obtained by filtration
Lithium hydroxide solution 3.2L and filter residue containing manganese and calcium phosphate, test to obtain lithium hydroxide by flame atomic absorption spectrometry
The amount containing lithium of solution is 12.5g/L；
Step 3: being placed in container containing manganese and calcium phosphate is added 3L water and the second slurries is made, continuously add salt acid for adjusting pH
Value is 0.5；
Step 4: to hydrogen peroxide is added obtained by step 3, if pH value rises to 1.5 or more during hydrogen peroxide is added,
Sulfuric acid is added, adjusts the manganese in the slag (butt) for detecting slurry after pH value is 0.5-1.0 by flame atomic absorption spectrometry
Content, testing result 0.3wt%, i.e., manganese content already below 0.5wt% stops that hydrogen peroxide is added immediately at this time；
Step 5: four gained slurry of filtration step, obtains manganese sulfate solution 4.5L and calcium phosphate filter residue, passes through Flame Atomic Absorption Spectrometry light
The manganese content that spectrometry is tested to obtain manganese sulfate solution is 49g/L, and manganese chloride crystal can be obtained in manganese sulfate solution condensing crystallizing.
In step 4, if after finding that the pH value of solution is greater than 1.5, then hydrochloric acid is added during hydrogen peroxide is added
It drops to pH in the range of 0.5-1.5 again, then proceedes to that hydrogen peroxide is added.
By Step 2: it is found that the present embodiment passes through the recycling waste and old lithium manganese phosphate of 1kg after test result calculations in step 4
Available lithium 40g and manganese 221g.
Embodiment 3
A method of recycling waste and old lithium manganese phosphate, comprising the following steps:
Step 1: waste and old lithium manganese phosphate 1kg is uniformly mixed with calcium oxide 1.5kg, 2h then is heat-treated under the conditions of 450 DEG C；
Step 2: the product after step 1 is heat-treated is placed in container, 5L water is added, the first slurries are made, be then obtained by filtration
Lithium hydroxide solution 3.2L and filter residue containing manganese and calcium phosphate, test to obtain lithium hydroxide by flame atomic absorption spectrometry
The amount containing lithium of solution is 12.5g/L；
Step 3: being placed in container containing manganese and calcium phosphate is added 3L water and the second slurries is made, continuously add salt acid for adjusting pH
Value is 0.5；
Step 4: to hydrogen peroxide is added obtained by step 3, if pH value rises to 1.5 or more during hydrogen peroxide is added,
Hydrochloric acid is added, adjusts the manganese in the slag (butt) for detecting slurry after pH value is 0.5-1.0 by flame atomic absorption spectrometry
Content, testing result are 0.3 wt%, stop that hydrogen peroxide is added immediately；
Step 5: four gained slurry of filtration step, obtains manganese chloride solution 4.5L and calcium phosphate filter residue, passes through Flame Atomic Absorption Spectrometry light
The manganese content that spectrometry is tested to obtain manganese chloride solution is 49g/L, and manganese chloride crystal can be obtained in manganese chloride solution condensing crystallizing.
In step 4, if after finding that the pH value of solution is greater than 1.5, then hydrochloric acid is added during hydrogen peroxide is added
It drops to pH in the range of 0.5-1.5 again, then proceedes to that hydrogen peroxide is added.
By Step 2: it is found that the present embodiment passes through the recycling waste and old lithium manganese phosphate of 1kg after test result calculations in step 4
Available lithium 40g and manganese 221g.
Claims (6)
1. a kind of method for recycling waste and old lithium manganese phosphate, which comprises the following steps:
Step 1: waste and old lithium manganese phosphate is uniformly mixed in mass ratio for 1:1.5-1:1 with calcium oxide, then in 300-600 DEG C
Under the conditions of be heat-treated 0.5-3.0h；
Step 2: the product after step 1 is heat-treated is placed in container, it is that 1:5-1:2 addition water is made first according to solid-to-liquid ratio
Then lithium hydroxide solution, the filter residue containing manganese and calcium phosphate is obtained by filtration in slurries；
It is that water is added in 1:7-1:2 according to solid-to-liquid ratio Step 3: the filter residue containing manganese and calcium phosphate obtained by step 2 is placed in container
The second slurries are made, continuously adds sulfuric acid or salt acid for adjusting pH value is 0.5-1.5；
Step 4: the content of manganese in the slag of slurry is detected to reducing agent is added obtained by step 3 after adjusting pH value is 0.5-1.0,
Stop adding reducing agent when manganese content is already below 0.5wt%, continues if manganese content is higher than 0.5wt% plus reducing agent is until manganese
Content is lower than 0.5wt%；
Step 5: the manganese compound is chlorine by filtering obtained by step 4 to get solution and calcium phosphate filter residue containing manganese compound
Change manganese or manganese sulfate.
2. the method for the waste and old lithium manganese phosphate of recycling according to claim 1, which is characterized in that the waste and old lithium manganese phosphate by
Following methods obtain: disassembling waste and old lithium manganese phosphate battery to obtain positive electrode, then crushed, sieved to obtain the final product.
3. the method for the waste and old lithium manganese phosphate of recycling according to claim 1, which is characterized in that waste and old phosphorus described in step 1
Mass ratio between sour manganese lithium and calcium oxide is 1:1.25.
4. the method for the waste and old lithium manganese phosphate of recycling according to claim 1, which is characterized in that after being heat-treated in step 2
Solid-to-liquid ratio between product and water is 1:3.5.
5. the method for the waste and old lithium manganese phosphate of recycling according to claim 1, which is characterized in that contain manganese and phosphoric acid in step 3
Solid-to-liquid ratio between the filter residue and water of calcium is 1:5.
6. the method for the waste and old lithium manganese phosphate of recycling according to claim 1, which is characterized in that reducing agent described in step 4 is
Sodium sulfite or hydrogen peroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201810942891.0A CN108977665A (en) | 2018-08-17 | 2018-08-17 | A method of recycling waste and old lithium manganese phosphate |
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| CN201810942891.0A CN108977665A (en) | 2018-08-17 | 2018-08-17 | A method of recycling waste and old lithium manganese phosphate |
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