CN114388776A - Method for removing impurity sodium by washing nickel-cobalt-manganese ternary precursor - Google Patents
Method for removing impurity sodium by washing nickel-cobalt-manganese ternary precursor Download PDFInfo
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- CN114388776A CN114388776A CN202111480201.2A CN202111480201A CN114388776A CN 114388776 A CN114388776 A CN 114388776A CN 202111480201 A CN202111480201 A CN 202111480201A CN 114388776 A CN114388776 A CN 114388776A
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/058—Construction or manufacture
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a method for removing impurity sodium by washing a nickel-cobalt-manganese ternary precursor, which comprises the following steps: s1, carrying out solid-liquid separation on a solid-liquid mixture of the nickel-cobalt-manganese ternary precursor crude product to obtain a solid ternary precursor crude product; s2, washing the solid ternary precursor crude product by using a sodium hydroxide solution to remove surface sulfate ions, and then dehydrating to obtain a dehydrated solid phase; s3, washing the dehydrated solid phase substance by using a dimethyl sulfoxide aqueous solution, and then carrying out solid-liquid separation to obtain a solid material; and S4, washing the solid material by using pure water, and dehydrating and drying to obtain a finished product. The advantages are that: the content of sodium ions in the nickel-cobalt-manganese ternary precursor can be obviously reduced.
Description
Technical Field
The invention relates to a production process of a precursor of a lithium ion battery anode material, in particular to a method for removing impurities in the precursor.
Background
The lithium ion battery mainly comprises a positive electrode material, a negative electrode material, a diaphragm, electrolyte and the like. The positive electrode material accounts for more than 40% of the total cost of the lithium battery, and the performance of the positive electrode material directly influences various performance indexes of the lithium battery. The ternary precursor is a main raw material of the ternary cathode material, in other words, the quality of the ternary precursor directly determines the performance of the ternary cathode material.
Besides conventional tap density, specific surface area and morphology parameters of the ternary precursor, impurities contained in the product can also influence the production and performance of the ternary cathode material, such as sodium ion content and sulfur element content. The Na and S elements in the ternary precursor are usually Na+、SO4 2-The content of the compound (A) can vary according to the product characteristics and the production process. There are two possible forms of sodium in the ternary precursor: 1. the crystal lattice of the ternary precursor is embedded into the crystal lattice of the ternary precursor, so that defects are caused to the crystal lattice of the ternary precursor; 2. exist between the ternary precursor layers. The content of the two existing modes cannot be reduced in the subsequent sintering process of the ternary cathode material, and on the contrary, part of sodium ions may occupy lithium ion sites in the sintering process, so that the performance of the ternary cathode material is irreversibly reduced. And the sulfur element generates corresponding pollution gas in the later calcination process of the ternary material and causes corrosion to calcination equipment. At present, the ternary precursor industry mainly removes sodium by removing mother liquor and washing, and the sodium content of the NCM523 product is about 200 ppm. While the mode of sulfur removal is usually thatCaustic soda is used for alkaline cleaning, and the sulfur content of the NCM523 product is about 1500 ppm. In order to further improve the quality of the ternary precursor, the reduction of the content of sodium-sulfur impurities in the ternary precursor is a compelling research content.
Disclosure of Invention
In order to further reduce the content of sodium-sulfur impurities in the ternary precursor, the invention provides a method for removing impurity sodium by washing the nickel-cobalt-manganese ternary precursor.
The technical scheme adopted by the invention is as follows: the method for removing impurity sodium by washing the nickel-cobalt-manganese ternary precursor comprises the step of washing by using a dimethyl sulfoxide aqueous solution.
The method can be specifically carried out according to the following operation steps:
s1, carrying out solid-liquid separation on a solid-liquid mixture of the nickel-cobalt-manganese ternary precursor crude product to obtain a solid ternary precursor crude product;
s2, washing the solid ternary precursor crude product by using a sodium hydroxide solution to remove surface sulfate ions, and then dehydrating to obtain a dehydrated solid phase;
s3, washing the dehydrated solid phase substance by using a dimethyl sulfoxide aqueous solution, and then carrying out solid-liquid separation to obtain a solid material;
and S4, washing the solid material by using pure water, and dehydrating and drying to obtain a finished product.
Wherein the concentration of the dimethyl sulfoxide aqueous solution is preferably 0.1-0.3 mol/L.
The invention also discloses a production method of the nickel-cobalt-manganese ternary precursor, which is characterized by comprising the method for removing impurity sodium by washing the nickel-cobalt-manganese ternary precursor.
The invention also discloses a nickel-cobalt-manganese ternary precursor, which is prepared by the production method of the nickel-cobalt-manganese ternary precursor.
The invention also discloses a production method of the lithium ion battery anode material, which is characterized in that the production raw material comprises the nickel-cobalt-manganese ternary precursor.
The invention also discloses a lithium ion battery anode material which is prepared by the production method of the lithium ion battery anode material.
The invention also discloses a production method of the lithium ion battery, which is characterized in that the production raw material comprises the lithium ion battery anode material.
The invention also discloses a lithium ion battery which is prepared by the production method of the lithium ion battery.
The invention also discloses a transportation tool comprising the lithium ion battery.
The invention has the beneficial effects that: the content of sodium ions in the nickel-cobalt-manganese ternary precursor can be obviously reduced.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The first embodiment is as follows:
washing the crude product of the nickel-cobalt-manganese ternary precursor according to the following method:
(1) 1m is3Performing intermediate-speed dehydration on a solid-liquid mixture of the nickel-cobalt-manganese ternary precursor crude product (slurry of the same batch is used in each embodiment and comparative example, and the granularity is 3.5-3.8 um) for 30min by using a centrifugal machine to obtain a solid ternary precursor crude product;
(2) using 1m3Carrying out spray washing on the solid ternary precursor crude product by using a sodium hydroxide solution with the concentration of 0.15mol/L to remove surface sulfate ions, and then carrying out intermediate-speed dehydration for 25min by using a centrifugal machine to obtain a dehydrated solid-phase substance;
(3) using 0.5m3Spraying and washing the dehydrated solid phase substance by using a dimethyl sulfoxide aqueous solution with the concentration of 0.15mol/L, and then dehydrating at a medium speed for 30min by using a centrifugal machine to obtain a solid material;
(4) using 3m3And spraying and washing the solid material by pure water, and dehydrating for 180min at a high speed by a centrifugal machine to obtain the centrifugal material.
Example two:
washing the crude product of the nickel-cobalt-manganese ternary precursor according to the following method:
(1) 1m is3Performing intermediate-speed dehydration on a solid-liquid mixture of the nickel-cobalt-manganese ternary precursor crude product (slurry of the same batch is used in each embodiment and comparative example, and the granularity is 3.5-3.8 um) for 30min by using a centrifugal machine to obtain a solid ternary precursor crude product;
(2) using 1m3Carrying out spray washing on the solid ternary precursor crude product by using a sodium hydroxide solution with the concentration of 0.15mol/L to remove surface sulfate ions, and then carrying out intermediate-speed dehydration for 25min by using a centrifugal machine to obtain a dehydrated solid-phase substance;
(3) using 1m3Spraying and washing the dehydrated solid phase substance by using a dimethyl sulfoxide aqueous solution with the concentration of 0.3mol/L, and then dehydrating at a medium speed for 30min by using a centrifugal machine to obtain a solid material;
(4) using 3m3And spraying and washing the solid material by pure water, and dehydrating for 180min at a high speed by a centrifugal machine to obtain the centrifugal material.
Comparative example one:
this comparative example is a comparative experiment to example two, carried out according to the same procedure and conditions as example two, with the only difference that: replacing the dimethyl sulfoxide aqueous solution in the step (3) with pure water with the same volume. The method comprises the following specific steps:
(1) 1m is3Performing intermediate-speed dehydration on a solid-liquid mixture of the nickel-cobalt-manganese ternary precursor crude product (slurry of the same batch is used in each embodiment and comparative example, and the granularity is 3.5-3.8 um) for 30min by using a centrifugal machine to obtain a solid ternary precursor crude product;
(2) using 1m3Carrying out spray washing on the solid ternary precursor crude product by using a sodium hydroxide solution with the concentration of 0.15mol/L to remove surface sulfate ions, and then carrying out intermediate-speed dehydration for 25min by using a centrifugal machine to obtain a dehydrated solid-phase substance;
(3) using 1m3Spraying and washing the dehydrated solid phase substance by pure water, and then dehydrating for 30min at a medium speed by using a centrifugal machine to obtain a solid material;
(4) using 3m3And spraying and washing the solid material by pure water, and dehydrating for 180min at a high speed by a centrifugal machine to obtain the centrifugal material.
The experimental results are as follows:
the centrates described in the above examples and comparative examples were tested for sodium content.
The detection method comprises the following steps:
1. after the centrifugal washing of the materials is finished, the materials are discharged to a containing container, and then 9g of the materials are sampled and are discharged to a PE bag for sodium content detection. (sampling 3g of material from the upper, middle and lower surfaces of the container respectively)
2. And measuring the sodium content by using an ICP (inductively coupled plasma) element analyzer, and taking the average of the two measurements as a result.
The results are shown in Table 1.
TABLE 1 table of sodium content test results of the centrifuge
From table 1, it can be seen that the sodium content of the centrifuge of example two, which was washed with the aqueous solution of dimethyl sulfoxide, is significantly lower than that of comparative example one, which was not washed with the aqueous solution of dimethyl sulfoxide under the same conditions, indicating that the sodium ion content of the nickel-cobalt-manganese ternary precursor can be significantly reduced by washing with the aqueous solution of dimethyl sulfoxide. The reason may be related to that the dimethyl sulfoxide aqueous solution can open the sheets of the crude ternary precursor product, increase the distance between the sheets of the crude ternary precursor product and weaken the acting force between layers.
Claims (10)
1. The method for removing impurity sodium by washing the nickel-cobalt-manganese ternary precursor is characterized by comprising the following steps: comprising a step of washing with an aqueous solution of dimethyl sulfoxide.
2. The method for washing the nickel-cobalt-manganese ternary precursor to remove impurity sodium according to claim 1, which is characterized by comprising the following steps:
s1, carrying out solid-liquid separation on a solid-liquid mixture of the nickel-cobalt-manganese ternary precursor crude product to obtain a solid ternary precursor crude product;
s2, washing the solid ternary precursor crude product by using a sodium hydroxide solution to remove surface sulfate ions, and then dehydrating to obtain a dehydrated solid phase;
s3, washing the dehydrated solid phase substance by using a dimethyl sulfoxide aqueous solution, and then carrying out solid-liquid separation to obtain a solid material;
and S4, washing the solid material by using pure water, and dehydrating and drying to obtain a finished product.
3. The method for removing impurity sodium by washing nickel cobalt manganese ternary precursor according to claim 1, characterized in that: the concentration of the dimethyl sulfoxide aqueous solution is 0.1-0.3 mol/L.
4. The production method of the nickel-cobalt-manganese ternary precursor is characterized by comprising the following steps of: the method for removing impurity sodium by washing the nickel-cobalt-manganese ternary precursor as claimed in any one of claims 1 to 3.
5. The nickel-cobalt-manganese ternary precursor obtained by the method for producing a nickel-cobalt-manganese ternary precursor according to claim 4.
6. The production method of the lithium ion battery anode material is characterized by comprising the following steps: the production feedstock comprises the nickel-cobalt-manganese ternary precursor of claim 5.
7. The lithium ion battery cathode material prepared by the lithium ion battery cathode material production method of claim 6.
8. The production method of the lithium ion battery is characterized by comprising the following steps: the production raw material comprises the lithium ion battery cathode material of claim 7.
9. A lithium ion battery produced by the lithium ion battery production method of claim 8.
10. A vehicle comprising the lithium ion battery of claim 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115995552A (en) * | 2023-03-23 | 2023-04-21 | 深圳中芯能科技有限公司 | Preparation method and application of sodium ion battery anode material |
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