CN113264561A - Water washing method of lithium ion cathode material - Google Patents
Water washing method of lithium ion cathode material Download PDFInfo
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- CN113264561A CN113264561A CN202110611591.6A CN202110611591A CN113264561A CN 113264561 A CN113264561 A CN 113264561A CN 202110611591 A CN202110611591 A CN 202110611591A CN 113264561 A CN113264561 A CN 113264561A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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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
- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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- 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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Abstract
The invention discloses a water washing method of a lithium ion anode material, which is characterized in that liquid nitrogen and ammonia azide are added into a water washing system when the lithium ion anode material is washed. The method has good cleaning effect on the residual alkali metal of the lithium ion anode material, has small structural damage to the material, and has small influence on the capacity, the cycle performance and the safety performance of the material.
Description
Technical Field
The invention belongs to the field of lithium ion anode materials, and relates to a water washing method of a lithium ion anode material.
Background
The water washing process is a key process of the lithium ion battery anode material, in particular to a ternary high nickel anode material. In the anode material washing process in the industry at present, deionized water is mainly adopted to directly carry out stirring, centrifuging, drying and other processes on the material at different times so as to take out residual alkali metals (lithium carbonate and lithium hydroxide) on the surface of the material, thereby improving the capacity, circulation and safety performance of the material.
However, when the deionized water is used for cleaning the cathode material, the main crystal structure of the cathode material is often damaged, so that the theoretical capacity and the cycle performance are reduced, and the deionized water is poor in removing effect of lithium carbonate and easy to remain, so that the safety performance and the cycle performance of the material are affected.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a water washing method of a lithium ion cathode material, which has good washing effect on residual alkali metal, small structural damage to the material and small influence on capacity, cycle performance and safety performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for washing a lithium ion anode material comprises the step of adding liquid nitrogen and ammonia azide into a washing system when the lithium ion anode material is washed.
The above-mentioned method for washing a lithium ion positive electrode material with water preferably comprises the steps of:
s1, adding ammonia azide into the ionized water, and adding liquid nitrogen to keep the temperature of the ionized water at 0-20 ℃;
s2, adding a lithium ion positive electrode material, stirring, washing, and continuously adding liquid nitrogen during the washing period to ensure that the temperature of the water-washed slurry is 0-20 ℃;
and S3, removing residual water in the water-washing slurry treated in the step S2, and drying to obtain the product.
In the above method for washing the lithium ion cathode material with water, the amount of the ammonia azide is preferably 0.05wt% to 1.00 wt% of the weight of the lithium ion cathode material.
In the above method for washing the lithium ion cathode material, preferably, the amount of the deionized water is 30-110 wt% of the lithium ion cathode material.
In the above method for washing a lithium ion positive electrode material, in step S2, the stirring time is preferably 0 to 60 min.
The method for washing the lithium ion cathode material is characterized in that in step S3, the drying is double-cone drying or roller kiln drying spray drying; the drying temperature is 80-250 ℃.
In the above-described method for washing the lithium ion positive electrode material with water, it is preferable that in step S3, spray drying, filter-press filtration or centrifugal filtration is used to remove residual water.
Compared with the prior art, the invention has the advantages that:
through a great deal of research and development, in the process of washing the residual alkali metal on the surface of the lithium ion battery material, the method improves the content of the residual Li by adding liquid nitrogen and ammonia azide into water2CO3The cleaning effect and efficiency can be realized, and simultaneously the material structure can be protected, and Li in the material can be prevented+Persistent withdrawal. Through analysis, the liquid nitrogen maintains the proper temperature of the solution in the water washing process, and accelerates Li on the surface of the matrix material2CO3The dissolution of (2) improves the washing efficiency, and then improves the washing and reduces the effect of the residual Li of the lithium carbonate on the surface of the material, and the ammonia azide forms a protective layer on the surface of the material, thereby preventing the sustainable damage of the water washing process water to the material, and balancing the solution Li of the water washing process+Concentration as buffer inhibitionLi in the material+The continuous separation is carried out to achieve the aim of the matrix material, and the liquid nitrogen can improve the solubility of the ammonia azide in the water washing solution while maintaining the low temperature, thereby further inhibiting Li in the water washing process+Can be continuously released. Therefore, the amount of Li remaining in the reaction solution is increased2CO3The cleaning effect and efficiency can be realized, and simultaneously the material structure can be protected, and Li in the material can be prevented+Is removed.
Drawings
Fig. 1 is a graph comparing cycle performance of lithium ion batteries manufactured from the positive electrode materials after being washed with water by the water washing method of examples 1 to 3 and the conventional water washing method.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The invention discloses a lithium ion positive electrode material, which is characterized in that a main crystal structure of the positive electrode material is easy to damage when residual alkali metal on the surface of the positive electrode material is cleaned by using the conventional water washing agent and the conventional water washing method, and the removal effect is poor and the residual alkali metal is easy to remain, so that the theoretical capacity is reduced, the safety performance and the cycle performance of the material are influenced, and the technical problem can be effectively solved by adding liquid nitrogen and ammonia azide into a water washing system in the water washing process through a large amount of researches.
The materials and equipment used in the following examples are commercially available.
Example 1:
a water washing method of a lithium ion cathode material comprises the following steps:
(1) introducing the deionized water into a beaker, wherein the weight of the deionized water is 80wt% of that of water washing materials, and the water washing materials are high-nickel NCM (811) polycrystalline materials;
(2) adding a proper amount of liquid nitrogen, and ensuring the temperature of the deionized water in the step (1) to be 5 ℃;
(3) adding ammonia azide, wherein the weight of the ammonia azide is 0.05wt% of that of the water-washed material;
(4) slowly adding the water-washed material at a constant speed within 2 minutes, stirring for 10 minutes, continuously adding liquid nitrogen during the stirring, ensuring the temperature of the water-washed slurry to be 5 ℃, and obtaining the water-washed material;
(5) filter pressing and filtering to remove residual water;
(6) and (3) drying: drying by adopting a double cone at the drying temperature of 200 ℃.
XRD detection is carried out on the lithium ion battery anode material after washing, and the crystal form is not changed, which indicates that the main structure of the material after washing is not changed.
Example 2:
a water washing method of a lithium ion cathode material comprises the following steps:
(1) introducing the deionized water into a beaker, wherein the weight of the deionized water is 80wt% of that of water washing materials, and the water washing materials are high-nickel NCM (811) polycrystalline materials;
(2) adding a proper amount of liquid nitrogen, and ensuring the temperature of the deionized water in the step (1) to be 15 ℃;
(3) adding ammonia azide, wherein the weight of the ammonia azide is 0.20wt% of that of the water washing material;
(4) slowly adding the water-washed material at a constant speed within 2 minutes, stirring for 10 minutes, continuously adding liquid nitrogen during the stirring, ensuring the temperature of the water-washed slurry to be 15 ℃, and obtaining the water-washed material;
(5) removing residual water; one of spray drying, filter pressing filtration and centrifugal filtration can be selected;
(6) drying at 200 deg.C; one of bipyramid drying and roller kiln drying and spray drying can be selected.
XRD detection is carried out on the lithium ion battery anode material after washing, and the crystal form is not changed, which indicates that the main structure of the material after washing is not changed.
Example 3:
a water washing method of a lithium ion cathode material comprises the following steps:
(1) introducing the deionized water into a beaker, wherein the weight of the deionized water is 80wt% of that of water washing materials, and the water washing materials are high-nickel NCM (811) polycrystalline materials;
(2) adding a proper amount of liquid nitrogen, and ensuring the temperature of the deionized water in the step (1) to be 5 ℃;
(3) adding ammonia azide, wherein the weight of the ammonia azide is 0.60wt% of that of the water washing material;
(4) slowly adding the water-washed material at a constant speed within 2 minutes, stirring for 10 minutes, continuously adding liquid nitrogen during the stirring, ensuring the temperature of the water-washed slurry to be 5 ℃, and obtaining the water-washed material;
(5) removing residual water; one of spray drying, filter pressing filtration and centrifugal filtration can be selected;
(6) drying at 200 deg.C; one of bipyramid drying and roller kiln drying and spray drying can be selected.
XRD detection is carried out on the lithium ion battery anode material after washing, and the crystal form is not changed, which indicates that the main structure of the material after washing is not changed.
The surface residual Li of the positive electrode material cleaned by the above-mentioned each example and the conventional cleaning method is carried out2CO3And Li/Me (i.e., the molar ratio of Li to other metals in the cathode material after water washing) with the results shown in table 1.
The positive electrode material cleaned by the above-mentioned embodiments and the conventional cleaning method is matched with metal Li to manufacture a half cell, wherein the positive electrode slurry for preparing the positive electrode plate comprises the positive electrode material, the conductive agent and the binder (mass ratio is 92:4: 4) after water washing. And (3) carrying out charge and discharge tests on the prepared battery, wherein the test conditions are as follows: the charging and discharging voltage range is 2.8-4.25V, the capacity test is 0.1C, the cycle test is 1C, and the accuracy of data is reduced when the cycle performance test of the half-cell exceeds 50 weeks, so the cycle number is 50 weeks. The electrochemical properties of the test are shown in table 1, and the cycle performance chart is shown in fig. 1.
TABLE 1
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (7)
1. A washing method of a lithium ion anode material is characterized in that liquid nitrogen and ammonia azide are added into a washing system in the process of washing the lithium ion anode material.
2. The method for washing a lithium ion positive electrode material according to claim 1, comprising the steps of:
s1, adding ammonia azide into the ionized water, and adding liquid nitrogen to keep the temperature of the ionized water at 0-20 ℃;
s2, adding a lithium ion positive electrode material, stirring, washing, and continuously adding liquid nitrogen during the washing period to ensure that the temperature of the water-washed slurry is 0-20 ℃;
and S3, removing residual water in the water-washing slurry treated in the step S2, and drying to obtain the product.
3. The method for washing a lithium ion positive electrode material according to claim 2, wherein the amount of the ammonia azide is 0.05 to 1.00% by weight based on the weight of the washed material.
4. The method for washing a lithium ion positive electrode material according to claim 2, wherein the amount of the deionized water is 30 to 110wt% of the lithium ion positive electrode material.
5. The method for washing a lithium ion positive electrode material according to claim 2, wherein the stirring time in step S2 is 0 to 60 min.
6. The method for washing a lithium ion positive electrode material according to claim 2, wherein the drying is double cone drying or roller kiln drying spray drying in step S3; the drying temperature is 80-250 ℃.
7. The method for washing a lithium ion positive electrode material according to claim 2, wherein in step S3, residual water in the washing slurry is removed by spray drying, filter-press filtration or centrifugal filtration.
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