CN110550668A - Process preparation method of power type single crystal NCM622 type precursor concentrator - Google Patents
Process preparation method of power type single crystal NCM622 type precursor concentrator Download PDFInfo
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- CN110550668A CN110550668A CN201910674349.6A CN201910674349A CN110550668A CN 110550668 A CN110550668 A CN 110550668A CN 201910674349 A CN201910674349 A CN 201910674349A CN 110550668 A CN110550668 A CN 110550668A
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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
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
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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
Abstract
The invention relates to the field of new energy NCM ternary precursors, in particular to a process preparation method of a power type single crystal NCM622 type precursor concentrator, which comprises the following steps: (1) preparing a nickel-cobalt-manganese sulfate solution with a certain concentration by using soluble salts of nickel sulfate, manganese sulfate and cobalt sulfate as raw materials; (2) adding ammonia water into the prepared nickel-cobalt-manganese solution according to a certain proportion to form a mixed solution, taking a sodium hydroxide solution as a precipitator, and carrying out coprecipitation reaction to obtain mixed slurry; (3) reacting in a reaction kettle, stopping overflowing when the solid content meets the requirement, concentrating, and controlling the particle size to be below 2.6 microns; (4) and finally, washing by a washing tank, drying, screening, deironing and packaging to obtain the dynamic single crystal NCM622 precursor. The precursor prepared by the method has the advantages of simple process, high sphericity, compact surface particles, low cost and good safety.
Description
Technical Field
The invention belongs to the field of new energy NCM ternary precursors, and particularly relates to a process preparation method of a power type single crystal NCM622 type precursor concentrator.
Background
With the problem of increasingly worsening global environment, new energy clean automobiles are vigorously popularized and developed all over the world. Here, the technology of the lithium battery is indispensable, and government departments increasingly promote, propose and advocate development of new energy automobiles, and nowadays, electric vehicles are used in many areas. Therefore, the development of the lithium battery has certain prospects.
The physical properties of the ternary precursor determine the performance of the cathode material to a certain extent, because the particle size, the morphology and the structure of the nickel-cobalt-manganese hydroxide particles have a direct relationship with the physical properties of the ternary cathode material. At present, a plurality of methods for preparing the ternary precursor are available, such as a one-step synthesis method, a sol-gel method, a hydrothermal and solvothermal synthesis method, a microwave thermosynthesis method, a low-heat solid phase reaction, a coprecipitation synthesis method and the like, and the hydroxide coprecipitation method adopted by the production of the ternary precursor of most manufacturers is that a mixed solution of nickel, cobalt and manganese, a precipitator, a complexing agent and the like are added to the bottom of a reaction kettle in a parallel flow mode, and the ternary precursor, namely nickel-cobalt-manganese hydroxide can be synthesized under certain conditions.
the common ternary precursor nickel-cobalt-manganese ratio is 424, 333, 523, 701 and 515, the gram capacity of the ternary precursor is generally about 150mAh/g, the energy density is low, and the battery prepared on the basis of the method is low in capacity and is not suitable for pursuing the requirement of a high-capacity battery.
Disclosure of Invention
Based on the prior art, the invention aims to provide a process of a dynamic single crystal NCM622 type precursor concentrator, and the single crystal NCM622 type precursor prepared by the invention has the advantages of simple process, high sphericity, compact surface particles, low cost and good safety.
In order to achieve the above purpose, the invention adopts the technical scheme that:
A process preparation method of a dynamic single crystal NCM622 precursor concentrator comprises the following steps:
(1) Preparing a nickel-cobalt-manganese sulfate solution with a certain concentration by using soluble salts of nickel sulfate, manganese sulfate and cobalt sulfate as raw materials;
(2) Adding ammonia water into the prepared nickel-cobalt-manganese solution according to a certain proportion to form a mixed solution, taking a sodium hydroxide solution as a precipitator, and carrying out coprecipitation reaction to obtain mixed slurry;
(3) Carrying out coprecipitation reaction in a reaction kettle, stopping overflowing when the solid content meets the requirement, concentrating, and controlling the particle size to be below 2.6 microns;
(4) and finally, washing by a washing tank, drying, screening, deironing and packaging to obtain the dynamic single crystal NCM622 precursor.
In order to better realize the invention, further, the molar concentration of the nickel-cobalt-manganese sulfate solution prepared in the step (1) is 1.5-1.7 mo1/L, and in the nickel-cobalt-manganese sulfate mixed solution, the molar ratio of nickel, cobalt and manganese is x: y: z, wherein x + y + z is 1.
In order to better implement the present invention, the chemical formula of the nickel-cobalt-manganese precursor formulated in step (1) is (NixCoyMnz) OH 2, wherein x + y + z is 1, x is 0.6, y is 0.2, and z is 0.2.
in order to better realize the method, the molar concentration of the complexing agent ammonia water in the step (2) is 12-14 mol/L; the molar concentration content of the sodium hydroxide solution is 4-6 mol/L.
In order to better implement the present invention, further, the control conditions of the coprecipitation reaction process in step (3) are as follows: controlling the flow of the nickel-cobalt-manganese solution entering the reaction kettle to be 40-44L/h, the stirring speed to be 900-1100 r/min, the reaction temperature to be 49-51 ℃, the ammonia value to be 7-8 g/L, the protective atmosphere to be a nitrogen atmosphere, the precipitation reaction time to be 30-96 h, and the pH value in the reaction kettle to be 11.45-11.74.
In order to better realize the method, in the step (3), the material liquid in the reaction kettle overflows to the aging kettle in the front reaction period, in the process, a sample in the reaction kettle is taken, the solid content is measured, when the solid content reaches a certain value, the overflow valve is closed, the concentrated solution enters a concentrator for concentration, and the reaction and the discharging are stopped when the granularity is 3.44-3.80 microns after the concentration.
In order to better realize the method, the prepared precursor is washed by deionized water in the step (4), the temperature of the deionized water is 60-80 ℃, Na in the product is less than or equal to 0.0052%, S is less than or equal to 0.36%, and the resistivity of the washed NCM622 is less than 0.025 cm/us.
In order to better realize the method, the drying in the step (4) adopts microwave drying, the microwave frequency is 2.2-2.7 GHz, and the temperature is less than 200 ℃.
In order to better realize the invention, the chemical formula of the prepared NCM622 precursor is Ni 0.6 Co 0.2 Mn 0.2 (OH) 2, the appearance is spherical, the D50 is 3.44-3.80 microns, and the apparent density is 0.89-1.33 g/cm 3.
advantageous effects
The invention has the following beneficial effects:
1. According to the method for preparing the nickel-cobalt-manganese precursor, the prepared nickel-cobalt-manganese solution is added with ammonia water according to a certain proportion to form a mixed solution, then sodium hydroxide is added to be used as a precipitator for coprecipitation reaction, the solid content is improved by using a concentrator process in the reaction process, and finally the obtained product is aged, washed and dried to obtain the nickel-cobalt-manganese precursor which has the advantages of high sphericity, compact surface particles, simple production process, low cost, high gram volume and good safety.
2. In the process, a concentrator process is used, and the crystallization density of the final finished product can be better controlled by controlling the particle size after concentration, so that the finished product has good spherical shape and high density, and the battery prepared on the basis of the finished product has high capacity.
3. The microwave drying technology is better than the rotary kiln technology in drying the ternary precursor, metal pollution is completely avoided, and the drying speed is high, the ternary precursor can be dried in a few minutes, and the drying is uniform, the quality is good, the drying temperature is low, the energy consumption is reduced, and the like.
Drawings
FIG. 1 is a schematic diagram of a process for preparing type 622 precursor by a thickener process;
FIG. 2 is a 3000-fold scanning electron microscope image of the nickel-cobalt-manganese hydroxide 622 prepared in example 1 of the present invention;
FIG. 3 is a 5000 times scanning electron microscope image of nickel cobalt manganese hydroxide 622 prepared in example 1 of the present invention;
FIG. 4 is a 3000-fold scanning electron microscope image of the nickel-cobalt-manganese hydroxide 622 prepared in example 2 of the present invention;
FIG. 5 is a 5000 times scanning electron microscope image of Ni-Co-Mn hydroxide 622 prepared in example 2 of the present invention;
FIG. 6 is a 2000-fold scanning electron micrograph of nickel-cobalt-manganese hydroxide 622 prepared according to example 3 of the present invention;
FIG. 7 is a 5000 times scanning electron microscope image of nickel cobalt manganese hydroxide 622 prepared in example 3 of the present invention;
Detailed Description
the present invention will be described in further detail with reference to specific examples.
Example 1
The embodiment provides a process preparation method of a dynamic single crystal NCM622 precursor concentrator, which comprises the following steps:
The preparation method comprises the steps of preparing nickel sulfate NiSO 4 & 6H 2 O, cobalt sulfate CoSO 4 & 7H 2 O and manganese sulfate MnSO 4 & H 2 O according to the molar ratio of Ni to Co to Mn being 6:2:2, preparing a nickel-cobalt-manganese sulfate mixed solution with the concentration of 1.5-1.55 mol/L, preparing a 5mol/L NaOH solution as a precipitator, respectively feeding the nickel-cobalt-manganese sulfate mixed solution, the NaOH solution and an ammonia solution into a reaction kettle by using a pump, improving the solid content by overflowing within the first 24 hours, closing an overflow valve when the solid content meets the requirement, enabling the material to enter the reaction kettle through a concentrator for circulation, continuously growing particles when the particles grow to be between 3.44 and 3.71 micrometers, discharging the fine powder after disappearance, discharging the material when the solid content meets the requirement, discharging the overflow valve, discharging the discharged supernatant when the solid content meets the requirement, discharging the supernatant after the discharge, discharging the supernatant after the discharge, the.
example 2
The embodiment provides a process preparation method of a dynamic single crystal NCM622 precursor concentrator, which comprises the following steps:
The preparation method comprises the steps of preparing nickel sulfate NiSO 4 & 6H 2 O, cobalt sulfate CoSO 4 & 7H 2 O and manganese sulfate MnSO 4 & H 2 O into a nickel-cobalt-manganese sulfate mixed solution with the concentration of 1.55-1.6 mol/L and a 5mol/L NaOH solution as a precipitating agent according to the mol ratio of Ni to Co to Mn of 6:2:2, respectively feeding the nickel-cobalt-manganese sulfate mixed solution, the NaOH solution and the ammonia solution into a reaction kettle with the effective volume of 2m 3 by a pump, strictly controlling the temperature in the reaction kettle to be 50 ℃ under the protection of N 2, enabling the pH value to fluctuate between 11.50 and 11.70, enabling the stirring rate to be about 1100r/min, increasing the solid content within the first 24 hours by overflowing, closing an overflow valve when the solid content meets the requirement, enabling the material to enter the reaction kettle for circulation through a concentrator, continuously growing particles when the particles grow to be between 3.5 and 3.7 microns and disappear, discharging the particles to be discharged after the solid content reaches the requirement, discharging the overflow valve is removed, enabling the supernatant to be discharged to be less than 0.8290.5-1-0-hour, washing the supernatant of a supernatant fluid of a deionized water with a washing slurry with a microwave washing process of a washing slurry with the temperature of less than 30-80-30-20-cm, and a washing slurry with a microwave washing slurry with a washing temperature of a washing slurry of a deionized water of a washing slurry of a supernatant fluid of a washing tank with a washing machine to be less than a supernatant fluid of a washing slurry with a supernatant fluid of a microwave washing machine to be less than a washing temperature of a washing machine to.
example 3
The embodiment provides a process preparation method of a dynamic single crystal NCM622 precursor concentrator, which comprises the following steps:
The preparation method comprises the steps of preparing nickel sulfate NiSO 4 & 6H 2 O, cobalt sulfate CoSO 4 & 7H 2 O and manganese sulfate MnSO 4 & H 2 O according to the molar ratio of Ni to Co to Mn being 6:2:2, preparing a nickel-cobalt-manganese sulfate mixed solution with the concentration of 1.6-1.7 mol/L, preparing a 5mol/L NaOH solution as a precipitator, respectively feeding the nickel-cobalt-manganese sulfate mixed solution, the NaOH solution and an ammonia solution into a reaction kettle by using a pump, enabling the effective volume of the reaction kettle to be 2m 3, strictly controlling the temperature in the reaction kettle to be 51 ℃, enabling the pH value to fluctuate between 11.45 and 11.70 under the protection of N2, enabling the stirring rate to be about 1100r/min through overflow within the first 24 hours, increasing the solid content through overflow, closing the overflow valve when the solid content meets the requirement, enabling the material to enter the reaction kettle to circulate, enabling particles to grow continuously when the particles grow to be 3.44-3.60 micrometers, stopping the reactor after the fine powder disappears, discharging the solid content reaches the requirement, discharging the discharge is completed, enabling the supernatant to be discharged, enabling the supernatant to be larger than 0.26 cm, enabling the supernatant to be larger than 0.44 cm, enabling the supernatant to be larger than 0.80 mm, washing temperature of the supernatant to be larger than the washing temperature of a washing tank to be smaller than 0.80-60, and the washing temperature of a washing tank to be smaller than 0.20 cm, and the washing temperature of a washing slurry to be smaller than a washing temperature of a washing tank to be smaller than 0.80-60-53 micron washing slurry, and enabling the supernatant to be smaller than the washing.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A process preparation method of a dynamic single crystal NCM622 precursor concentrator is characterized by comprising the following steps:
(1) Preparing a nickel-cobalt-manganese sulfate solution with a certain concentration by using soluble salts of nickel sulfate, manganese sulfate and cobalt sulfate as raw materials;
(2) adding ammonia water into the prepared nickel-cobalt-manganese solution according to a certain proportion to form a mixed solution, taking a sodium hydroxide solution as a precipitator, and carrying out coprecipitation reaction to obtain mixed slurry;
(3) carrying out coprecipitation reaction in a reaction kettle, stopping overflowing when the solid content meets the requirement, concentrating, and controlling the particle size to be below 2.6 microns;
(4) and finally, washing by a washing tank, drying, screening, deironing and packaging to obtain the dynamic single crystal NCM622 precursor.
2. The process preparation method of the power type single crystal NCM622 precursor concentrator according to claim 1, wherein the molar concentration of the nickel cobalt manganese sulfate solution prepared in the step (1) is 1.5-1.7 mo1/L, and the molar ratio of nickel, cobalt and manganese in the nickel cobalt manganese sulfate mixed solution is x: y: z, wherein x + y + z is 1.
3. The method of claim 1, wherein the ni-co-mn precursor formulated in step (1) has a chemical formula of (NixCoyMnz) OH 2, wherein x + y + z is 1, x is 0.6, y is 0.2, and z is 0.2.
4. The process preparation method of the power type monocrystal NCM622 precursor concentrator according to claim 1, characterized in that the ammonia water molar concentration of the complexing agent in the step (2) is 12-14 mol/L; the molar concentration content of the sodium hydroxide solution is 4-6 mol/L.
5. The process preparation method of a dynamic single crystal NCM622 precursor according to claim 1, wherein the coprecipitation reaction process control conditions in step (3) are as follows: controlling the flow of the nickel-cobalt-manganese solution entering the reaction kettle to be 40-44L/h, the stirring speed to be 900-1100 r/min, the reaction temperature to be 49-51 ℃, the ammonia value to be 7-8 g/L, the protective atmosphere to be a nitrogen atmosphere, the precipitation reaction time to be 30-96 h, and the pH value in the reaction kettle to be 11.45-11.74.
6. The process preparation method of a power type single crystal NCM622 type precursor concentrator according to claim 1, characterized in that in the step (3), the reaction front period time is that the feed liquid in the reaction kettle overflows to the aging kettle, in the process, the sample in the reaction kettle is taken, the solid content is measured, when the solid content reaches a certain value, the overflow valve is closed, the sample enters the concentrator for concentration, and the reaction discharging is stopped when the particle size is 3.44-3.80 microns after the concentration.
7. The process preparation method of the power type monocrystal NCM622 type precursor concentrator as claimed in claim 1, wherein the prepared precursor is washed by deionized water in the step (4), the temperature of the deionized water is 60-80 ℃, Na in the product is less than or equal to 0.0052%, S in the product is less than or equal to 0.36%, and the resistivity of the washed NCM622 is less than 0.025 cm/us.
8. the process preparation method of the power type single crystal NCM622 precursor concentrator according to claim 1, characterized in that the drying in the step (4) adopts microwave drying, the microwave frequency is 2.2-2.7 GHz, and the temperature is less than 200 ℃.
9. The method for preparing a dynamic single crystal NCM622 precursor by the concentrator process according to claim 1, wherein the chemical formula of the prepared NCM622 precursor is Ni 0.6 Co 0.2 Mn 0.2 (OH) 2, the appearance is spherical, D50 is 3.44-3.80 microns, and the apparent density is 0.89-1.33 g/cm 3.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111847529A (en) * | 2020-07-23 | 2020-10-30 | 华友新能源科技（衢州）有限公司 | Method for removing sulfur content in hydroxide precursor |
| CN112194194A (en) * | 2020-08-27 | 2021-01-08 | 浙江美都海创锂电科技有限公司 | Method for preparing single crystal NCMA precursor material |
| CN112694139A (en) * | 2020-12-29 | 2021-04-23 | 福建常青新能源科技有限公司 | Preparation method of single crystal NCM ternary positive electrode material precursor |
| CN113130886A (en) * | 2019-12-30 | 2021-07-16 | 荆门市格林美新材料有限公司 | Preparation method and application of superfine high-nickel ternary precursor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112694139A (en) * | 2020-12-29 | 2021-04-23 | 福建常青新能源科技有限公司 | Preparation method of single crystal NCM ternary positive electrode material precursor |
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