CN107623124B - Preparation method of spherical nickel-cobalt-manganese precursor material - Google Patents
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Abstract
The invention discloses a preparation method of a spherical nickel-cobalt-manganese precursor material, which comprises the following steps: preparing slurry containing spherical nickel-cobalt-manganese precursor particles by a coprecipitation method, performing solid-liquid separation on the slurry to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, aging the obtained spherical nickel-cobalt-manganese precursor particles, washing with water to obtain a spherical nickel-cobalt-manganese precursor material product, collecting the mother liquor obtained after the solid-liquid separation and washing wastewater generated in the washing process respectively, mixing the collected mother liquor and the washing wastewater to obtain a wastewater solution, supplementing pure water to control the concentration of sodium ions in the wastewater solution to be less than 25g/L, filtering the wastewater solution by a fine filter to obtain recycled water, and returning the recycled water to the coprecipitation method for preparing the spherical nickel-cobalt-manganese precursor particles to be used as alkali liquor for recycling. The preparation method has the advantages of low water consumption, low sewage generation and low production cost, and the physicochemical indexes of the obtained product meet the standard requirements.
Description
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a preparation method of a spherical nickel-cobalt-manganese precursor material.
Background
The lithium ion battery as a novel green secondary battery has the advantages of large specific capacity, small self-discharge, light weight, no memory effect and the like. The electric vehicle is widely applied to the fields of various mobile electronic products (such as mobile phones, cameras, notebook computers and the like), artificial satellites, aerospace and the like, and has breakthrough development in the field of electric vehicles. In order to meet the requirements of the increasing development of the application fields, the nickel-cobalt-manganese precursor material is rapidly developed, and the yield is increased.
At present, the common method for preparing nickel-cobalt-manganese precursor material is controlled crystal hydroxide coprecipitation method, i.e. wet synthesis, and mixed metal hydroxide precipitate is obtained by precipitating mixed metal salt solution with sodium hydroxide under the action of complexing agent. The precursor material nickel cobalt manganese element prepared by the wet synthesis has uniform precipitation distribution and stable product quality, and is a main method of the current industrialized production. However, the wet synthesis preparation can generate a large amount of wastewater in the production process, 20 t-25 t of wastewater can be generated in the production of 1t of nickel-cobalt-manganese precursor material, and the wastewater contains a large amount of sodium sulfate, ammonia water and a small amount of heavy metals of nickel and cobalt. Through the common wastewater treatment, only ammonia and heavy metals in the wastewater can be simply treated and recovered, the treatment cost is very high, and the cost for treating the wastewater is about 80 yuan/t.
Therefore, in order to reduce the production cost and reduce the sewage discharge, it is necessary to develop a preparation method of the nickel-cobalt-manganese precursor material with less water consumption on the premise of not affecting the product quality.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings in the background technology and provide a preparation method of a spherical nickel-cobalt-manganese precursor material with low water consumption, less sewage and low production cost.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a spherical nickel-cobalt-manganese precursor material comprises the following steps: preparing slurry containing spherical nickel-cobalt-manganese precursor particles by a coprecipitation method, performing solid-liquid separation on the slurry to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, aging the obtained spherical nickel-cobalt-manganese precursor particles, washing with water to obtain a spherical nickel-cobalt-manganese precursor material product, collecting the mother liquor obtained after the solid-liquid separation and washing wastewater generated in the washing process respectively, mixing the collected mother liquor and the washing wastewater to obtain a wastewater solution, supplementing pure water to control the concentration of sodium ions in the wastewater solution to be less than 25g/L, filtering the wastewater solution by a fine filter to obtain recycled water, and returning the recycled water to the coprecipitation method for preparing the spherical nickel-cobalt-manganese precursor particles to be used as alkali liquor for recycling.
The water consumption in the water washing procedure in the production process of the nickel-cobalt-manganese precursor material is large, 1t of product is generated, and about 10t of washing water is needed; in addition, the amount of mother liquor generated in the precipitation process is large, the volume of the generated 1t of product mother liquor is about 15 cubic, and the concentration and the pH value of sodium ions in the mother liquor are high. The method comprises the steps of modifying the process flow, mixing the mother liquor with the washing wastewater, adding pure water for dilution, controlling the concentration of sodium ions in the wastewater solution to be less than 25g/L, carrying out fine filtration to obtain reuse water, and returning the reuse water to the production process of the coprecipitation method for reuse as alkali liquor. By the method, the mother liquor and the washing wastewater are recycled, the water consumption and the wastewater consumption in production are reduced, the difficulty in sewage treatment is reduced, and the ammonia is directly recycled. The method effectively reduces the production cost of the spherical nickel-cobalt-manganese precursor material, reduces the water consumption for production by more than 50 percent, simultaneously reduces the reuse rate of ammonia water by more than 50 percent and the alkali liquor by about 10 percent, does not influence each physical and chemical index of the product, and meets the quality standard requirement of qualified products.
In the above preparation method, preferably, the concentration of sodium ions in the mother liquor is 40g/L to 80g/L, and the concentration of sodium ions in the washing wastewater is 10g/L to 25 g/L.
In the preparation method, preferably, the specific process of preparing the slurry containing the spherical nickel-cobalt-manganese precursor particles by the coprecipitation method is as follows:
(1) preparing soluble salts of nickel, cobalt and manganese into a nickel-cobalt-manganese ion mixed solution according to the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese precursor, and controlling the total concentration of nickel, cobalt and manganese ions in the nickel-cobalt-manganese ion mixed solution to be 60 g/L-120 g/L;
(2) uniformly mixing the ammonia water solution and the sodium hydroxide water solution according to a certain volume ratio to obtain alkali liquor with the ammonia concentration of 6-40 g/L;
(3) adding the obtained mixed solution of nickel, cobalt and manganese ions and alkali liquor into a reaction kettle with a base solution in a parallel flow manner, wherein the base solution is a mixed solution of ammonia water and sodium hydroxide with the ammonia concentration of 6-35 g/L, the pH value of 10.3-11 and the temperature of 45-70 ℃, and nitrogen is continuously introduced for protection before and during the reaction;
(4) and in the reaction, controlling the pH of the reaction solution to be 10.8-11.5, the temperature to be 45-70 ℃, the stirring speed to be 150-350 r/min and the ammonia concentration to be 6-35 g/L, and carrying out continuous coprecipitation reaction to obtain the slurry containing spherical nickel-cobalt-manganese precursor particles.
In the preparation method, more preferably, the recycling of the reuse water as the alkali liquor in the process of preparing the spherical nickel-cobalt-manganese precursor particles by the coprecipitation method specifically includes: in the step (2), the reuse water, the ammonia water solution and the sodium hydroxide water solution are uniformly mixed according to a certain volume ratio to obtain the alkali liquor with the ammonia concentration of 6-40 g/L.
In the above preparation method, preferably, in the step (1), the soluble salt of nickel, cobalt and manganese specifically refers to sulfate, chloride or nitrate of nickel, cobalt and manganese.
In the preparation method, preferably, the chemical molecular formula of the spherical nickel-cobalt-manganese precursor material is Ni1-x- yCoxMny(OH)2Wherein x is more than 0.01 and less than 0.1, and y is more than 0.01 and less than 0.1.
Compared with the prior art, the invention has the advantages that: the method comprises the steps of uniformly mixing mother liquor and washing wastewater generated in the production of a nickel-cobalt-manganese precursor material by a coprecipitation method, diluting with pure water, and finely filtering to obtain reuse water; the reuse water is returned to the production process of the coprecipitation method and is used as alkali liquor for recycling. The method can reduce the production water by more than 50 percent, reduce the ammonia water dosage by more than 50 percent and the alkali dosage by more than 10 percent, greatly reduce the production cost and the environmental protection pressure on the premise of ensuring the product quality, create profits for enterprises, well protect the environment and play a win-win role for the enterprises and the society.
In general, compared with the existing wet synthesis process of nickel-cobalt-manganese precursors, the method can save production water, reduce the consumption of ammonia water and reduce the production cost on the premise of ensuring the product quality; the preparation method provided by the invention is simple in process flow, can realize continuous production, and is stable and excellent in product quality.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a preparation method of a spherical nickel-cobalt-manganese precursor material, which comprises the following specific steps:
(1) dissolving nickel chloride, cobalt chloride and manganese chloride into water according to the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese precursor material to be prepared to prepare a nickel-cobalt-manganese ion mixed solution, and controlling the total concentration of nickel, cobalt and manganese ions in the nickel-cobalt-manganese ion mixed solution to be 115 g/L;
(2) uniformly mixing the ammonia water solution and the sodium hydroxide water solution to prepare an alkali liquor with the ammonia concentration of 20 g/L; mixing the mixed solution of nickel, cobalt and manganese ions with alkaliThe solution is added into a reaction kettle with good tightness and bottom solution in parallel flow to carry out continuous coprecipitation reaction, nitrogen is continuously introduced in the reaction process, the pH value of the reaction solution is controlled to be 10.8-11.2, the temperature is controlled to be 60 ℃, the stirring speed is controlled to be 175r/min, and the ammonia concentration is controlled to be 15 g/L; the used base solution is a mixed solution of ammonia water and sodium hydroxide, wherein the ammonia concentration is 15g/L, the pH value is 10.9-11, and the temperature is 60 ℃; preparing slurry containing nickel, cobalt and manganese precursor particles, wherein the chemical molecular formula of the spherical nickel, cobalt and manganese precursor particles is Ni1-x-yCoxMny(OH)2Wherein 0.01 < x < 0.1, 0.01 < y < 0.1, for example Ni0.6Co0.2Mn0.2(OH)2；
(3) Carrying out solid-liquid separation on the slurry containing the nickel-cobalt-manganese precursor particles to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, then aging the spherical nickel-cobalt-manganese precursor particles, and then washing the precursor material on a centrifugal machine or a filter press by pure water to obtain a spherical nickel-cobalt-manganese precursor material, wherein the concentration of sodium ions in the mother liquor is 40-50 g/L, and the concentration of sodium ions in washing wastewater is 10-25 g/L;
(4) respectively collecting mother liquor obtained after solid-liquid separation and washing wastewater generated in the washing process, mixing the collected mother liquor with the washing wastewater to obtain a wastewater solution, adding pure water to dilute the sodium ion concentration in the wastewater solution to 20g/L, filtering the wastewater solution by using a fine filter to obtain reuse water, and returning the reuse water to the step (2) to be mixed with the ammonia water solution and the sodium hydroxide aqueous solution to be reused as alkali liquor.
After multiple cycles of reuse water, a small amount of washed spherical nickel-cobalt-manganese precursor material is taken as a sample A, and the physicochemical performance indexes of the sample A are tested, and the test results are shown in Table 1.
Comparative example 1:
a preparation method of an existing spherical nickel-cobalt-manganese precursor material comprises the following specific steps:
(1) dissolving nickel chloride, cobalt chloride and manganese chloride into water according to the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese precursor material to be prepared to prepare a nickel-cobalt-manganese ion mixed solution, and controlling the total concentration of nickel, cobalt and manganese ions in the nickel-cobalt-manganese ion mixed solution to be 115 g/L;
(2) uniformly mixing the ammonia water solution and the sodium hydroxide water solution to prepare an alkali liquor with the ammonia concentration of 20 g/L; the method comprises the following steps of adding a nickel-cobalt-manganese ion mixed solution and an alkali liquor into a reaction kettle which is filled with a base solution and has good sealing performance to perform continuous coprecipitation reaction, continuously introducing nitrogen in the reaction process, controlling the pH value of a reaction solution to be 10.8-11.2, controlling the temperature to be 60 ℃, controlling the stirring speed to be 175r/min and controlling the ammonia concentration to be 15 g/L; the used base solution is a mixed solution of ammonia water and sodium hydroxide, wherein the ammonia concentration is 15g/L, the pH value is 10.9-11, and the temperature is 60 ℃; preparing slurry containing nickel, cobalt and manganese precursor particles, wherein the chemical molecular formula of the spherical nickel, cobalt and manganese precursor particles is Ni1-x-yCoxMny(OH)2Wherein 0.01 < x < 0.1, 0.01 < y < 0.1, for example Ni0.6Co0.2Mn0.2(OH)2；
(3) Carrying out solid-liquid separation on the slurry containing the nickel-cobalt-manganese precursor particles to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, then aging the spherical nickel-cobalt-manganese precursor particles, and then washing the precursor material on a centrifugal machine or a filter press by pure water to obtain the spherical nickel-cobalt-manganese precursor material, wherein the concentration of sodium ions in the mother liquor is 40-50 g/L, the concentration of sodium ions in washing wastewater is 10-25 g/L, the mother liquor and the washing wastewater are not recycled, and the pure water is used for preparing alkali liquor and washing products.
A small amount of washed spherical nickel-cobalt-manganese precursor material is taken as a sample B, and the physicochemical performance index of the sample B is tested, and the test result is shown in Table 1.
Comparative example 2:
a preparation method of a spherical nickel-cobalt-manganese precursor material comprises the following specific steps:
(1) dissolving nickel chloride, cobalt chloride and manganese chloride into water according to the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese precursor material to be prepared to prepare a nickel-cobalt-manganese ion mixed solution, and controlling the total concentration of nickel, cobalt and manganese ions in the nickel-cobalt-manganese ion mixed solution to be 115 g/L;
(2) uniformly mixing the ammonia water solution and the sodium hydroxide water solution to prepare an alkali liquor with the ammonia concentration of 20 g/L; the method comprises the following steps of adding a nickel-cobalt-manganese ion mixed solution and an alkali liquor into a reaction kettle which is filled with a base solution and has good sealing performance to perform continuous coprecipitation reaction, continuously introducing nitrogen in the reaction process, controlling the pH value of a reaction solution to be 10.8-11.2, controlling the temperature to be 60 ℃, controlling the stirring speed to be 175r/min and controlling the ammonia concentration to be 15 g/L; the used base solution is a mixed solution of ammonia water and sodium hydroxide, wherein the ammonia concentration is 15g/L, the pH value is 10.9-11, and the temperature is 60 ℃; preparing slurry containing nickel, cobalt and manganese precursor particles, wherein the chemical molecular formula of the spherical nickel, cobalt and manganese precursor particles is Ni1-x-yCoxMny(OH)2Wherein 0.01 < x < 0.1, 0.01 < y < 0.1, for example Ni0.6Co0.2Mn0.2(OH)2；
(3) Carrying out solid-liquid separation on the slurry containing the nickel-cobalt-manganese precursor particles to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, then aging the spherical nickel-cobalt-manganese precursor particles, and then washing the precursor material on a centrifugal machine or a filter press by pure water to obtain a spherical nickel-cobalt-manganese precursor material, wherein the concentration of sodium ions in the mother liquor is 40-50 g/L, and the concentration of sodium ions in washing wastewater is 10-25 g/L;
(4) respectively collecting mother liquor obtained after solid-liquid separation and washing wastewater generated in the washing process, mixing the collected mother liquor with the washing wastewater to obtain a wastewater solution, adding pure water to dilute the sodium ion concentration in the wastewater solution to 30g/L, filtering the wastewater solution by using a fine filter to obtain reuse water, and returning the reuse water to the step (2) to be mixed with the ammonia water solution and the sodium hydroxide aqueous solution to be reused as alkali liquor.
After multiple cycles of reuse water, a small amount of washed spherical nickel-cobalt-manganese precursor material is taken as a sample C, and the physicochemical property indexes of the sample C are tested, and the test results are shown in Table 1.
Comparative example 3:
a preparation method of a spherical nickel-cobalt-manganese precursor material comprises the following specific steps:
(1) dissolving nickel chloride, cobalt chloride and manganese chloride into water according to the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese precursor material to be prepared to prepare a nickel-cobalt-manganese ion mixed solution, and controlling the total concentration of nickel, cobalt and manganese ions in the nickel-cobalt-manganese ion mixed solution to be 115 g/L;
(2) uniformly mixing the ammonia water solution and the sodium hydroxide water solution to prepare an alkali liquor with the ammonia concentration of 20 g/L; the method comprises the following steps of adding a nickel-cobalt-manganese ion mixed solution and an alkali liquor into a reaction kettle which is filled with a base solution and has good sealing performance to perform continuous coprecipitation reaction, continuously introducing nitrogen in the reaction process, controlling the pH value of a reaction solution to be 10.8-11.2, controlling the temperature to be 60 ℃, controlling the stirring speed to be 175r/min and controlling the ammonia concentration to be 15 g/L; the used base solution is a mixed solution of ammonia water and sodium hydroxide, wherein the ammonia concentration is 15g/L, the pH value is 10.9-11, and the temperature is 60 ℃; preparing slurry containing nickel, cobalt and manganese precursor particles, wherein the chemical molecular formula of the spherical nickel, cobalt and manganese precursor particles is Ni1-x-yCoxMny(OH)2Wherein 0.01 < x < 0.1, 0.01 < y < 0.1, for example Ni0.6Co0.2Mn0.2(OH)2；
(3) Carrying out solid-liquid separation on the slurry containing the nickel-cobalt-manganese precursor particles to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, then aging the spherical nickel-cobalt-manganese precursor particles, and then washing the precursor material on a centrifugal machine or a filter press by pure water to obtain a spherical nickel-cobalt-manganese precursor material, wherein the concentration of sodium ions in the mother liquor is 40-50 g/L, and the concentration of sodium ions in washing wastewater is 10-25 g/L;
(4) respectively collecting mother liquor obtained after solid-liquid separation and washing wastewater generated in the washing process, mixing the collected mother liquor with the washing wastewater to obtain a wastewater solution, adding pure water to dilute the sodium ion concentration in the wastewater solution to 25g/L, filtering the wastewater solution by using a fine filter to obtain reuse water, and returning the reuse water to the step (2) to be mixed with the ammonia water solution and the sodium hydroxide aqueous solution to be reused as alkali liquor.
After multiple cycles of reuse water, a small amount of washed spherical nickel-cobalt-manganese precursor material is taken as a sample D, and the physicochemical property indexes of the sample D are tested, and the test results are shown in Table 1.
TABLE 1 physicochemical indices of samples obtained in example 1 and comparative examples 1, 2 and 3
As can be seen from Table 1, when the sodium ion concentration of the reuse water is less than 25g/L (example 1, sample A), each index of the product is basically the same as that of the product prepared by pure water (comparative example 1, sample B), and the technical requirements can be met; when the concentration of sodium ions in the reuse water reaches 30g/L (comparative example 2, sample C), the crystallinity of the product is deteriorated, the density is low, the content of sodium and sulfur is increased, and the technical requirements of the product cannot be met.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. 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 (4)
1. A preparation method of a spherical nickel-cobalt-manganese precursor material comprises the following steps: preparing slurry containing spherical nickel-cobalt-manganese precursor particles by a coprecipitation method, performing solid-liquid separation on the slurry to obtain mother liquor and spherical nickel-cobalt-manganese precursor particles, aging the obtained spherical nickel-cobalt-manganese precursor particles, and then washing with water to obtain a spherical nickel-cobalt-manganese precursor material product, wherein the mother liquor obtained after the solid-liquid separation and washing wastewater generated in the washing process are respectively collected, then the collected mother liquor and the washing wastewater are mixed to obtain a wastewater solution, then pure water is supplemented to control the concentration of sodium ions in the wastewater solution to be less than 25g/L, then the wastewater solution is filtered by a fine filter to obtain reuse water, and the reuse water is returned to the coprecipitation method for preparing the spherical nickel-cobalt-manganese precursor particles to be reused as alkali liquor;
the concentration of sodium ions in the mother liquor is 40 g/L-80 g/L, and the concentration of sodium ions in the washing wastewater is 10 g/L-25 g/L;
the specific process for preparing the slurry containing the spherical nickel-cobalt-manganese precursor particles by the coprecipitation method comprises the following steps:
(1) preparing soluble salts of nickel, cobalt and manganese into a nickel-cobalt-manganese ion mixed solution according to the molar ratio of nickel, cobalt and manganese in the nickel-cobalt-manganese precursor, and controlling the total concentration of nickel, cobalt and manganese ions in the nickel-cobalt-manganese ion mixed solution to be 60-120 g/L;
(2) uniformly mixing the ammonia water solution and the sodium hydroxide water solution according to a certain volume ratio to obtain an alkali liquor with the ammonia concentration of 6-40 g/L;
(3) adding the obtained nickel-cobalt-manganese ion mixed solution and alkali liquor into a reaction kettle with a base solution in a parallel flow mode, wherein the base solution is an ammonia water and sodium hydroxide mixed solution with the ammonia concentration of 6 g/L-35 g/L, the pH of 10.3-11 and the temperature of 45-70 ℃, and continuously introducing nitrogen for protection before and during the reaction;
(4) and controlling the pH of the reaction solution to be 10.8-11.5, the temperature to be 45-70 ℃, the stirring speed to be 150-350 r/min and the ammonia concentration to be 6-35 g/L in the reaction, and carrying out continuous coprecipitation reaction to obtain the slurry containing spherical nickel-cobalt-manganese precursor particles.
2. The preparation method according to claim 1, wherein the recycling of the reuse water to the coprecipitation process for preparing the spherical nickel-cobalt-manganese precursor particles as an alkali solution is specifically:
in the step (2), the reuse water, the ammonia water solution and the sodium hydroxide water solution are uniformly mixed according to a certain volume ratio, and the alkali liquor with the ammonia concentration of 6-40 g/L is obtained.
3. The preparation method according to claim 1 or 2, characterized in that in the step (1), the soluble salt of nickel, cobalt and manganese specifically refers to sulfate, chloride or nitrate of nickel, cobalt and manganese.
4. The method of claim 1 or 2, wherein the spherical nickel cobalt manganese precursor material has a chemical formula of Ni1-x-yCoxMny(OH)2Wherein x is more than 0.01 and less than 0.1, and y is more than 0.01 and less than 0.1.
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| CN109256532B (en) * | 2018-03-27 | 2021-04-02 | 清远佳致新材料研究院有限公司 | Method for comprehensively utilizing mother liquor in synthesis process of ternary cathode material precursor of lithium ion battery |
| CN109279664A (en) * | 2018-11-19 | 2019-01-29 | 长沙矿冶研究院有限责任公司 | A kind of water-saving preparation method of tertiary cathode material hydroxide precursor and water-saving preparation system |
| WO2020171088A1 (en) * | 2019-02-21 | 2020-08-27 | 住友金属鉱山株式会社 | Method for producing positive electrode active material for lithium ion secondary batteries, positive electrode active material for lithium ion secondary batteries, and lithium ion secondary battery |
| CN109761288B (en) * | 2019-04-09 | 2019-07-12 | 金驰能源材料有限公司 | A kind of preparation method of spherical nickel cobalt manganese persursor material |
| CN110980818A (en) * | 2019-12-03 | 2020-04-10 | 河南电池研究院有限公司 | Preparation method of lithium-rich manganese-based precursor and positive electrode material, precursor and material |
| CN113213552A (en) * | 2021-03-20 | 2021-08-06 | 长沙理工大学 | Quasi-spherical porous nickel-cobalt-manganese precursor and preparation method thereof |
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