CN114906887A - Nickel-cobalt-aluminum hydroxide and preparation method and application thereof - Google Patents
Nickel-cobalt-aluminum hydroxide and preparation method and application thereof Download PDFInfo
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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Abstract
The invention provides a nickel-cobalt-aluminum hydroxide and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) mixing a nickel source, a cobalt source, an aluminum source and a solvent to obtain a ternary solution, simultaneously injecting the ternary solution, an inorganic strong alkali solution and an ammonia-free complexing agent solution into a stirrer for stirring, and controlling the pH value, wherein the molar ratio of a ternary solution solute to an inorganic strong alkali solute to an ammonia-free complexing agent solute is 1 (2-2.2) to (0.02-0.13), so as to obtain a reaction solution; (2) the method can realize uniform coprecipitation of nickel, cobalt and aluminum by strictly controlling the feeding speed and the raw material concentration in the reaction liquid and further controlling the proportion of each component in cooperation with pH regulation and ammonia-free complexing agent selection, avoids the problem of element proportion imbalance caused by separate feeding, is not suitable for using ammonia water as a chelating agent, and is environment-friendly.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to nickel-cobalt-aluminum hydroxide, and a preparation method and application thereof.
Background
With the development of new energy industry, the lithium battery field is concerned. As one of the core components of lithium ion batteries, a positive electrode material has been continuously searched and developed as LiNiO 2 The basic Nickel Cobalt Manganese (NCM) and Nickel Cobalt Aluminum (NCA) ternary materials are now widely used.
At present, the NCA ternary material can be synthesized by various methods such as a sol-gel synthesis method, a solution combustion route, a spray pyrolysis method, a coprecipitation method, and the like. Coprecipitation is the most commonly used method in view of its ability to produce target materials with uniform element distribution, uniform spherical morphology, and high tap at the atomic level. The NCA ternary material is prepared by preparing NiCoAl (OH) 2 The precursor is then further mixed with lithium and sintered to obtain the NiCoAl (OH) 2 In the precursor process, Ni is added in a typical coprecipitation route 2+ 、Co 2+ And Al 3+ The salt solution is pumped into the reactor and thenA strong base solution and a solution of a chelating agent are simultaneously added to the reactor at a controlled rate, the chelating agent serving to slow the reaction and help form the spherical morphology of the product. When ammonia is used as the chelating agent, aluminum is hardly directly complexed, and at the same time, Al 3+ Ksp of the hydroxide is much smaller than that of Ni 2+ And Co 2+ Therefore, the three are difficult to realize uniform coprecipitation, which also directly affects the quality of the product.
CN103296263A separates the deposit of nickel cobalt and aluminium through forming the alcosol earlier, has avoided the influence to precursor appearance and homogeneity when three kinds of elements coprecipitate, but, the preparation of alcosol has increased the reaction process, has increased manufacturing cost, and the part feeding also leads to the element proportion to be maladjusted easily, needs adjustment flow in good time and monitors.
CN104425815A adopts more than two mixed complexing agents to perform complexing on an aluminum salt solution in advance, then the aluminum complexing solution, a nickel-cobalt-containing solution and a precipitator are respectively added into a reactor at a certain flow rate to perform reaction, the mode of obtaining the aluminum complexing solution in advance improves the formation of Al (OH) in an aqueous solution by aluminum ions 3 Obviously faster than nickel cobalt ions, and further obtain the precursor material with uniformly dispersed elements. However, the addition of multiple complexing agents and the pre-complexing method increase the operation procedure and cost, and the separate feeding may also cause the proportion to be out of order, so that the feeding flow needs to be controlled.
In the method of the scheme, the pretreatment of the aluminum solution increases the operation reaction process and cost, the separate feeding of aluminum and nickel and cobalt easily causes element proportion imbalance, and the flow monitoring needs to be adjusted timely; the reaction process still uses ammonia water as a chelating agent, is not environment-friendly and is not beneficial to the coprecipitation reaction of nickel, cobalt and aluminum.
Disclosure of Invention
The invention aims to provide a nickel-cobalt-aluminum hydroxide and a preparation method and application thereof, wherein the proportion of each component is controlled by strictly controlling the feeding speed and the concentration of raw materials in a reaction solution, and the uniform coprecipitation of nickel, cobalt and aluminum can be realized by matching with the regulation and control of pH and the selection of ammonia-free complexing agent, so that the problem of element proportion imbalance caused by separate feeding is avoided, and ammonia water is not suitable for being used as a chelating agent and is environment-friendly.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing nickel cobalt aluminum hydroxide, comprising the steps of:
(1) mixing a nickel source, a cobalt source, an aluminum source and a solvent to obtain a ternary solution, simultaneously injecting the ternary solution, an inorganic strong base solution and a complexing agent solution into a stirrer for stirring, controlling the pH value, and controlling the molar ratio of a ternary solution solute, an inorganic strong base solution solute and a complexing agent solution solute in the stirrer to be 1 (2-2.2) to (0.02-0.2), for example: 1:2:0.02, 1:2.05:0.08, 1:2:0.1, 1:2.1:0.12 or 1:2.2:0.2 and the like to obtain a reaction solution;
(2) carrying out centrifugal treatment on the reaction liquid obtained in the step (1) to obtain the nickel cobalt aluminum hydroxide;
wherein, the solute in the complexing agent solution in the step (1) is an ammonia-free complexing agent.
The invention realizes the uniform coprecipitation of nickel, cobalt and aluminum by strictly controlling the proportion of each component solution and the pH value of a reaction system, adopts an ammonia-free system complexing agent, eliminates the use of ammonia water, and is environment-friendly; the method avoids a separate feeding mode of nickel, cobalt and aluminum, reduces redundant working procedures, reduces cost, and can effectively stabilize the element proportion of nickel, cobalt and aluminum; the original mature ammonia water coprecipitation process can be adopted, the process improvement is reduced, and the cost is reduced.
Preferably, the nickel source in step (1) comprises any one of nickel sulfate, nickel nitrate or nickel chloride or a combination of at least two of them.
Preferably, the cobalt source comprises any one of cobalt sulfate, cobalt nitrate or cobalt chloride or a combination of at least two thereof.
Preferably, the aluminium source comprises any one of aluminium sulphate, aluminium nitrate or aluminium chloride, or a combination of at least two thereof.
Preferably, the molar ratio of the nickel element in the nickel source, the cobalt element in the cobalt source and the aluminum element in the aluminum source is 0.9 (0.08-0.1) to (0-0.02).
Preferably, the molar concentration of the solute in the ternary solution in the step (1) is 0.5-1.5 mol/L, such as: 0.5mol/L, 0.8mol/L, 1mol/L, 1.2mol/L, 1.5mol/L, etc.
Preferably, the solute of the inorganic strong alkali solution in the step (1) comprises sodium hydroxide and/or potassium hydroxide.
Preferably, the molar concentration of the solute in the inorganic strong alkali solution is 6-9 mol/L, such as: 6mol/L, 7mol/L, 8mol/L or 9mol/L, etc.
Preferably, the ammonia-free complexing agent comprises any one of sulfosalicylic acid, oxalic acid, salicylic acid, or acetylacetone, or a combination of at least two thereof.
Preferably, the ammonia-free complexing agent has a molar concentration of 0.1 to 0.5mol/L, such as: 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, etc.
Preferably, the pH value in the step (1) is controlled to be 10-13, such as: 10. 10.5, 11, 12 or 13, etc.
Preferably, the injection into the agitator is accompanied by agitation;
preferably, the stirring speed is 200-400 rpm, such as: 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, or the like.
Preferably, the reaction temperature of the reaction solution is 40-70 ℃, for example: 40 deg.C, 45 deg.C, 50 deg.C, 60 deg.C or 70 deg.C, etc.
Preferably, the separation treatment in step (2) comprises centrifuging the reaction solution in a centrifuge, and washing with hot water and liquid alkali.
Preferably, the centrifugation treatment is followed by a drying treatment.
Preferably, the temperature of the drying treatment is 100-160 ℃, for example: 100 ℃, 110 ℃, 120 ℃, 150 ℃, 160 ℃ or the like.
In a second aspect, the present invention provides a nickel cobalt aluminium hydroxide, prepared by a process as described in the first aspect.
In a third aspect, the invention provides a ternary nickel-cobalt-aluminum cathode material, which is prepared from the nickel-cobalt-aluminum hydroxide in the second aspect.
In a fourth aspect, the invention provides a positive electrode plate, wherein the positive electrode plate comprises the ternary nickel-cobalt-aluminum positive electrode material according to the third aspect.
In a fifth aspect, the invention provides a lithium ion battery, which comprises the positive electrode plate according to the fourth aspect.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the proportion of each component is controlled by strictly controlling the feeding speed and the concentration of the raw materials in the reaction liquid, and the uniform coprecipitation of nickel, cobalt and aluminum can be realized by matching with the regulation of pH and the selection of an ammonia-free complexing agent, so that the problem of element proportion imbalance caused by separate feeding is avoided, and the method is not suitable for using ammonia water as a chelating agent and is environment-friendly.
Drawings
FIG. 1 is an XRD pattern of nickel cobalt aluminum hydroxide obtained in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
This embodiment provides a nickel cobalt aluminum hydroxide, and a preparation method of the nickel cobalt aluminum hydroxide is as follows:
(1) preparing 0.5mol/L ternary solution (sulfate) with the molar ratio of Ni, Co and Al being 0.9:0.1:0.1, controlling the flow rates of the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution to be 10L/h, 1.8L/h and 1L/h, injecting the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution into a stirrer, stirring at the speed of 360rpm, at the temperature of 50 ℃ and at the pH value of 11, and obtaining reaction liquid;
(2) and (3) pumping the reaction solution into a centrifuge, washing by using hot water and liquid alkali, and drying filter residues obtained by centrifugal washing in an oven at 150 ℃ to finally obtain the nickel-cobalt-aluminum hydroxide.
The XRD pattern of the nickel cobalt aluminum hydroxide is shown in fig. 1.
Example 2
This example provides a nickel cobalt aluminum hydroxide, and the preparation method of the nickel cobalt aluminum hydroxide is as follows:
(1) preparing 1mol/L ternary solution (sulfate) with the molar ratio of Ni, Co and Al being 0.9:0.1:0.1, controlling the flow rates of the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution to be 32L/h, 8L/h and 13L/h, injecting the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution into a stirrer, stirring at the speed of 240rpm, the temperature of 70 ℃ and the pH being 10.6 to obtain reaction liquid, wherein the concentration of the sodium hydroxide solution is 8mol/L and the concentration of the sulfosalicylic acid solution is about 0.3 mol/L;
(2) and (3) pumping the reaction solution into a centrifuge, washing by using hot water and liquid alkali, and drying filter residues obtained by centrifugal washing in an oven at 100 ℃ to finally obtain the nickel-cobalt-aluminum hydroxide.
Example 3
This example provides a nickel cobalt aluminum hydroxide, and the preparation method of the nickel cobalt aluminum hydroxide is as follows:
(1) preparing 1.5mol/L ternary solution (sulfate) with the molar ratio of Ni, Co and Al being 0.9:0.1:0.1, controlling the flow rates of the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution to be 6L/h, 1.6L/h and 1.8L/h, injecting the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution into a stirrer, stirring at the speed of 380rpm, the temperature of 60 ℃ and the pH value being 12 to obtain reaction liquid;
(2) and (3) pumping the reaction solution into a centrifuge, washing by using hot water and liquid alkali, and drying filter residues obtained by centrifugal washing in an oven at 150 ℃ to finally obtain the nickel-cobalt-aluminum hydroxide.
Example 4
The difference between this embodiment and embodiment 1 is only that, the temperature in step (1) is 30 ℃, other conditions and parameters are completely the same as those in embodiment 1, and when the reaction temperature is too low, the co-precipitation reaction rate is slowed, and the growth of hydroxide precursor particles is affected.
Example 5
The difference between this example and example 1 is that the temperature in step (1) is 80 ℃, the other conditions and parameters are the same as those in example 1, and the nickel-cobalt-aluminum hydroxide is prepared, and the reaction temperature is too high, which causes the fluctuation of pH value, and further causes the deterioration of the quality of the hydroxide precursor.
Example 6
The difference between this example and example 1 is only that, in step (1), the pH is 9.5, and other conditions and parameters are completely the same as those in example 1, so that the nickel-cobalt-aluminum hydroxide is prepared, and during the reaction, the pH is too low to facilitate the formation of hydroxide precursor crystal nuclei, which may affect the morphology of primary particles, and the primary particles may be thick.
Example 7
The difference between this example and example 1 is that, in step (1), the pH is 13.5, and other conditions and parameters are the same as those in example 1, so that nickel-cobalt-aluminum hydroxide is prepared, and when the reaction pH is too high, the growth of particles is not facilitated, a large number of crystal nuclei are generated, the particles are very fine, and for a nickel-cobalt-aluminum reaction system, the precipitation of aluminum is dissolved back.
Comparative example 1
The difference between the comparative example and the example 1 is that the flow rates of the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution are 10L/h, 3L/h and 0.5L/h, other conditions and parameters are completely the same as those of the example 1, the nickel-cobalt-aluminum hydroxide is prepared, the growth and the particle morphology of the hydroxide precursor can be influenced by reducing the addition of the sulfosalicylic acid complexing agent under the condition of a certain ternary-liquid-alkali ratio, and the precursor morphology is usually loose under the low complexing state.
Comparative example 2
The difference between the comparative example and the example 1 is that the flow rates of the ternary solution, the sodium hydroxide solution and the sulfosalicylic acid solution are 10L/h, 3L/h and 5L/h, other conditions and parameters are completely the same as those of the example 1, and the nickel-cobalt-aluminum hydroxide is prepared.
As can be seen from comparison of examples 1 to 5, in the preparation process of the nickel-cobalt-aluminum hydroxide, the reaction temperature affects the quality of the prepared nickel-cobalt-aluminum hydroxide, the reaction temperature is controlled to be 40-70 ℃, the quality of the prepared nickel-cobalt-aluminum hydroxide is high, and if the reaction temperature is too low, the growth of precursor particles is not facilitated, and the reaction efficiency is reduced; if the temperature of the reaction is too high, the energy consumption for maintaining the high temperature is increased, and the too high temperature is also limited for promoting the growth of particles, but the too high temperature can cause the fluctuation of pH, so that the quality of the precursor is deteriorated.
As can be seen from comparison between the embodiment 1 and the embodiments 6 to 7, in the preparation process of the nickel-cobalt-aluminum hydroxide, the pH can influence the quality of the prepared nickel-cobalt-aluminum hydroxide, the pH is controlled to be 10-13, the quality of the prepared nickel-cobalt-aluminum hydroxide is high, if the pH is too low, the generation of crystal nuclei is inhibited, the particle growth is thicker and larger, and the sphericity of the obtained precursor is poorer; if the pH is too high, the aluminum precipitate will be dissolved back, resulting in the imbalance of the metal element ratio of Ni-Co-Al hydroxide.
Compared with the comparative examples 1 and 2, the method has the advantages that the feeding speed and the raw material concentration in the reaction liquid are strictly controlled to further control the proportion of each component, the uniform coprecipitation of the nickel, the cobalt and the aluminum can be realized by matching with the regulation and control of pH and the selection of the ammonia-free complexing agent, the problem of element proportion imbalance caused by separate feeding is avoided, and the method does not use ammonia water as a chelating agent and is environment-friendly.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of nickel cobalt aluminum hydroxide is characterized by comprising the following steps:
(1) mixing a nickel source, a cobalt source, an aluminum source and a solvent to obtain a ternary solution, simultaneously injecting the ternary solution, an inorganic strong base solution and a complexing agent solution into a stirrer, controlling the pH value, and controlling the molar ratio of a ternary solution solute to an inorganic strong base solution solute to a complexing agent solution solute in the stirrer to be 1 (2-2.2) to (0.02-0.2) to obtain a reaction solution;
(2) separating the reaction liquid obtained in the step (1) to obtain the nickel cobalt aluminum hydroxide;
wherein, the solute in the complexing agent solution in the step (1) is an ammonia-free complexing agent.
2. The method of claim 1, wherein the nickel source of step (1) comprises any one of nickel sulfate, nickel nitrate, or nickel chloride, or a combination of at least two thereof;
preferably, the cobalt source comprises any one of cobalt sulfate, cobalt nitrate or cobalt chloride or a combination of at least two thereof;
preferably, the aluminium source comprises any one of aluminium sulphate, aluminium nitrate or aluminium chloride, or a combination of at least two thereof;
preferably, the molar ratio of the nickel element in the nickel source, the cobalt element in the cobalt source and the aluminum element in the aluminum source is 0.9 (0.08-0.1) to (0-0.02);
preferably, the molar concentration of the solute in the ternary solution in the step (1) is 0.5-1.5 mol/L.
3. The method of claim 1 or 2, wherein the solute of the inorganic strong alkali solution of step (1) comprises sodium hydroxide and/or potassium hydroxide;
preferably, the molar concentration of the solute in the inorganic alkali solution is 6-9 mol/L.
4. The process according to any one of claims 1 to 3, wherein the ammonia-free complexing agent comprises any one of sulfosalicylic acid, oxalic acid, salicylic acid, or acetylacetone or a combination of at least two thereof;
preferably, the molar concentration of the solute in the ammonia-free complexing agent is 0.1-0.5 mol/L.
5. The method according to any one of claims 1 to 4, wherein the pH is controlled to 10 to 13 in the step (1);
preferably, the injection into the agitator is accompanied by agitation;
preferably, the stirring speed is 200-400 rpm;
preferably, the reaction temperature of the reaction solution is 40-70 ℃.
6. The method according to any one of claims 1 to 5, wherein the separation treatment in the step (2) comprises subjecting the reaction solution to a centrifugation treatment by feeding the reaction solution into a centrifuge, and washing the reaction solution with hot water and a liquid alkali;
preferably, the drying treatment is carried out after the centrifugation treatment;
preferably, the temperature of the drying treatment is 100-160 ℃.
7. A nickel cobalt aluminium hydroxide, wherein the nickel cobalt aluminium hydroxide is obtainable by a process according to any one of claims 1 to 6.
8. A ternary nickel-cobalt-aluminum cathode material, characterized in that it is prepared from the nickel-cobalt-aluminum hydroxide according to claim 7.
9. A positive electrode plate, characterized in that the positive electrode plate comprises the ternary nickel-cobalt-aluminum positive electrode material as claimed in claim 8.
10. A lithium ion battery comprising the positive electrode sheet of claim 9.
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| CN115818733A (en) * | 2022-11-18 | 2023-03-21 | 荆门市格林美新材料有限公司 | Zirconium-doped uniform nickel-manganese hydroxide and preparation method and application thereof |
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