CN113184919A - Preparation method of aluminum-doped cobaltosic oxide - Google Patents
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Abstract
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of aluminum-doped cobaltosic oxide, which prepares a uniform aluminum-doped cobalt hydroxide product by adding alkaline nano aluminum sol in a cocurrent flow manner in the preparation process of cobalt hydroxide; and then washing, drying and calcining the uniform aluminum-doped cobalt hydroxide product to obtain an aluminum-doped cobaltosic oxide product. By utilizing the process, the laser granularity D can be prepared5016-18 mu m, 0.4-0.8% of aluminum doping amount and tap density ≧ 2.0g/cm3The specific surface area is 1.0-3.0 m2The aluminum-doped cobaltosic oxide product has the shape of block or sphere-like. The aluminum in the aluminum-doped cobaltosic oxide product prepared by the invention is uniformly distributed, and the charge and discharge voltage of the lithium cobaltite product is favorably improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of aluminum-doped cobaltosic oxide.
Background
The lithium ion battery prepared by taking lithium cobaltate as the anode material has the characteristics of light weight, large capacity, high specific energy, high working voltage, stable discharge, suitability for large-current discharge, good cycle performance, long service life and the like, and is mainly applied to the field of 3C digital codes.
Lithium cobaltate is developing towards high voltage, high compaction and high cycle performance, and the requirement on the raw material cobaltosic oxide is higher and higher. Co3O4Is a functional material with special structure and performance, and the aluminum-doped cobaltosic oxide product can improve the charging voltage and the cycle performance of lithium cobaltate, so the aluminum-doped Co3O4The market demand is gradually highlighted. It has become a focus of research on how to prepare aluminum-doped cobaltosic oxide.
The Chinese invention patent CN201810455841.X discloses a preparation method of large-particle-size aluminum-doped cobaltosic oxide, which specifically comprises the steps of adopting a continuous production method, carrying out neutralization and precipitation reaction while separating supernatant liquid without materials to obtain cobalt carbonate seed crystals containing aluminum and having a particle size D50 of 10-14.5 mu m, continuously adding an aluminum cobalt solution and an ammonium bicarbonate solution into the seed crystals to carry out neutralization and precipitation reaction until large-particle-size aluminum-doped cobalt carbonate with a particle size D50 of 18-21 mu m is obtained, removing iron, dehydrating, washing, drying, and carrying out sectional thermal decomposition to obtain a black powdery aluminum-doped cobalt oxide product with a particle size D50 of 17.5-19 mu m; chinese patent CN201711217367.9 discloses a method for preparing large-particle-size uniformly-doped aluminum cobaltosic oxide, which adopts a wet method to synthesize large-particle-size aluminum-doped cobalt carbonate, sets parameters in principle aiming at the problem of aluminum-doping uniformity of a cobalt carbonate system, prevents aluminum compounds from being separated out and aggregated independently, and enables doped Al elements to be uniformly distributed in the cobaltosic oxide, the particle size reaches more than 15 mu m, and the particle size distribution is uniform. The above patents all adopt the preparation of aluminum-doped cobaltosic oxide products by firstly synthesizing aluminum-doped cobalt carbonate and then calcining, which is obviously different from the present patent.
Disclosure of Invention
The invention aims to provide a preparation method of aluminum-doped cobaltosic oxide, which aims to solve the problems of long reaction time, complicated process and difficulty in preparing the aluminum-doped cobaltosic oxide with uniformly distributed aluminum in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of aluminum-doped cobaltosic oxide is characterized by comprising the following specific steps:
taking cobalt salt as a raw material, and preparing a cobalt solution with the cobalt concentration of 90-110 g/L as an A solution; preparing a sodium hydroxide solution of 200-300 g/L as a B solution; preparing 90g/L ammonia water solution as solution C, wherein 5-10 mL of hydrazine hydrate solution with the mass concentration of 80% is added into each liter of ammonia water solution; diluting the aluminum sol with pH value of 7-9 and particle size of 5-15 nm with pure water until the aluminum content is 4-8 g/L, wherein the diluted aluminum sol solution is solution D.
And (2) preparing the aluminum-doped cobalt hydroxide in a reaction kettle. At the beginning of the synthesis reaction, A, B, C, D solution is added into the reaction kettle in parallel flow, and the preparation of aluminum-doped cobalt hydroxide is carried out under the stirring condition. When the volume of the slurry in the reaction kettle reaches a certain value, the precision filter is started, the slurry pump pumps the slurry in the reaction kettle into the precision filter for concentration, the concentrated slurry returns to the reaction kettle for continuous synthesis, and the liquid level of the reaction kettle is kept on a determined scale by adjusting the amount of the discharged mother liquor. The solution flow rate, reaction pH value, reaction temperature, stirring intensity and reaction time of A, B, C, D are strictly controlled in the reaction process.
And (3) closing the precision filter of the reaction kettle and starting aging after the synthesis reaction is finished. And after aging, filtering, washing and drying the synthesized product to obtain the aluminum-doped cobalt hydroxide product.
And (4) calcining the aluminum-doped cobalt hydroxide obtained in the step (3) to obtain an aluminum-doped cobaltosic oxide product.
Preferably, in the step (1), the cobalt salt is one of cobalt sulfate, cobalt nitrate and cobalt chloride.
Preferably, in the step (2), the reaction kettle is 10m3And when the volume of the slurry in the reaction kettle reaches a certain value, starting the precision filter until the volume of the slurry in the reaction kettle reaches 80-85% of the volume of the reaction kettle, and adjusting the amount of the discharged mother liquor to keep the liquid level of the reaction kettle on a liquid level scale where the determined scale is 80-85% of the volume of the reaction kettle. In the reaction process, the flow rate of A, B, C, D solution, the reaction pH value, the reaction temperature, the stirring intensity and the reaction time A solution is strictly controlled to be 400L/h, the flow rate of C solution is 70L/h, the flow rate of D sol solution is 50-60L/h, the flow rate of B solution is adjusted according to the reaction pH value, the reaction pH value is 8.4-8.8, the reaction temperature is 74-76 ℃, the stirring intensity is 140-160 r/min, and the reaction time is 40-50 h.
Preferably, in the step (3), the aging time is 1-2 hours, the washing is performed by using a centrifuge, the washing material is deionized water at 80-90 ℃, the material drying equipment is a disc type dryer, and the drying temperature is 200-300 ℃.
Preferably, in the step (4), the calcining condition is roller kiln calcining, the calcining temperature is 700-750 ℃, and the calcining time is 4-6 h.
Preferably, in the step (4), the physical and chemical indexes of the aluminum-doped cobaltosic oxide product include: laser particle size D5016-18 mu m, 0.4-0.8% of aluminum doping amount and not less than 2.0g/cm of tap density3The specific surface area is 1.0-3.0 m2The shape is blocky or sphere-like.
Compared with the prior art, the invention has the beneficial effects that:
due to Co (OH)2Has a Ksp of 1.6X 10-15，Al(OH)3Has a Ksp of 3.0X 10-34Under the condition of the same temperature and pH value, the precipitation speed of the aluminum hydroxide is far greater than that of the cobalt hydroxide, and the cobalt-aluminum solution coprecipitation method is not easy to usePreparing the uniform aluminum-doped cobalt hydroxide. The invention adopts alkaline aluminum sol as aluminum dopant, and prepares the uniform aluminum-doped cobalt hydroxide by the slow peptization of the alkaline aluminum sol under the cobalt hydroxide synthesis condition. After the synthesis is finished, the synthesized product is washed, dried and calcined to obtain the aluminum-doped cobaltosic oxide product, and aluminum in the aluminum-doped cobaltosic oxide product is uniformly distributed, so that the charging and discharging voltage of the lithium cobaltite product is favorably improved.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a SEM test result of the aluminum-doped cobaltosic oxide product prepared in example 1;
FIG. 3 is the SEM test result of the aluminum-doped cobaltosic oxide product prepared in example 2;
FIG. 4 is the SEM test result of the aluminum-doped cobaltosic oxide product prepared in example 3.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-4, an embodiment of the present invention is shown:
example one
The production steps are the same as above and are not described herein again. The specific parameters in each step are as follows:
the prepared solution A is 90g/L cobalt chloride solution; the prepared solution B is 200g/L of sodium hydroxide solution; the prepared solution C is 90g/L ammonia water solution, wherein 5mL of hydrazine hydrate solution with the mass concentration of 80% is added in each liter of ammonia water solution; the prepared solution D is an alkaline aluminum sol solution with the aluminum content of 4 g/L.
At 10m3The aluminum-doped cobalt hydroxide is prepared in the reaction kettle. When the synthesis reaction starts, the solution A is 400L/h, the solution C is 70L/h, and the aluminum sol solution D is 50L/hAnd adding the solution B into the reaction kettle in a concurrent flow manner, and synthesizing the aluminum-doped cobalt hydroxide under the stirring condition. When the volume of the slurry in the reaction kettle reaches 80% of the volume of the reaction kettle, the precision filter is started, the slurry in the reaction kettle is pumped into the precision filter by a pump for concentration, the concentrated slurry is returned to the reaction kettle for continuous synthesis, and the slurry liquid level in the reaction kettle is kept on the scale of 80% by adjusting the amount of the discharged mother liquid. The pH value of the reaction is strictly controlled to be 8.8 in the reaction process, the reaction temperature is 74 ℃, the stirring intensity is 160 r/min, and the reaction time is 50 h.
After the reaction is finished, the precision filter of the reaction kettle is closed, and the aging is started. And aging for 1h, filtering and washing the synthesized product by using a centrifugal machine, wherein the washing material adopts 80 ℃ deionized water, the drying material equipment is a disc type dryer, and the drying temperature is 200 ℃, so that the homogeneous aluminum-doped cobalt hydroxide product is obtained.
And calcining the obtained homogeneous aluminum-doped cobalt hydroxide on a roller kiln at the calcining temperature of 700 ℃ for 6 hours. And obtaining the aluminum-doped cobaltosic oxide product.
The partial physicochemical indices of example 1 are given in the following table:
| Co（%） | Al（%） | D10(μm) | D50(μm) | D90(μm) | Cl-（%） | TD(g/cm3) | BET(m2/g) |
| 72.77 | 0.41 | 11.3 | 17.5 | 26.8 | 0.008 | 2.34 | 1.79 |
the micro-morphology index of the prepared product is shown in figure 2.
Example two
The production steps are the same as above and are not described herein again. The specific parameters in each step are as follows:
the prepared solution A is 100g/L cobalt sulfate solution; the prepared solution B is 250g/L sodium hydroxide solution; the prepared solution C is 90g/L ammonia water solution, wherein 8mL of hydrazine hydrate solution with the mass concentration of 80% is added in each liter of ammonia water solution; the prepared solution D is an alkaline aluminum sol solution with the aluminum content of 6 g/L.
At 10m3The aluminum-doped cobalt hydroxide is prepared in the reaction kettle. When the synthesis reaction starts, adding the solution A into the reaction kettle at a flow rate of 400L/h, the solution C at a flow rate of 70L/h and the solution D at a flow rate of 55L/h in parallel with the solution B, and carrying out aluminum-doped cobalt hydroxide synthesis under stirring. When the volume of the slurry in the reaction kettle reaches 85% of the volume of the reaction kettle, the precision filter is started, the slurry in the reaction kettle is pumped into the precision filter by a pump for concentration, the concentrated slurry is returned to the reaction kettle for continuous synthesis, and the slurry liquid level in the reaction kettle is kept on the scale of 85% by adjusting the amount of the discharged mother liquor. In the reaction process, the pH value of the reaction is strictly controlled to be 8.6, the reaction temperature is 75 ℃, the stirring intensity is 150 r/min, and the reaction time is 45 h.
After the reaction is finished, the precision filter of the reaction kettle is closed, and the aging is started. And aging for 1.5h, filtering and washing the synthesized product by using a centrifugal machine, wherein deionized water with the temperature of 85 ℃ is adopted as a washing material, a disc type drier is adopted as a material drying device, and the drying temperature is 250 ℃, so that the homogeneous aluminum-doped cobalt hydroxide product is obtained.
And calcining the obtained homogeneous aluminum-doped cobalt hydroxide on a roller kiln at the temperature of 720 ℃ for 5 hours. And obtaining the aluminum-doped cobaltosic oxide product.
The partial physicochemical indices of example 2 are given in the following table:
the micro-morphology index of the prepared product is shown in figure 3.
EXAMPLE III
The production steps are the same as above and are not described herein again. The specific parameters in each step are as follows:
the prepared solution A is a cobalt nitrate solution with the concentration of 110 g/L; the prepared solution B is 300g/L of sodium hydroxide solution; the prepared solution C is 90g/L ammonia water solution, wherein 10mL of hydrazine hydrate solution with the mass concentration of 80% is added in each liter of ammonia water solution; the prepared solution D is alkaline aluminum sol solution with the aluminum content of 8 g/L.
At 10m3The aluminum-doped cobalt hydroxide is prepared in the reaction kettle. When the synthesis reaction starts, adding the solution A into the reaction kettle at a flow rate of 400L/h, the solution C at a flow rate of 70L/h and the solution D at a flow rate of 60L/h in parallel with the solution B, and carrying out aluminum-doped cobalt hydroxide synthesis under stirring. When the volume of the slurry in the reaction kettle reaches 85% of the volume of the reaction kettle, the precision filter is started, the slurry in the reaction kettle is pumped into the precision filter by a pump for concentration, the concentrated slurry is returned to the reaction kettle for continuous synthesis, and the slurry liquid level in the reaction kettle is kept on the scale of 85% by adjusting the amount of the discharged mother liquor. In the reaction process, the pH value of the reaction is strictly controlled to be 8.4, the reaction temperature is 76 ℃, the stirring intensity is 140 r/min, and the reaction time is 40 h.
After the reaction is finished, the precision filter of the reaction kettle is closed, and the aging is started. And aging for 2h, filtering and washing the synthesized product by using a centrifugal machine, wherein deionized water with the temperature of 90 ℃ is adopted as a washing material, a disc type drier is adopted as a material drying device, and the drying temperature is 300 ℃ to obtain a homogeneous aluminum-doped cobalt hydroxide product.
And calcining the obtained homogeneous aluminum-doped cobalt hydroxide on a roller kiln at the temperature of 740 ℃ for 4 hours. And obtaining the aluminum-doped cobaltosic oxide product.
The physicochemical indexes of the product part of example 3 are as follows in Table 2:
| Co（%） | Na+（%） | D10(μm) | D50(μm) | D90(μm) | Al（%） | TD(g/cm3) | BET(m2/g) |
| 72.29 | ≤0.002 | 11.2 | 17.4 | 26.6 | 0.79 | 2.28 | 1.97 |
the micro-morphology index of the prepared product is shown in figure 4.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. A preparation method of aluminum-doped cobaltosic oxide is characterized by comprising the following specific steps:
taking cobalt salt as a raw material, and preparing a cobalt solution with the cobalt concentration of 90-110 g/L as an A solution; preparing a sodium hydroxide solution of 200-300 g/L as a B solution; preparing 90g/L ammonia water solution as solution C, wherein 5-10 ml of hydrazine hydrate solution with the mass concentration of 80% is added into each liter of ammonia water solution; diluting the aluminum sol with the pH value of 7-9 and the particle size of 5-15 nm by pure water until the aluminum content is 4-8 g/L, wherein the diluted aluminum sol solution is solution D;
preparing aluminum-doped cobalt hydroxide in a reaction kettle, adding A, B, C, D solution into the reaction kettle in a parallel flow mode when a synthesis reaction starts, preparing the aluminum-doped cobalt hydroxide under a stirring condition, starting a precision filter when the volume of slurry in the reaction kettle reaches a certain value, pumping the slurry in the reaction kettle into the precision filter by using a slurry pump for concentration, returning concentrated slurry to the reaction kettle for continuous synthesis, keeping the liquid level of the reaction kettle on a determined scale by adjusting the amount of discharged mother liquor, and strictly controlling A, B, C, D solution flow, reaction pH value, reaction temperature, stirring intensity and reaction time in the reaction process;
step (3) after the synthesis reaction is finished, closing a precision filter of the reaction kettle, starting aging, and after aging is finished, filtering, washing and drying the synthesized product to obtain an aluminum-doped cobalt hydroxide product;
and (4) calcining the aluminum-doped cobalt hydroxide obtained in the step (3) to obtain an aluminum-doped cobaltosic oxide product.
2. The method for preparing aluminum-doped cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step (1), the cobalt salt is one of cobalt sulfate, cobalt nitrate or cobalt chloride.
3. The method for preparing aluminum-doped cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step (2), the reaction kettle is 10m3When the volume of the slurry in the reaction kettle reaches a certain value, starting a certain value in the precision filter to be a liquid level scale where the volume of the slurry in the reaction kettle reaches 80% -85% of the volume of the reaction kettle, and keeping the liquid level of the reaction kettle on the determined scale where the volume of the reaction kettle is 80% -85% of the volume of the reaction kettle by adjusting the amount of the drained mother liquid, wherein the flow rate of A, B, C, D solution, the reaction pH value, the reaction temperature, the stirring strength and the reaction time of the solution A are strictly controlled to be 400L/h, the flow rate of the solution C is 70L/h, the flow rate of the solution D of alumina sol is 50-60L/h, the flow rate of the solution B is adjusted according to the reaction pH value, the reaction pH value is 8.4-8.8, the reaction temperature is 74-76 ℃, the stirring strength is 140-160 r/min, and the reaction time is 40-50 h.
4. The method for preparing aluminum-doped cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step (3), the aging time is 1-2 h, the washing is performed by using a centrifuge, the washing material is deionized water at 80-90 ℃, the material drying equipment is a disc type dryer, and the drying temperature is 200-300 ℃.
5. The method for preparing aluminum-doped cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step (4), the calcining condition is roller kiln calcining, the calcining temperature is 700-750 ℃, and the calcining time is 4-6 h.
6. The method for preparing aluminum-doped cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step (4), the physicochemical indexes of the aluminum-doped cobaltosic oxide product comprise: laser particle size D5016-18 mu m, 0.4-0.8% of aluminum doping amount and not less than 2.0g/cm of tap density3The specific surface area is 1.0-3.0 m2The shape is blocky or sphere-like.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113735183A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of aluminum-doped cobaltosic oxide |
| CN114906878A (en) * | 2022-04-07 | 2022-08-16 | 浙江格派钴业新材料有限公司 | Preparation method of battery-grade cobalt hydroxide nanosheet |
| CN115108591A (en) * | 2022-08-31 | 2022-09-27 | 金川集团股份有限公司 | Preparation method of low-sulfur cobaltosic oxide |
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| CN112499692A (en) * | 2020-12-02 | 2021-03-16 | 金川集团股份有限公司 | Preparation method of aluminum-doped cobaltosic oxide |
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| CN103709798A (en) * | 2013-12-30 | 2014-04-09 | 昆明理工大学 | Inorganic fireproof material and preparation method thereof |
| CN105170195A (en) * | 2015-09-14 | 2015-12-23 | 新奥科技发展有限公司 | Forming method of catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113735183A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of aluminum-doped cobaltosic oxide |
| CN114906878A (en) * | 2022-04-07 | 2022-08-16 | 浙江格派钴业新材料有限公司 | Preparation method of battery-grade cobalt hydroxide nanosheet |
| CN115108591A (en) * | 2022-08-31 | 2022-09-27 | 金川集团股份有限公司 | Preparation method of low-sulfur cobaltosic oxide |
| CN115108591B (en) * | 2022-08-31 | 2024-05-03 | 金川集团镍钴有限公司 | Preparation method of low-sulfur cobaltosic oxide |
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Application publication date: 20210730 |