CN113651366A - Secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide - Google Patents
Secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide Download PDFInfo
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- C01P2006/11—Powder tap density
Abstract
The invention belongs to the technical field of preparation methods of battery-grade cobaltosic oxide, and discloses a secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide, which comprises the following steps: adding pure water and a precipitator solution into a reaction kettle to serve as a base solution, stirring, simultaneously adding a cobalt-aluminum solution and the precipitator solution into the reaction kettle, carrying out precipitation reaction, controlling the reaction pH to be 7.2-7.3, keeping the flow of the cobalt-aluminum solution unchanged, and reacting for 90-120 h to obtain a slurry finished product; centrifuging, washing and dehydrating the slurry finished product to obtain a wet material finished product; calcining the wet material finished product once at low temperature in a roller kiln to obtain an aluminum-doped cobaltosic oxide semi-finished product; and calcining the aluminum-doped cobaltosic oxide semi-finished product at high temperature in a rotary kiln to obtain the aluminum-doped cobaltosic oxide. The preparation method of the invention can produce the lower small-particle-size aluminum-doped cobaltosic oxide with high tap density, uniform particle size distribution and no agglomeration phenomenon.
Description
Technical Field
The invention belongs to the technical field of preparation methods of battery-grade cobaltosic oxide, and particularly relates to a secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide.
Background
In the positive electrode material of lithium ion battery, LiCoO2Has been dominated by LiCoO2The lithium ion battery is very suitable for the insertion and the desorption of lithium ions, has the advantages of high voltage, stable discharge, high specific energy, good cycle performance, simple preparation process and the like, and can adapt to large-current charge and discharge. The small-particle cobaltosic oxide is mainly used for preparing high-rate lithium cobaltate. At present, the common small-particle cobaltosic oxide in the market, such as cobaltosic oxide with a small particle size doped with metal elements, has the problems of low tap density and serious agglomeration phenomenon, which can cause poor cycle performance and poor stability of the lithium ion battery.
Disclosure of Invention
In view of the above, the invention provides a secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide, in order to solve the problems of uneven particle size distribution and serious agglomeration of the aluminum-doped cobaltosic oxide prepared by the existing preparation method of small-particle-size metallic element-doped cobaltosic oxide.
The invention is realized by the following scheme:
a secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide comprises the following steps:
firstly, calcining the finished product of the aluminum-doped cobalt carbonate wet material in a roller kiln at a low temperature to obtain a semi-finished product of the aluminum-doped cobaltosic oxide;
and then calcining the aluminum-doped cobaltosic oxide semi-finished product at high temperature in a rotary kiln to obtain the aluminum-doped cobaltosic oxide.
Preferably, the low-temperature calcination conditions are as follows: calcining for 16-24 h at 300-400 ℃ to obtain the aluminum-doped cobaltosic oxide semi-finished product. In a specific embodiment, the low-temperature calcination temperature may be 300 ℃, 400 ℃, or any temperature value between 300 ℃ and 400 ℃, for example, 350 ℃; the low-temperature calcination time can be 16h, 24h, or any time value between 16h and 24h, such as 20 h.
Preferably, the high-temperature calcination conditions are as follows: calcining for 2-5 h at 650-700 ℃ to obtain the aluminum-doped cobaltosic oxide. In a specific embodiment, the high-temperature calcination temperature may be 650 ℃, 700 ℃, or any temperature value between 650 ℃ and 700 ℃, for example 680 ℃; the high-temperature calcination time can be 2 hours, 5 hours, or any time value between 2 and 5 hours, such as 3.5 hours.
Preferably, the finished product of the aluminum-doped cobalt carbonate wet material is prepared by the following method:
s1, respectively preparing cobalt-aluminum solutions containing cobalt ions and aluminum ions, and preparing a precipitator solution containing carbonate ions for later use;
s2, adding pure water and a precipitant solution into a reaction kettle to serve as a base solution, stirring, simultaneously adding the cobalt-aluminum solution and the precipitant solution into the reaction kettle, carrying out precipitation reaction, controlling the pH of the reaction to be 7.2-7.3, keeping the flow of the cobalt-aluminum solution unchanged, and reacting for 90-120 h to obtain a slurry finished product;
and S3, centrifuging, washing and dehydrating the slurry finished product to obtain a wet material finished product.
Preferably, in the step S1, the cobalt ion concentration in the cobalt-aluminum solution is 100-150 g/L, and the aluminum ion concentration is 0.5-1 g/L. In the embodiment, the concentration of cobalt ions in the cobalt-aluminum solution may be 100g/L, 150g/L, or 125 g/L; the concentration of aluminum ions may be 0.5g/L, 1g/L, or 0.75 g/L.
Preferably, the precipitant solution is one or at least two of ammonium bicarbonate solution, ammonium carbonate solution, sodium bicarbonate solution and sodium carbonate solution, and the concentration of carbonate ions in the precipitant solution is 200-250 g/L. In a specific embodiment, the concentration of carbonate ions in the precipitant solution may be 200g/L, may be 250g/L, or may be any one concentration value between 200 and 250g/L, for example, 220 g/L.
Preferably, in the step S2, the flow rate of the cobalt-aluminum solution is 200-400L/h, and the flow rate of the precipitant solution is 900-1500L/h. In a specific embodiment, the flow rate of the cobalt-aluminum solution may be 200L/h, may be 400L/h, or may be any flow rate value between 200 and 400L/h, for example, 300L/h; or the flow of the cobalt-aluminum solution can be timely adjusted within the range of 200-400L/h according to the actual production process; the flow rate of the precipitant solution is 900-1500L/h, and the precipitant solution mainly has the function of adjusting the pH of the reaction system to maintain the pH of the reaction system within the range of 7.2-7.3, so that in the specific production process, the flow rate of the precipitant solution needs to be within the range of 900-1500L/h, and the pH of the reaction system is timely adjusted.
Preferably, in S2, the process of preparing the base solution is as follows:
mixing 1 to 3m3Adding pure water into a reaction kettle, heating to 30-50 ℃, adding 300-450L of the S1 precipitant solution, and stirring at 1500-2500 rpm.
Preferably, in the step S3, the slurry finished product is pumped to a centrifuge, washed with water at 60 to 80 ℃ for 3 to 6 times, and then dehydrated to obtain a wet material finished product. In an embodiment, the amount of hot water for washing may be 2m3。
Compared with the prior art, the invention adopting the scheme has the beneficial effects that:
when the method is used for calcining, the small-particle-size aluminum-doped cobaltosic oxide is successfully prepared by firstly calcining at low temperature in a roller kiln and then calcining at high temperature in a rotary kiln. Detection shows that the small-particle-size aluminum-doped cobaltosic oxide prepared by the method has uniform particle size distribution (about 4.0-5.0 mu m in particle size), high tap density and no agglomeration phenomenon among particles.
Drawings
FIG. 1 is an electron microscope image of small-particle-size aluminum-doped cobaltosic oxide prepared by the secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide provided by the embodiment of the invention;
FIG. 2 is an electron microscope image of small-particle-size aluminum-doped cobaltosic oxide prepared by the one-time calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide provided in comparative example 1 of the present invention;
FIG. 3 is an electron microscope image of small-particle-size aluminum-doped cobaltosic oxide prepared by the one-time calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide provided in comparative example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the following examples, when preparing a cobalt-aluminum solution containing cobalt ions and aluminum ions, the cobalt salt used may be cobalt salt capable of being completely ionized in water, such as cobalt chloride, cobalt sulfate, or cobalt nitrate; the aluminum salt used may be aluminum sulfate, aluminum chloride, or other aluminum salt that can be ionized in water.
In the following examples, when a precipitant solution containing carbonate ions is prepared, the solute used is a salt capable of ionizing carbonate ions in water, and may be, for example, ammonium bicarbonate, sodium bicarbonate, ammonium carbonate, or sodium carbonate.
When preparing a cobalt-aluminum-containing solution, firstly respectively preparing a cobalt solution containing cobalt ions and an aluminum solution containing aluminum ions; the cobalt solution and the aluminum solution are then mixed to obtain a cobalt aluminum solution. This ensures that the cobalt ions and the aluminum ions are uniformly mixed.
Examples
The embodiment provides a secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide, which comprises the following steps:
s1, respectively preparing cobalt-aluminum solution containing cobalt ions and aluminum ions, and preparing ammonium bicarbonate solution with the concentration of 200g/L for later use; wherein, in the cobalt-aluminum solution, the concentration of cobalt ions is 100g/L, and the concentration of aluminum ions is 0.5 g/L;
s2, selecting 8m3The reaction kettle is taken as a reaction vessel, and 1m of the reaction kettle is added3Heating the pure water to 30 ℃, adding 300L of ammonium bicarbonate solution prepared in S1 into the reaction kettle, and stirring at the rotating speed of 1500rpm for later use;
simultaneously adding the cobalt-aluminum solution and the ammonium bicarbonate solution prepared in the step S1 into the reaction kettle, continuously stirring, carrying out precipitation reaction, wherein the flow rate of the cobalt-aluminum solution is 300L/h, the flow rate of the ammonium bicarbonate is adjusted to be 900L/h-1500L/h, the reaction pH is controlled to be 7.2-7.3, the flow rate of the cobalt-aluminum solution is kept unchanged, and reacting for 90 hours to obtain a slurry finished product;
s3, pumping the slurry finished product obtained in the step S3 to a centrifuge, washing the centrifuge five times for 5min each time according to the program, and sharing hot water for 2m3The temperature of the hot water is 60 ℃, and then the wet material is dehydrated to obtain a finished product of the wet material;
s4, directly adding the wet material finished product into a sagger of a roller kiln, setting the temperature of the roller kiln to be 300 ℃, and calcining for 24 hours to obtain an aluminum-doped cobaltosic oxide semi-finished product; wherein the saggars move forwards at the speed of 2.7m/min, and each saggar is filled with 6-10 kg of wet material finished products;
s5, putting the aluminum-doped cobaltosic oxide semi-finished product into a rotary kiln through a spiral feeding device at a feeding amount of 150kg/h, carrying out high-temperature calcination at the temperature of 650 ℃ for 5h, and then discharging, screening and removing iron to obtain the aluminum-doped cobaltosic oxide.
The detection of the aluminum-doped cobaltosic oxide prepared in the example shows that the tap density is 2.03g/cm3The tap density of the embodiment meets the requirement of the battery grade cobaltosic oxide field on the tap density of small-particle-size aluminum-doped cobaltosic oxide; in addition, as can be seen from a scanning electron microscope (as shown in fig. 1) photographed, the particle size distribution of the aluminum-doped cobaltosic oxide prepared by the present embodiment is uniform, about 4.0-5.0 μm, and there is almost no agglomeration phenomenon.
In addition, after the base solution is prepared, the reaction pH is controlled by controlling the flow rate of the precipitant solution, and the aluminum-doped cobaltosic oxide can be successfully prepared by controlling less parameters such as reaction time, reaction temperature and the like, so that the preparation method of the embodiment is easy for batch and large-scale production; and the performance of the product generated in a large scale is relatively uniform.
Comparative example 1
The comparative example provides a one-time calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide, which comprises the following steps:
s1, respectively preparing cobalt-aluminum solution containing cobalt ions and aluminum ions, and preparing ammonium bicarbonate solution with the concentration of 220g/L for later use; wherein, in the cobalt-aluminum solution, the concentration of cobalt ions is 100g/L, and the concentration of aluminum ions is 0.50 g/L;
s2, selecting 8m3The reaction kettle is taken as a reaction vessel, and 1m of the reaction kettle is added3Heating the pure water to 40 ℃, adding 340L of the ammonium bicarbonate solution prepared in the S1 into the reaction kettle, and stirring at the rotating speed of 1500rpm for later use;
adding the cobalt-aluminum solution and the ammonium bicarbonate solution prepared in the step S1 into the reaction kettle at the same time, continuously stirring, carrying out a precipitation reaction, wherein the flow rate of the cobalt-aluminum solution is 300L/h, the flow rate of the ammonium bicarbonate is adjusted to be 900L/h-1500L/h, the reaction pH is controlled to be 7.2-7.3, the flow rate of the cobalt-aluminum solution is kept unchanged, and reacting for 115 hours to obtain a slurry finished product;
s3, pumping the slurry finished product obtained in the step S3 to a centrifuge, washing the centrifuge five times for 5min each time according to the program, and sharing hot water for 2m3The temperature of the hot water is 60 ℃, and then the wet material is dehydrated to obtain a finished product of the wet material;
s4, directly adding the wet material finished product into a sagger of a roller kiln, setting the temperature of the roller kiln to 700 ℃, and calcining for 4-5 hours to obtain an aluminum-doped cobaltosic oxide semi-finished product; wherein the saggars move forwards at the speed of 2.7m/min, each saggar is filled with 6-10 kg of wet material finished products, and then the materials are discharged, screened and deironized to obtain the aluminum-doped cobaltosic oxide.
Namely, the steps of comparative examples S1 to S3, are the same as those of examples S1 to S3. The comparative example is different from the examples in that:
in the comparative example, the wet material finished product obtained by S3 is directly added into a roller kiln and calcined for 20 hours at high temperature (700 ℃);
in the example, the wet material obtained in S3 is calcined in a roller kiln at a low temperature (300 ℃) for 24 hours, and then calcined in a rotary kiln at a high temperature (650 ℃) for 5 hours.
The detection of the aluminum-doped cobaltosic oxide prepared by the comparative example shows that the tap density is 2.05g/cm3The tap density meets the requirement of the battery grade cobaltosic oxide field on the tap density of the small-particle-size aluminum-doped cobaltosic oxide; in addition, as can be seen from the scanning electron microscope (as shown in fig. 2) photographed, the particle size distribution of the aluminum-doped cobaltosic oxide prepared by the comparative example is not uniform, and although the particle size is about 4.0-5.20 μm, the comparative example has a serious sintering agglomeration phenomenon compared with the sintering case of the example (fig. 1).
Comparative example 2
The comparative example provides a preparation method of small-particle-size aluminum-doped cobaltosic oxide by secondary calcination, which comprises the following steps:
s1, respectively preparing cobalt-aluminum solution containing cobalt ions and aluminum ions, and preparing ammonium bicarbonate solution with the concentration of 200g/L for later use; wherein, in the cobalt-aluminum solution, the concentration of cobalt ions is 100g/L, and the concentration of aluminum ions is 0.50 g/L;
s2, selecting 8m3The reaction kettle is taken as a reaction vessel, and 1m of the reaction kettle is added3Heating the pure water to 50 ℃, adding 340L of the ammonium bicarbonate solution prepared in the S1 into the reaction kettle, and stirring at the rotating speed of 1500rpm for later use;
adding the cobalt-aluminum solution and the ammonium bicarbonate solution prepared in the step S1 into the reaction kettle at the same time, continuously stirring, carrying out a precipitation reaction, wherein the flow rate of the cobalt-aluminum solution is 300L/h, the flow rate of the ammonium bicarbonate is adjusted to be 900L/h-1500L/h, the reaction pH is controlled to be 7.2-7.3, the flow rate of the cobalt-aluminum solution is kept unchanged, and reacting for 115 hours to obtain a slurry finished product;
s3, pumping the slurry finished product obtained in the step S3 to a centrifuge, washing the centrifuge five times for 5min each time according to the program, and sharing hot water for 2m3The temperature of the hot water is 60 ℃, and then the wet material is dehydrated to obtain a finished product of the wet material;
s4, putting the aluminum-doped cobaltosic oxide semi-finished product into a rotary kiln through a spiral feeding device at a feeding amount of 150kg/h, carrying out high-temperature calcination at 700 ℃ for 4-5h, and then discharging, screening and removing iron to obtain the aluminum-doped cobaltosic oxide.
Namely, the steps of comparative examples S1 to S3, are the same as those of examples S1 to S3. The comparative example is different from the examples in that:
in the comparative example, the wet material finished product obtained by S3 is directly added into a rotary kiln and calcined for 4 to 5 hours at high temperature (700 ℃);
in the example, the wet material obtained in S3 is calcined in a roller kiln at a low temperature (300 ℃) for 24 hours, and then calcined in a rotary kiln at a high temperature (650 ℃) for 5 hours.
As can be seen from the scanning electron microscope (as shown in FIG. 3) taken by the present embodiment, although the particle size distribution of the aluminum-doped cobaltosic oxide prepared by the present embodiment is uniform, about 4.5 to 5.0 μm, and there is almost no agglomeration phenomenon; however, the tap density of the aluminum-doped cobaltosic oxide prepared in the comparative example was 1.80g/cm3The tap density is obviously lower than that of the embodiment, namely the tap density of the comparative example can not meet the requirement of the battery grade cobaltosic oxide field on the tap density of the small-particle-size aluminum-doped cobaltosic oxide.
In summary, it can be seen from the above examples and comparative examples that only by using the preparation method of the present invention, the wet material product of aluminum-doped cobalt carbonate is first calcined in a roller kiln at a low temperature, and then calcined in a rotary kiln at a high temperature, i.e. by using two calcining processes, the tap density can be successfully prepared, i.e. the tap density meets the requirement of the battery grade cobaltosic oxide field on the tap density of small-particle-size aluminum-doped cobaltosic oxide; the particle size distribution is uniform, and the agglomeration problem among particles is hardly caused.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide is characterized by comprising the following steps:
firstly, calcining the finished product of the aluminum-doped cobalt carbonate wet material in a roller kiln at a low temperature to obtain a semi-finished product of the aluminum-doped cobaltosic oxide;
and then calcining the aluminum-doped cobaltosic oxide semi-finished product at high temperature in a rotary kiln to obtain the aluminum-doped cobaltosic oxide.
2. The method for preparing small-particle-size aluminum-doped cobaltosic oxide by secondary calcination according to claim 1, wherein the low-temperature calcination conditions are as follows: calcining for 16-24 h at 300-400 ℃ to obtain the aluminum-doped cobaltosic oxide semi-finished product.
3. The method for preparing small-particle-size aluminum-doped cobaltosic oxide by secondary calcination according to claim 1, wherein the high-temperature calcination conditions are as follows: calcining for 2-5 h at 650-700 ℃ to obtain the aluminum-doped cobaltosic oxide.
4. The method for preparing small-particle-size aluminum-doped cobaltosic oxide through secondary calcination as claimed in claim 1, wherein the finished product of the aluminum-doped cobalt carbonate wet material is prepared by the following method:
s1, respectively preparing cobalt-aluminum solutions containing cobalt ions and aluminum ions, and preparing a precipitator solution containing carbonate ions for later use;
s2, adding pure water and a precipitant solution into a reaction kettle to serve as a base solution, stirring, simultaneously adding the cobalt-aluminum solution and the precipitant solution into the reaction kettle, carrying out precipitation reaction, controlling the pH of the reaction to be 7.2-7.3, keeping the flow of the cobalt-aluminum solution unchanged, and reacting for 90-120 h to obtain a slurry finished product;
and S3, centrifuging, washing and dehydrating the slurry finished product to obtain the aluminum-doped cobalt carbonate wet material finished product.
5. The method for preparing small-particle-size aluminum-doped cobaltosic oxide through secondary calcination according to claim 4, wherein in S1, the concentration of cobalt ions in the cobalt-aluminum solution is 100-150 g/L, and the concentration of aluminum ions is 0.5-1 g/L.
6. The method for preparing aluminum-doped cobaltosic oxide with small particle size by secondary calcination as claimed in claim 4, wherein the precipitant solution is one or at least two of ammonium bicarbonate solution, ammonium carbonate solution, sodium bicarbonate solution and sodium carbonate solution, and the concentration of carbonate ions in the precipitant solution is 200-250 g/L.
7. The method for preparing small-particle-size aluminum-doped cobaltosic oxide through secondary calcination according to claim 4, wherein in S2, the flow rate of the cobalt-aluminum solution is 200-400L/h, and the flow rate of the precipitant solution is 900-1500L/h.
8. The method for preparing small-particle-size aluminum-doped cobaltosic oxide through secondary calcination according to claim 4, wherein in the step S2, the process of preparing the base solution comprises the following steps:
mixing 1 to 3m3Adding pure water into a reaction kettle, heating to 30-50 ℃, adding 300-450L of the S1 precipitant solution, and stirring at 1500-2500 rpm.
9. The secondary calcination preparation method of small-particle-size aluminum-doped cobaltosic oxide as claimed in any one of claims 4 to 8, wherein in S3, the slurry finished product is pumped to a centrifuge, washed with water at 60 ℃ to 80 ℃ for 3 to 6 times, and then dehydrated to obtain a wet material finished product.
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| CN105731551A (en) * | 2014-12-09 | 2016-07-06 | 荆门市格林美新材料有限公司 | Doped cobalt carbonate, doped tricobalt tetroxide and preparation methods thereof |
| CN108609666A (en) * | 2018-04-25 | 2018-10-02 | 中南林业科技大学 | A kind of preparation method of the cobaltosic oxide of metallic element grade doping |
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