CN112850803A - Synthesis method of high-tap-density superfine cobaltosic oxide - Google Patents
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Abstract
The invention discloses a method for synthesizing high-tap superfine cobaltosic oxide, which comprises the following three stages: 1) adding the base solution into the reaction kettle, keeping the temperature of the base solution stable, adding a complexing agent, adjusting the pH value of the base solution, and stirring and mixing; 2) keeping the stirring speed unchanged, simultaneously adding the cobalt salt solution and the alkali solution into a reaction kettle, and carrying out stirring reaction by controlling the flow rates of the cobalt salt solution and the alkali solution and keeping the pH value between 10.5 and 11.5 to obtain a cobalt salt precipitate; 3) and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain a target product. By adopting the method for preparing the cobaltosic oxide in the staged ammonia-free environment, the invention has the advantages that the whole preparation process has little influence on the environment, the particle size of the prepared cobaltosic oxide is small, the particle size distribution consistency is high, the tap density is high, and when the cobaltosic oxide is applied to the production of 3C batteries, the standby time of the batteries can be prolonged, and the safety performance of the batteries can be improved.
Description
Technical Field
The invention belongs to the technical field of preparation of cobaltosic oxide, and particularly relates to a synthesis method of high-tap-density ultrafine cobaltosic oxide.
Background
Lithium cobaltate is a main anode material for producing 3C batteries, and along with the continuous improvement of living standard, the specific energy requirement of people on the 3C batteries is improved, so that 3C electronic products are required to have longer standby time and more excellent safety performance; therefore, the preparation of high-capacity and high-power lithium ion storage batteries is a necessary trend in the development of 3C electronic products.
Two industry-recognized technical approaches are available for realizing high capacity quantization of 3C lithium batteries: firstly, adopting a high-nickel ternary precursor material; secondly, preparing a lithium cobaltate precursor material with wide particle size distribution; the high-nickel ternary material has the original characteristic of high capacity in the aspect of genetics, but the safety performance of the high-nickel ternary material needs to be improved, and the high-nickel ternary material is not widely applied to the 3C electronic industry at present; the lithium cobaltate precursor with wide particle size distribution is designed and adjusted to achieve high compaction so as to realize high capacity of the battery.
The current lithium cobaltate material technology development direction is independent research and reasonable collocation of large and small particles; at present, large-particle cobaltosic oxide in the market is mature, high-tap-density ultrafine cobaltosic oxide (less than 2.0um) is in a development stage, and the product in the market is not an enterprise for industrial supply. The high tap density superfine cobaltosic oxide is urgently needed in the development direction of high capacity of lithium cobaltate materials.
Some enterprises synthesize small-particle cobalt carbonate through an ammonium bicarbonate system, and then the cobalt carbonate is calcined into superfine cobaltosic oxide at high temperature, and the technology has the defects that: the tap density of the superfine cobaltosic oxide is lower than 1.8g/cm 3; secondly, the environmental treatment pressure of an ammonium bicarbonate system is too high;
the sodium hydroxide system is used for synthesizing superfine cobalt oxide by a continuous method, and the superfine cobalt oxide is calcined into superfine cobaltosic oxide by high temperature, and the technology has the defects that: the uniformity of the particle size of the superfine cobalt oxide is poor, and a product with uniform particle size distribution cannot be obtained; secondly, the one-time yield is low, and the production cost is high; thirdly, the tap fluctuation of the superfine cobalt oxide is large; and fourthly, the production operation is complex.
Disclosure of Invention
In view of the above, the present invention provides a method for synthesizing high tap density ultrafine cobaltosic oxide, which solves the problems of the prior art that the cobaltosic oxide obtained has a large particle size and a small tap density, which results in an insufficient application, and the prepared 3C battery has a short standby time and a poor safety performance.
In order to achieve the purpose, the technical scheme of the invention is realized as follows: a method for synthesizing high tap density superfine cobaltosic oxide specifically comprises the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding pure water with the temperature of 70-100 ℃ into a reaction kettle to serve as base liquid, keeping the temperature of the base liquid stable, adding a complexing agent, adjusting the pH value of the base liquid to 11.5-12.5 through sodium hydroxide, and stirring and mixing;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed in the first stage unchanged, simultaneously adding a cobalt salt solution and an alkali solution into a reaction kettle containing the base solution, and stirring and reacting by controlling the flow rates of the cobalt salt solution and the alkali solution and keeping the pH value between 10.5 and 11.5 within 4 to 8 hours to obtain a cobalt salt precipitate;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Preferably, in the first stage, the complexing agent is at least one of sodium EDTA and ammonium bicarbonate.
In the first stage, the stirring speed is 150-250 r/min.
Preferably, in the second stage, the concentration of cobalt ions in the cobalt salt solution is 120-140 g/L; the mass concentration of the alkali solution is 32-33%.
Preferably, in the second stage, the flow rate of the cobalt salt solution is 300-500L/h, and the flow rate of the alkali solution is 100-200L/h.
Preferably, in the second stage, the stirring speed is 150-250 r/min, and the stirring reaction temperature is 70-80 ℃.
Preferably, in the second stage, the reaction temperature is 70-85 ℃; the reaction time is 50-85.
Preferably, in the second stage, the ratio of the flow rate of the compressed air to the flow rate of the cobalt chloride is controlled to be (70-100): 1
Preferably, in the second stage, the cobalt salt in the cobalt salt solution is at least one of cobalt chloride, cobalt sulfate and cobalt nitrate.
Compared with the prior art, the method for preparing the cobaltosic oxide by stages in an ammonia-free environment ensures that the whole preparation process has small influence on the environment, the prepared cobaltosic oxide has small particle size (1.7-2.0um), high particle size distribution consistency and high tap density (2.3-2.5 g/cm)3) When the lithium iron phosphate is applied to the production of 3C batteries, the standby time of the batteries can be prolonged, the safety performance of the batteries is improved, and the lithium iron phosphate is worthy of being widely popularized and used; the method is simple to operate and easy to control the production process.
Drawings
FIG. 1 is an SEM image of the ultrafine cobaltosic oxide prepared by the method of example 4 according to the present invention at 10000 times magnification;
FIG. 2 is an SEM image of the ultrafine cobaltosic oxide prepared by the method of example 4 according to the invention at 5000 times magnification;
FIG. 3 is an SEM image of the superfine cobaltosic oxide prepared by the method of example 4 with high tap density at 3000 times magnification;
fig. 4 is an SEM image of the ultrafine cobaltosic oxide prepared by the method for preparing high tap density ultrafine cobaltosic oxide according to example 4 of the present invention under a state of 1000 times magnification.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and 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.
The embodiment of the invention provides a method for synthesizing high-tap superfine cobaltosic oxide, which comprises the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding pure water with the temperature of 70-100 ℃ into a reaction kettle as a base solution, keeping the temperature of the base solution stable, adding a complexing agent, adjusting the pH value of the base solution to 11.5-12.5 by using sodium hydroxide, and mixing at the stirring speed of 150-250 r/min; wherein the complexing agent is at least one of EDTA sodium salt and ammonium bicarbonate;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 150-250 r/min unchanged, simultaneously adding a cobalt salt solution with the cobalt ion concentration of 120-140 g/L and an alkali solution with the mass concentration of 32-33% into a reaction kettle containing the base solution, controlling the flow rate of the cobalt salt solution at 300-500L/h and the flow rate of the alkali solution at 100-200L/h, keeping the pH value between 10.5 and 11.5 within 4-8 h, and reacting for 50-85 h at the temperature of 70-85 ℃ and the stirring speed of 150-250 r/min to obtain a cobalt salt precipitate; wherein the ratio of the flow of the compressed air to the flow of the cobalt chloride is controlled to be (70-100) in the feeding process: 1; the cobalt salt in the cobalt salt solution is at least one of cobalt chloride, cobalt sulfate and cobalt nitrate;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 1
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 4m into a reaction kettle3Using pure water at 70 deg.C as base solution, maintainingThe temperature of the base solution is stable, EDTA sodium salt is added, the pH value of the base solution is adjusted to 11.5 by sodium hydroxide, and the base solution is mixed at the stirring speed of 150 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 150r/min, simultaneously adding 130g/L cobalt chloride solution with cobalt ion concentration and 32% aqueous alkali into a reaction kettle containing the base solution, controlling the flow rate of the cobalt chloride solution at 300L/h and the flow rate of the sodium hydroxide solution at 100L/h, keeping the pH value between 10.5 and 10.7 within 5h, and reacting for 50h at 70 ℃, 24000L/h of compressed air introduction and 200r/min of stirring speed to obtain a cobalt salt precipitate with D50 of 1.9 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 2
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 5m into a reaction kettle3Taking pure water at 75 ℃ as a base solution, keeping the temperature of the base solution stable, adding EDTA sodium salt, adjusting the pH value of the base solution to 12.0 by using sodium hydroxide, and mixing at the stirring speed of 170 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 170r/min unchanged, simultaneously adding a cobalt chloride solution with the concentration of 130g/L cobalt ions and an alkali solution with the mass concentration of 32% into a reaction kettle containing the base solution, keeping the pH value between 11.0 and 11.2 within 6h by controlling the flow rate of the cobalt chloride solution at 350L/h and the flow rate of a sodium hydroxide solution at 130L/h, and reacting for 60h at 75 ℃, wherein the introduction amount of compressed air is 35000L/h and the stirring speed is 170r/min to obtain a cobalt salt precipitate with the D50 of 1.8 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 3
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 5m into a reaction kettle3Taking pure water at 80 ℃ as a base solution, keeping the temperature of the base solution stable, adding EDTA sodium salt, adjusting the pH value of the base solution to 12.5 by using sodium hydroxide, and mixing at a stirring speed of 200 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 200r/min, simultaneously adding 130g/L cobalt chloride solution with cobalt ion concentration and 32% aqueous alkali into a reaction kettle containing the base solution, controlling the flow rate of the cobalt chloride solution at 400L/h and the flow rate of the sodium hydroxide solution at 145L/h, keeping the pH value between 11.2 and 11.4 within 8h, and reacting for 67h at 80 ℃, with the introduction amount of compressed air at 35000L/h and the stirring speed at 200r/min to obtain a cobalt salt precipitate with D50 of 1.8 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 4
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 6m into a reaction kettle3Taking pure water at 85 ℃ as a base solution, keeping the temperature of the base solution stable, adding an ammonium bicarbonate solution, adjusting the pH value of the base solution to 12.5 by sodium hydroxide, and mixing at a stirring speed of 200 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 200r/min, simultaneously adding 130g/L cobalt chloride solution with cobalt ion concentration and 32% aqueous alkali with mass concentration into a reaction kettle containing the base solution, keeping the pH value between 11.2 and 11.4 within 8h by controlling the flow rate of the cobalt chloride solution at 500L/h and the flow rate of the sodium hydroxide solution at 175L/h, and reacting for 85h at 85 ℃, wherein the introduction amount of compressed air is 50000L/h, and the stirring speed is 200r/min, so as to obtain a cobalt salt precipitate with D50 of 2.0 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
The high tap density ultrafine cobaltosic oxide obtained in the example 4 is subjected to electron microscope scanning detection, the detection results are shown in fig. 1-4, and it can be seen from the figure that the cobaltosic oxide obtained by the method of the present invention has the advantages of large density, small particle size and uniform distribution, and the application universality is effectively increased.
Example 5
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 5m into a reaction kettle3Taking pure water at 85 ℃ as a base solution, keeping the temperature of the base solution stable, adding an ammonium bicarbonate solution, adjusting the pH value of the base solution to 12.0 by sodium hydroxide, and mixing at a stirring speed of 200 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 200r/min, simultaneously adding a cobalt chloride solution with the concentration of 130g/L cobalt ions and an alkali solution with the mass concentration of 33% into a reaction kettle containing the base solution, keeping the pH value between 11.0 within 6h by controlling the flow of the cobalt chloride solution at 400L/h and the flow of the sodium hydroxide solution at 140L/h, and reacting for 55h at 75 ℃, the introduction amount of compressed air at 35000L/h and the stirring speed at 200r/min to obtain a cobalt salt precipitate with the D50 of 1.9 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 6
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 4m into a reaction kettle3Using pure water at 70 ℃ as a base solution, keeping the temperature of the base solution stable, adding EDTA sodium salt, adjusting the pH value of the base solution to 11.5 by using sodium hydroxide, and mixing at a stirring speed of 150 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 150r/min, simultaneously adding a cobalt chloride solution with the concentration of cobalt ions of 120g/L and an alkali solution with the mass concentration of 33% into a reaction kettle containing the base solution, keeping the pH value between 10.5 within 4h by controlling the flow rate of the cobalt salt solution at 300L/h and the flow rate of the alkali solution at 100L/h, and reacting for 65h at 70 ℃, the introduction amount of compressed air of 24000L/h and the stirring speed of 150r/min to obtain a cobalt salt precipitate with the D50 of 1.8 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 7
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 6m into a reaction kettle3Taking pure water at 100 ℃ as a base solution, keeping the temperature of the base solution stable, adding EDTA sodium salt, adjusting the pH value of the base solution to 12.5 by using sodium hydroxide, and mixing at a stirring speed of 250 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 250r/min, simultaneously adding a cobalt chloride solution with the cobalt ion concentration of 140g/L and an alkali solution with the mass concentration of 32% into a reaction kettle containing the base solution, keeping the pH value between 11.5 within 8h by controlling the flow rate of the cobalt salt solution at 500L/h and the flow rate of the alkali solution at 200L/h, and reacting for 70h at 80 ℃, the introduction amount of compressed air at 50000L/h and the stirring speed at 250r/min to obtain a cobalt salt precipitate with the D50 of 2.0 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 8
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 6m into a reaction kettle3Taking pure water at 85 ℃ as a base solution, keeping the temperature of the base solution stable, adding an ammonium bicarbonate solution, adjusting the pH value of the base solution to 12.0 by sodium hydroxide, and mixing at a stirring speed of 200 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 200r/min, simultaneously adding a cobalt sulfate solution with the concentration of cobalt ions of 120g/L and an alkali solution with the mass concentration of 33% into a reaction kettle containing the base solution, keeping the pH value between 10.5 within 4h by controlling the flow rate of the cobalt salt solution at 300L/h and the flow rate of the alkali solution at 100L/h, and reacting for 75h at 70 ℃, the introduction amount of compressed air of 24000L/h and the stirring speed of 150r/min to obtain a cobalt salt precipitate with the D50 of 1.8 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Example 9
The high tap density superfine cobaltosic oxide is realized by the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding 4m into a reaction kettle3Using pure water at 70 ℃ as a base solution, keeping the temperature of the base solution stable, adding EDTA sodium salt, adjusting the pH value of the base solution to 11.5 by using sodium hydroxide, and mixing at a stirring speed of 150 r/min;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed at 150r/min, simultaneously adding a cobalt salt solution with the concentration of 130g/L cobalt ions and an alkali solution into a reaction kettle containing the base solution, controlling the flow rate of a cobalt chloride solution at 400L/h and the flow rate of a sodium hydroxide solution at 140L/h, keeping the pH value between 11.0 within 6h, and reacting for 80h at 75 ℃, the introduction amount of compressed air at 35000L/h and the stirring speed at 200r/min to obtain a cobalt salt precipitate with the D50 of 2.0 um;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and (4) sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
Detection example 1
The average particle diameter (D50), Tap Density (TD) and sodium content of the cobaltosic oxide obtained in examples 1 to 9 were measured, and the results are shown in table 1;
as can be seen from the data in Table 1, the average particle diameter of the cobaltosic oxide obtained by the invention is 1.7-2.0um, and the tap density is 2.3-2.5g/cm3The requirements of high tap density and superfine cobaltosic oxide are met, when the high tap density and superfine cobaltosic oxide obtained by the method is applied to the production of 3C batteries, the standby time of a battery 10 can be well prolonged, the safety performance of the battery is improved, and the method is worthy of popularization and application; the method is simple to operate and easy to control the production process.
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. The method for synthesizing the high-tap-density superfine cobaltosic oxide is characterized by comprising the following three stages:
the first stage is as follows: the preparation period of the reaction is as follows:
adding pure water with the temperature of 70-100 ℃ into a reaction kettle to serve as base liquid, keeping the temperature of the base liquid stable, adding a complexing agent, adjusting the pH value of the base liquid to 11.5-12.5 through sodium hydroxide, and stirring and mixing;
and a second stage: the reaction stabilization period is as follows:
keeping the stirring speed in the first stage unchanged, simultaneously adding a cobalt salt solution and an alkali solution into a reaction kettle containing the base solution, and stirring and reacting by controlling the flow rates of the cobalt salt solution and the alkali solution and keeping the pH value between 10.5 and 11.5 within 4 to 8 hours to obtain a cobalt salt precipitate;
and a third stage: the post-reaction treatment period comprises the following specific steps:
and sequentially carrying out centrifugal washing, drying and roasting on the cobalt salt precipitate to obtain the high-tap-density superfine cobaltosic oxide.
2. The method for synthesizing high-tap ultrafine cobaltosic oxide according to claim 1, wherein in the first stage, the complexing agent is at least one of sodium EDTA and ammonium bicarbonate.
3. The method as claimed in claim 1, wherein the stirring speed in the first stage is 150-250 r/min.
4. The method for synthesizing high-tap superfine cobaltosic oxide according to claim 1, wherein in the second stage, the concentration of cobalt ions in the cobalt salt solution is 120-140 g/L; the mass concentration of the alkali solution is 32-33%.
5. The method for synthesizing high-tap density ultrafine cobaltosic oxide according to claim 1, wherein in the second stage, the flow rate of the cobalt salt solution is 300-500L/h, and the flow rate of the alkali solution is 100-200L/h.
6. The method for synthesizing high-tap density ultrafine cobaltosic oxide according to claim 1, wherein in the second stage, the stirring speed is 150-250 r/min, and the stirring reaction temperature is 70-80 ℃.
7. The method for synthesizing high-tap-density ultrafine cobaltosic oxide according to claim 1, wherein in the second stage, the reaction temperature is 70-85 ℃; the reaction time is 50-85.
8. The method for synthesizing high-tap superfine cobaltosic oxide according to claim 1, wherein in the second stage, the ratio of the flow rate of the compressed air to the flow rate of the cobalt chloride is controlled to be (70-100): 1.
9. The method as claimed in claim 1, wherein in the second stage, the cobalt salt in the cobalt salt solution is at least one of cobalt chloride, cobalt sulfate and cobalt nitrate.
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| CN115745013A (en) * | 2022-11-18 | 2023-03-07 | 金川集团股份有限公司 | Preparation method of homogeneous phase high-aluminum-doped small-granularity cobaltosic oxide |
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| CN110255629A (en) * | 2019-07-05 | 2019-09-20 | 衢州华友钴新材料有限公司 | A kind of preparation method of ultra-fine grain diameter cobaltosic oxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115745013A (en) * | 2022-11-18 | 2023-03-07 | 金川集团股份有限公司 | Preparation method of homogeneous phase high-aluminum-doped small-granularity cobaltosic oxide |
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