CN112408499A - Method for synthesizing cobaltosic oxide by adopting high-pressure reaction - Google Patents
Method for synthesizing cobaltosic oxide by adopting high-pressure reaction Download PDFInfo
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Abstract
The invention discloses a method for synthesizing cobaltosic oxide by adopting high-pressure reaction, which comprises the following steps: preparing a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution; after the reaction kettle with the base solution is adjusted to the technological conditions of the synthesis reaction, adding a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution into the reaction kettle in a parallel flow mode under the stirring action to obtain cobaltosic oxide with the target particle size; the process conditions of the synthesis reaction are as follows: the reaction pressure is 0.1MPa to 1MPa, the reaction temperature is 50 ℃ to 80 ℃, the reaction pH is 9.0 to 11.0, the oxidation-reduction potential of the reaction is 35mv to 55mv, and the stirring speed of the reaction is 150r/min to 400 r/min; and sequentially aging, filtering, washing and drying the cobaltosic oxide with the target particle size to obtain cobaltosic oxide powder. The method has the advantages of simplified process, stable product quality and capability of directly synthesizing the required cobaltosic oxide.
Description
Technical Field
The invention belongs to the technical field of synthesis of cobaltosic oxide, and particularly relates to a method for synthesizing cobaltosic oxide by adopting a high-pressure reaction.
Background
In recent years, the market scale of new materials for Chinese batteries is rapidly increased, and the technology and the production process are continuously improved. From the market structure, the new Chinese battery material market mainly takes lithium battery materials and solar battery materials as main materials. Since the domestic fuel cell has been applied for a period of time before large-scale application, and domestic manufacturers have gaps with international levels in technology and production process, most domestic fuel cell materials are imported at present. In market segments, the lithium battery material industrial chain is relatively complete, and the lithium battery material has certain advantages in the aspect of material matching; the solar cell material market develops rapidly, the technology is continuously improved, and the market potential is huge; the preparation of fuel cell materials and the technical process need to be broken through.
The prior art for preparing cobaltosic oxide is mainly prepared by intermediate products of Co (Ac), CoC2O4、CoSO4、CoCl2、CoCO3The cobalt compounds are obtained by direct thermal decomposition at high temperature, and the above intermediates are mainly synthesized by a solution direct precipitation method, a colloid chemical method, a uniform precipitation method, a micro-emulsion method, a chemical precipitation-thermal decomposition method, a hydrothermal method and the like, but all have certain problems, mainly the stability of the synthesized intermediates is poor, the data fluctuation is large, the production of lithium cobaltate is unstable, and the performance of the battery is influenced.
Disclosure of Invention
Aiming at the problems of complex production process, higher cost and unstable process quality of the cobaltosic oxide in the prior art, the invention provides a method for synthesizing the cobaltosic oxide by adopting high-pressure reaction, which has the advantages of simplified process, stable product quality and capability of directly synthesizing the required cobaltosic oxide.
The invention adopts the following technical scheme:
a method for synthesizing cobaltosic oxide by adopting a high-pressure reaction, which is characterized by comprising the following steps:
(1) preparing a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution; the cobalt ion concentration in the cobalt chloride solution is 85-95 g/L, the mass percent concentration of the sodium hydroxide solution is 25-36%, and the mass percent concentration of the hydrogen peroxide solution is 20-30%;
(2) after the reaction kettle with the base solution is adjusted to the technological conditions of the synthesis reaction, adding a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution into the reaction kettle in a parallel flow mode under the stirring action to obtain cobaltosic oxide with the target particle size; the process conditions of the synthesis reaction are as follows: the reaction pressure is 0.1MPa to 1MPa, the reaction temperature is 50 ℃ to 80 ℃, the reaction pH is 9.0 to 11.0, the oxidation-reduction potential of the reaction is 35mv to 55mv, and the stirring speed of the reaction is 150r/min to 400 r/min;
(3) sequentially aging, filtering and washing the cobaltosic oxide with the target particle size to obtain a cobaltosic oxide wet material;
(4) and drying the cobaltosic oxide wet material to obtain cobaltosic oxide powder.
The method for synthesizing cobaltosic oxide by adopting high-pressure reaction is characterized in that the feeding flow rate of the cobalt chloride solution added into the reaction kettle in the step (2) is 110L/h-130L/h.
The method for synthesizing cobaltosic oxide by adopting high-pressure reaction is characterized in that the base solution in the step (2) is water, and the base solution accounts for 20-50% of the volume of the reaction kettle.
The method for synthesizing cobaltosic oxide by high pressure reaction according to the above, wherein the target particle size of the cobaltosic oxide having the target particle size in the step (2) is 2 to 6 μm.
The method for synthesizing cobaltosic oxide by adopting the high-pressure reaction is characterized in that in the step (4), the cobaltosic oxide wet material is dried at the temperature of 100-180 ℃.
The invention has the beneficial technical effects that: the method directly synthesizes the cobaltosic oxide by controlling the concentration of materials, the synthesized pH and temperature and the oxidation-reduction potential in the reaction process in a high-pressure reaction kettle, and shortens the production period of the cobaltosic oxide in the prior art from 5-10 days to 3-7 days; in addition, the invention simplifies the production process, omits the sintering procedure of the later section, shortens the production period, reduces the production cost and has stable product quality.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
Referring to fig. 1, the method for synthesizing cobaltosic oxide by using high pressure reaction according to the present invention comprises the following steps:
(1) preparing a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution; the cobalt ion concentration in the cobalt chloride solution is 85-95 g/L, the mass percent concentration of the sodium hydroxide solution is 25-36%, and the mass percent concentration of the hydrogen peroxide solution is 20-30%;
(2) after the reaction kettle with the base solution is adjusted to the technological conditions of the synthesis reaction, under the stirring action, a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution are added into the reaction kettle in a parallel flow mode, the feeding flow rate of the cobalt chloride solution into the reaction kettle is 110L/h-130L/h, the feeding flow rate of the sodium hydroxide solution into the reaction kettle is automatically regulated according to online pH detection, and the feeding flow rate of the hydrogen peroxide solution into the reaction kettle is automatically regulated according to online oxidation-reduction potential detection. Monitoring the growth condition in the reaction process, and directly synthesizing high-purity cobaltosic oxide with the target particle size; the target particle size of the cobaltosic oxide is 2 to 6 μm. The process conditions of the synthesis reaction are as follows: the reaction pressure is 0.1MPa to 1MPa, the reaction temperature is 50 ℃ to 80 ℃, the reaction pH is 9.0 to 11.0, the oxidation-reduction potential of the reaction is 35mv to 55mv, and the stirring speed of the reaction is 150r/min to 400 r/min; the bottom liquid is water, and the bottom liquid accounts for 20-50% of the volume of the reaction kettle.
(3) Allowing cobaltosic oxide with the target particle size to enter an aging kettle for aging, allowing the aged material to enter a centrifugal machine or a filter press for dehydration, and automatically washing the aged material. And (4) dewatering the washed qualified material in a flash evaporation dryer to obtain the cobaltosic oxide wet material.
(4) Drying the wet cobaltosic oxide material at 100-180 ℃ to obtain cobaltosic oxide powder.
Example 1
Preparing a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution; the cobalt ion concentration in the cobalt chloride solution is 85 +/-5 g/L, the mass percent concentration of the sodium hydroxide solution is 31.5-32.5%, and the mass percent concentration of the hydrogen peroxide solution is 29.5-30.5%;
adjusting the pressure of the reaction kettle with the base solution to 0.2-0.3 MPa, heating the reaction kettle to 65 +/-5 ℃, adjusting and controlling the pH value of a reaction system in the reaction kettle to 9.9 +/-0.2, the oxidation-reduction potential of the reaction system to 50 +/-5 mv, and the stirring speed of the reaction system to 260 +/-10 r/min. Under the stirring action, adding a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution into a reaction kettle in a parallel flow mode, wherein the feeding flow rate of the cobalt chloride solution into the reaction kettle is 110L/h-130L/h, the feeding flow rate of the sodium hydroxide solution into the reaction kettle is automatically regulated and controlled according to online pH detection, the feeding flow rate of the hydrogen peroxide solution into the reaction kettle is automatically regulated and controlled according to online oxidation-reduction potential detection, the growth condition in the reaction process is monitored, and the high-purity cobaltosic oxide with the target particle size of 5 +/-0.5 mu m is directly synthesized. The bottom liquid is water, and the bottom liquid accounts for 30 +/-5% of the volume of the reaction kettle.
Allowing cobaltosic oxide with the target particle size to enter an aging kettle for aging, allowing the aged material to enter a centrifugal machine or a filter press for dehydration, and automatically washing the aged material. And (4) dewatering the washed qualified material in a flash evaporation dryer to obtain the cobaltosic oxide wet material.
Drying the cobaltosic oxide wet material at the temperature of 170 +/-10 ℃ to obtain cobaltosic oxide powder.
Example 2
Preparing a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution; the cobalt ion concentration in the cobalt chloride solution is 85 +/-5 g/L, the mass percent concentration of the sodium hydroxide solution is 31.5-32.5%, and the mass percent concentration of the hydrogen peroxide solution is 29.5-30.5%;
adjusting the pressure of the reaction kettle with the base solution to 0.2-0.3 MPa, heating the reaction kettle to 65 +/-5 ℃, adjusting and controlling the pH value of a reaction system in the reaction kettle to 10.6 +/-0.2, the oxidation-reduction potential of the reaction system to 50 +/-5 mv, and the stirring speed of the reaction system to 320 +/-10 r/min. Under the stirring action, adding a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution into a reaction kettle in a parallel flow mode, wherein the feeding flow rate of the cobalt chloride solution into the reaction kettle is 110L/h-130L/h, the feeding flow rate of the sodium hydroxide solution into the reaction kettle is automatically regulated and controlled according to online pH detection, the feeding flow rate of the hydrogen peroxide solution into the reaction kettle is automatically regulated and controlled according to online oxidation-reduction potential detection, the growth condition in the reaction process is monitored, and the high-purity cobaltosic oxide with the target particle size of 3 +/-0.2 mu m is directly synthesized. The bottom liquid is water, and the bottom liquid accounts for 30 +/-5% of the volume of the reaction kettle.
Allowing cobaltosic oxide with the target particle size to enter an aging kettle for aging, allowing the aged material to enter a centrifugal machine or a filter press for dehydration, and automatically washing the aged material. And (4) dewatering the washed qualified material in a flash evaporation dryer to obtain the cobaltosic oxide wet material.
Drying the cobaltosic oxide wet material at the temperature of 170 +/-10 ℃ to obtain cobaltosic oxide powder.
Claims (5)
1. A method for synthesizing cobaltosic oxide by adopting a high-pressure reaction, which is characterized by comprising the following steps:
(1) preparing a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution; the cobalt ion concentration in the cobalt chloride solution is 85-95 g/L, the mass percent concentration of the sodium hydroxide solution is 25-36%, and the mass percent concentration of the hydrogen peroxide solution is 20-30%;
(2) after the reaction kettle with the base solution is adjusted to the technological conditions of the synthesis reaction, adding a cobalt chloride solution, a sodium hydroxide solution and a hydrogen peroxide solution into the reaction kettle in a parallel flow mode under the stirring action to obtain cobaltosic oxide with the target particle size; the process conditions of the synthesis reaction are as follows: the reaction pressure is 0.1MPa to 1MPa, the reaction temperature is 50 ℃ to 80 ℃, the reaction pH is 9.0 to 11.0, the oxidation-reduction potential of the reaction is 35mv to 55mv, and the stirring speed of the reaction is 150r/min to 400 r/min;
(3) sequentially aging, filtering and washing the cobaltosic oxide with the target particle size to obtain a cobaltosic oxide wet material;
(4) and drying the cobaltosic oxide wet material to obtain cobaltosic oxide powder.
2. The method for synthesizing cobaltosic oxide by high pressure reaction according to claim 1, wherein the feeding flow rate of the cobalt chloride solution into the reaction vessel in the step (2) is 110L/h to 130L/h.
3. The method for synthesizing cobaltosic oxide by high pressure reaction according to claim 2, wherein the bottom liquid in the step (2) is water, and the bottom liquid accounts for 20-50% of the volume of the reaction kettle.
4. The method for synthesizing cobaltosic oxide using high pressure reaction according to claim 2, wherein the cobaltosic oxide having the target particle size in the step (2) has a target particle size of 2 to 6 μm.
5. The method for synthesizing cobaltosic oxide by high pressure reaction according to claim 4, wherein the wet cobaltosic oxide is dried at 100-180 ℃ in the step (4).
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Citations (6)
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| CN1623908A (en) * | 2003-12-02 | 2005-06-08 | 财团法人工业技术研究院 | Process for low temp synthesis of tricobalt tetraoxide |
| CN101434417A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Dry preparation of battery grade spherical cobaltosic oxide particle |
| CN103145200A (en) * | 2013-03-25 | 2013-06-12 | 安徽亚兰德新能源材料股份有限公司 | Method for synthesizing spherical cobaltosic oxide through mixing type oxidation |
| CN107768646A (en) * | 2017-10-23 | 2018-03-06 | 兰州金川新材料科技股份有限公司 | A kind of cobaltosic oxide preparation method of doped chemical gradient distribution |
| CN108557904A (en) * | 2018-05-21 | 2018-09-21 | 兰州金川新材料科技股份有限公司 | A kind of gradient mixes the preparation method of aluminium cobaltosic oxide |
| CN111115704A (en) * | 2018-10-31 | 2020-05-08 | 格林美（江苏）钴业股份有限公司 | Preparation method of cobaltosic oxide |
-
2020
- 2020-11-09 CN CN202011242915.5A patent/CN112408499A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623908A (en) * | 2003-12-02 | 2005-06-08 | 财团法人工业技术研究院 | Process for low temp synthesis of tricobalt tetraoxide |
| CN101434417A (en) * | 2008-11-28 | 2009-05-20 | 宁波金和新材料有限公司 | Dry preparation of battery grade spherical cobaltosic oxide particle |
| CN103145200A (en) * | 2013-03-25 | 2013-06-12 | 安徽亚兰德新能源材料股份有限公司 | Method for synthesizing spherical cobaltosic oxide through mixing type oxidation |
| CN107768646A (en) * | 2017-10-23 | 2018-03-06 | 兰州金川新材料科技股份有限公司 | A kind of cobaltosic oxide preparation method of doped chemical gradient distribution |
| CN108557904A (en) * | 2018-05-21 | 2018-09-21 | 兰州金川新材料科技股份有限公司 | A kind of gradient mixes the preparation method of aluminium cobaltosic oxide |
| CN111115704A (en) * | 2018-10-31 | 2020-05-08 | 格林美（江苏）钴业股份有限公司 | Preparation method of cobaltosic oxide |
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