CN109205684B - Preparation method of small-particle-size cobaltosic oxide - Google Patents
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- CN109205684B CN109205684B CN201811076694.1A CN201811076694A CN109205684B CN 109205684 B CN109205684 B CN 109205684B CN 201811076694 A CN201811076694 A CN 201811076694A CN 109205684 B CN109205684 B CN 109205684B
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Abstract
The invention discloses a preparation method of small-particle-size cobaltosic oxide, which is used for preparing small-particle-size cobaltosic oxide with a certain concentrationThe method comprises the steps of adding a certain amount of cobalt hydroxide flash evaporation drying dust collection material into a reaction kettle before synthesis begins, then carrying out synthesis reaction in the reaction kettle, wherein the cobalt hydroxide flash evaporation drying dust collection material prevents the growth of a synthesized product during the synthesis reaction, further controlling the product granularity, adding a certain amount of conductive carbon black into the reaction kettle after the synthesis reaction is finished, aging for a period of time, filtering, washing and drying the material to obtain a small-granularity cobaltosic oxide precursor product, and calcining the cobaltosic oxide precursor product to obtain the small-granularity cobaltosic oxide product. By the preparation method, the laser particle size of 3-5 mu m, the tap density of more than 2.0g/cm3, and the specific surface area of 1.0-3.0m can be easily and simply prepared2A spherical or spheroidal cobaltosic oxide product per gram.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a preparation method of small-particle-size 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 is Co with conventional grain size (6-10 microns)3O4The market has faced the current situation of progressive atrophy, small particle size Co3O4The market demand is gradually highlighted. It has become a hot spot to study how to prepare high-performance small-particle size cobaltosic oxide. The existing method for preparing the small-granularity cobaltosic oxide has complex process and is difficult to realize.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a preparation method of small-granularity cobaltosic oxide, which has the advantages of simple and easily-controlled production process, low production cost and high metal material direct yield in the production process.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of small-particle size cobaltosic oxide comprises the following steps:
a. preparing liquid: preparing a cobalt solution with the cobalt concentration of 1-2mol/L, namely an A solution, by taking cobalt salt as a raw material; preparing a mixed solution of sodium hydroxide and ammonia water, namely a solution B, wherein the concentration of the sodium hydroxide solution is 2-6mol/L, the concentration of the ammonia water solution is 5-10mol/L, and the volume ratio of the ammonia water solution to the sodium hydroxide solution in the mixed solution is 0.05-0.1; preparing hydrogen peroxide solution with the concentration of 5-10mol/L, namely C solution;
b. and (3) synthesis reaction: adding cobalt hydroxide flash evaporation drying dust collection materials into a reaction kettle before the synthetic reaction, then adding the solution A, the solution B and the solution C into the reaction kettle in a parallel flow manner, and carrying out the synthetic reaction under strong stirring;
c. aging: after the synthesis is finished, adding conductive carbon black into the reaction kettle, and aging under strong stirring;
d. filtering, washing and drying: after the aging process is finished, filtering, washing and drying the material to obtain a small-granularity cobaltosic oxide precursor product;
e. and (3) calcining: and calcining the small-granularity cobaltosic oxide precursor product to obtain the small-granularity cobaltosic oxide product.
Further, in the step a, the cobalt salt is one or a mixture of cobalt sulfate, cobalt nitrate and cobalt chloride.
Further, the addition amount of the cobalt hydroxide flash evaporation drying dust collection material in the step b is 30% of the mass of the cobalt in the solution A.
Further, the flow rate of the solution A in the step b is 300L/h, the flow rate of the solution C is 0.1-0.2 time of the flow rate of the solution A, the reaction temperature is 70-80 ℃, the reaction pH value is 8.0-9.0, the stirring intensity is 200-500 r/min, and the reaction time is 15-20 h.
Furthermore, the adding amount of the conductive carbon black in the step c is 5 percent of the mass of the cobalt in the solution A, the aging time is 1-2h, and the stirring intensity is 200-.
Furthermore, deionized water with the temperature of 80-100 ℃ is adopted as the washing material in the step d, and the washing equipment is a suction filtration cylinder.
Further, the temperature of the drying material in the step d is 100-150 ℃, and the drying equipment is a disc type dryer.
And further, calcining in a pusher furnace in the calcining step e, wherein the calcining temperature is 400-500 ℃, and the calcining time is 1-2 h.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method of small-granularity cobaltosic oxide comprises the steps of taking a cobalt solution with a certain concentration as a cobalt source, taking a sodium hydroxide solution as a precipitator, taking an ammonia water solution as a complexing agent, taking a hydrogen peroxide solution as an oxidant, adding a certain amount of cobalt hydroxide flash evaporation drying dust collection material into a reaction kettle before synthesis starts, then carrying out synthesis reaction in the reaction kettle, wherein during the synthesis reaction, the cobalt hydroxide flash evaporation drying dust collection material prevents the growth of a synthesized product, further controlling the granularity of the product, adding a certain amount of conductive carbon black into the reaction kettle after the synthesis reaction is finished, aging for a period of time, filtering, washing and drying the material to obtain a small-granularity cobaltosic oxide precursor product, and calcining the small-granularity cobaltosic oxide precursor product to obtain the small-granularity cobaltosic oxide product. By the preparation method, the laser particle size of 3-5 mu m, the tap density of more than 2.0g/cm3, and the specific surface area of 1.0-3.0m can be easily and simply prepared2A spherical or spheroidal cobaltosic oxide product per gram. Meanwhile, the cobalt hydroxide flash evaporation drying dust collection material is used as a raw material, dust collection waste generated by cobalt hydroxide flash evaporation is changed into valuable, the direct recovery rate of metal materials in the production process of the cobaltosic oxide product is improved, and the production cost is saved.
2. The invention adds the conductive graphite in the aging stage to uniformly mix the conductive graphite and the synthesized product, greatly improves the washing performance of the synthesized product due to the high water permeability of the conductive graphite, and solves the problem that the small-granularity product synthesized by a wet method is difficult to wash due to small granularity. And, by adding the conductive graphite in the aging stage, the chloride content or sulfate content of the synthesized product can be easily washed to be less than 0.01%. In addition, a large amount of heat can be released by burning the conductive graphite, and the conductive graphite is added into a synthesized product, so that the calcining temperature can be reduced, and the calcining time can be shortened. And the conductive graphite burns to release carbon dioxide gas, so that the cobaltosic oxide product prepared by calcination has good fluidity, the phenomenon of hardening can not occur, and the product index is improved.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a microscopic morphology of the cobalt hydroxide flash dried dust collection material of the present invention;
FIG. 3 is an SEM photograph of the final product of example 1 of the present invention;
FIG. 4 is an SEM photograph of the final product of example 2 of the present invention;
FIG. 5 is an SEM photograph of the final product of example 3 of the present invention.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
Example 1
a. Preparing liquid: preparing a cobalt chloride solution with the cobalt concentration of 1mol/L, namely a solution A; preparing a mixed solution of sodium hydroxide and ammonia water, namely a solution B, wherein the concentration of the sodium hydroxide solution is 2mol/L, the concentration of the ammonia water solution is 5mol/L, and the volume ratio of the ammonia water solution to the sodium hydroxide solution in the mixed solution is 0.05; preparing hydrogen peroxide solution with the concentration of 5mol/L, namely C solution.
b. And (3) synthesis reaction: adding cobalt hydroxide with the mass of 30% of that of cobalt in the solution A into a reaction kettle before the synthetic reaction, carrying out flash evaporation drying and dust collection, then simultaneously adding the solution A, the solution B and the solution C into the reaction kettle in a parallel flow manner, carrying out the synthetic reaction under strong stirring, controlling the flow rate of the solution A to be 300L/h, controlling the flow rate of the solution C to be 0.1 time of the flow rate of the solution A, controlling the reaction temperature to be 70 ℃, the reaction pH value to be 9.0, controlling the stirring intensity to be 200 revolutions per minute, controlling the reaction time to be 15h, and adjusting the flow rate of the solution B according to the reaction pH value.
c. Aging: after the synthesis is finished, adding conductive carbon black with the mass of 5% of the cobalt in the solution A into the reaction kettle, and aging under strong stirring for 1h with the stirring intensity of 200 r/min.
d. Filtering, washing and drying: and after the aging process is finished, filtering the material, washing the filtered material in a suction filtration cylinder by using 80 ℃ deionized water, drying the washed material by using a disc type dryer at the drying temperature of 100 ℃ to obtain a small-granularity cobaltosic oxide precursor product.
e. And (3) calcining: and (3) putting the small-granularity cobaltosic oxide precursor product into a push boat furnace for calcination, wherein the calcination temperature is 400 ℃, and the calcination time is 1h, so as to obtain the small-granularity cobaltosic oxide product. The prepared product index is shown in table 1.
TABLE 1 physicochemical index of Cobaltosic oxide prepared in example 1
As can be seen from Table 1, the laser particle size of 3-5 mu m and the tap density of more than 2.0g/cm can be prepared by the method3Specific surface area of 1.0-3.0m2The cobalt content is more than 72.5 percent and the chloride content is less than 0.01 percent.
Example 2
a. Preparing liquid: preparing a cobalt sulfate solution with the cobalt concentration of 1.5mol/L, namely a solution A; preparing a mixed solution of sodium hydroxide and ammonia water, namely a solution B, wherein the concentration of the sodium hydroxide solution is 4mol/L, the concentration of the ammonia water solution is 8mol/L, and the volume ratio of the ammonia water solution to the sodium hydroxide solution in the mixed solution is 0.08; preparing hydrogen peroxide solution with the concentration of 8mol/L, namely C solution.
b. And (3) synthesis reaction: adding cobalt hydroxide with the mass of 30% of that of cobalt in the solution A into a reaction kettle before the synthetic reaction, carrying out flash evaporation drying and dust collection on the cobalt hydroxide, then simultaneously adding the solution A, the solution B and the solution C into the reaction kettle in a parallel flow manner, carrying out the synthetic reaction under strong stirring, controlling the flow rate of the solution A to be 300L/h, controlling the flow rate of the solution C to be 0.15 times of that of the solution A, controlling the reaction temperature to be 75 ℃, the reaction pH value to be 8.5, controlling the stirring intensity to be 350 r/min, controlling the reaction time to be 18h, and adjusting the flow rate of the solution B according to the reaction pH value.
c. Aging: after the synthesis is finished, conductive carbon black with the mass of 5% of that of the cobalt in the solution A is added into the reaction kettle, and the mixture is aged under strong stirring, wherein the aging time is 1.5h, and the stirring intensity is 350 r/min.
d. Filtering, washing and drying: and after the aging process is finished, filtering the material, washing the filtered material in a suction filtration cylinder by using deionized water at 90 ℃, drying the washed material by using a disc type dryer at the drying temperature of 150 ℃, and drying to obtain a small-granularity cobaltosic oxide precursor product.
e. And (3) calcining: and (3) putting the small-granularity cobaltosic oxide precursor product into a push boat furnace for calcination at the temperature of 450 ℃ for 1.5h to obtain the small-granularity cobaltosic oxide product. The prepared product index is shown in table 2.
TABLE 2 physicochemical indices of Cobaltosic oxide prepared in example 2
As can be seen from Table 2, the laser particle size of 3-5 mu m and the tap density of more than 2.0g/cm can be prepared by the method3Specific surface area of 1.0-3.0m2The cobalt content is more than 72.5 percent and the chloride content is less than 0.01 percent.
Example 3
a. Preparing liquid: preparing a cobalt nitrate solution with the cobalt concentration of 2mol/L, namely a solution A; preparing a mixed solution of sodium hydroxide and ammonia water, namely a solution B, wherein the concentration of the sodium hydroxide solution is 6mol/L, the concentration of the ammonia water solution is 10mol/L, and the volume ratio of the ammonia water solution to the sodium hydroxide solution in the mixed solution is 0.1; preparing hydrogen peroxide solution with the concentration of 10mol/L, namely C solution.
b. And (3) synthesis reaction: adding cobalt hydroxide with the mass of 30% of that of cobalt in the solution A into a reaction kettle before the synthetic reaction, carrying out flash evaporation drying and dust collection, then simultaneously adding the solution A, the solution B and the solution C into the reaction kettle in a parallel flow manner, carrying out the synthetic reaction under strong stirring, controlling the flow rate of the solution A to be 300L/h, controlling the flow rate of the solution C to be 0.2 times of the flow rate of the solution A, controlling the reaction temperature to be 80 ℃, the reaction pH value to be 8.0, controlling the stirring intensity to be 500 r/min, controlling the reaction time to be 20h, and adjusting the flow rate of the solution B according to the reaction pH value.
c. Aging: after the synthesis is finished, adding conductive carbon black with the mass of 5% of the cobalt in the solution A into the reaction kettle, and aging under strong stirring for 2h with the stirring intensity of 500 r/min.
d. Filtering, washing and drying: and after the aging process is finished, filtering the material, washing the filtered material in a suction filtration cylinder by using 100 ℃ deionized water, drying the washed material by using a disc type dryer at the drying temperature of 120 ℃ to obtain a small-granularity cobaltosic oxide precursor product.
e. And (3) calcining: and (3) putting the small-granularity cobaltosic oxide precursor product into a push boat furnace for calcination, wherein the calcination temperature is 500 ℃, and the calcination time is 2 hours, so as to obtain the small-granularity cobaltosic oxide product. The prepared product index is shown in table 3.
TABLE 3 physicochemical indices of Cobaltosic oxide prepared in example 3
As can be seen from Table 3, the laser particle size of 3-5 mu m and the tap density of more than 2.0g/cm can be prepared by the method3Specific surface area of 1.0-3.0m2The cobalt content is more than 72.5 percent and the chloride content is less than 0.01 percent.
Claims (7)
1. A preparation method of small-particle-size cobaltosic oxide is characterized by comprising the following steps of:
a. preparing liquid: preparing a cobalt solution with the cobalt concentration of 1-2mol/L, namely an A solution, by taking cobalt salt as a raw material; preparing a mixed solution of sodium hydroxide and ammonia water, namely a solution B, wherein the concentration of the sodium hydroxide solution is 2-6mol/L, the concentration of the ammonia water solution is 5-10mol/L, and the volume ratio of the ammonia water solution to the sodium hydroxide solution in the mixed solution is 0.05-0.1; preparing hydrogen peroxide solution with the concentration of 5-10mol/L, namely C solution;
b. and (3) synthesis reaction: adding cobalt hydroxide into a reaction kettle for flash evaporation drying and dust collection before the synthetic reaction, then simultaneously adding the solution A, the solution B and the solution C into the reaction kettle in a parallel flow manner, and carrying out the synthetic reaction under strong stirring, wherein the flow rate of the solution A is 300L/h, the flow rate of the solution C is 0.1-0.2 times of the flow rate of the solution A, the reaction temperature is 70-80 ℃, the reaction pH value is 8.0-9.0, the stirring intensity is 200 plus materials and 500 revolutions per minute, and the reaction time is 15-20 h;
c. aging: after the synthesis is finished, adding conductive carbon black into the reaction kettle, and aging under strong stirring;
d. filtering, washing and drying: after the aging process is finished, filtering, washing and drying the material to obtain a small-granularity cobaltosic oxide precursor product;
e. and (3) calcining: and calcining the small-granularity cobaltosic oxide precursor product to obtain the small-granularity cobaltosic oxide product.
2. The method for preparing small-particle size cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step a, the cobalt salt is one or a mixture of cobalt sulfate, cobalt nitrate or cobalt chloride.
3. The method for preparing small-particle size cobaltosic oxide according to claim 1, wherein the method comprises the following steps: and the addition amount of the cobalt hydroxide flash evaporation drying dust collection material in the step b is 30% of the mass of the cobalt in the solution A.
4. The method for preparing small-particle size cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the adding amount of the conductive carbon black in the step c is 5 percent of the mass of the cobalt in the solution A, the aging time is 1-2h, and the stirring strength is 200-500 r/min.
5. The method for preparing small-particle size cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the step d, deionized water with the temperature of 80-100 ℃ is adopted as washing materials, and a washing device is a suction filtration cylinder.
6. The method for preparing small-particle size cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the temperature of the drying material in the step d is 100-150 ℃, and the drying equipment is a disc type dryer.
7. The method for preparing small-particle size cobaltosic oxide according to claim 1, wherein the method comprises the following steps: and e, calcining in a pusher furnace during calcining in the step e, wherein the calcining temperature is 400-500 ℃, and the calcining time is 1-2 h.
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| CN113215404B (en) * | 2021-04-20 | 2022-05-13 | 北京科技大学 | Method for preparing spherical cobaltosic oxide from cobalt-ammonia complex solution |
| CN113277569A (en) * | 2021-05-28 | 2021-08-20 | 金川集团股份有限公司 | Preparation method of wide-radius distance cobaltosic oxide |
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| CN103359794A (en) * | 2012-03-30 | 2013-10-23 | 北京当升材料科技股份有限公司 | Spherical cobaltosic oxide and preparation method thereof |
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| CN108483512A (en) * | 2018-04-03 | 2018-09-04 | 兰州金川新材料科技股份有限公司 | A kind of preparation method of big granularity cobaltosic oxide |
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Patent Citations (6)
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| JPH08208238A (en) * | 1995-02-02 | 1996-08-13 | Kiyoyuki Hagita | Cobalt monoxide |
| CN103359794A (en) * | 2012-03-30 | 2013-10-23 | 北京当升材料科技股份有限公司 | Spherical cobaltosic oxide and preparation method thereof |
| CN106335930A (en) * | 2016-08-16 | 2017-01-18 | 安徽师范大学 | Porous spherical cobaltosic oxide electrode material and preparation method and application thereof |
| CN107819125A (en) * | 2017-11-02 | 2018-03-20 | 济南大学 | A kind of preparation method of straw bundle shape cobaltosic oxide and its application in lithium ion battery |
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Effective date of registration: 20201203 Address after: No.9, Xinkai South Road, development zone, Nantong City, Jiangsu Province, 226000 Patentee after: NANTONG KINGTON ENERGY STORAGE POWER NEW MATERIAL Co.,Ltd. Address before: 730101 Jinchuan science and Technology Park, Heping Economic Development Zone, Gansu, Lanzhou Patentee before: LANZHOU JINCHUAN ADVANGCED MATERIALS TECHNOLOGY Co.,Ltd. |