CN113200573A - Preparation method of hollow shell ball cobaltosic oxide - Google Patents
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- CN113200573A CN113200573A CN202110592773.3A CN202110592773A CN113200573A CN 113200573 A CN113200573 A CN 113200573A CN 202110592773 A CN202110592773 A CN 202110592773A CN 113200573 A CN113200573 A CN 113200573A
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Abstract
The invention relates to a preparation method of hollow shell sphere cobaltosic oxide, which comprises the following steps: step one, cobalt chloride is used as a raw material, and a cobalt solution is prepared as an A solution; preparing a sodium carbonate solution as a B solution; step two, adding the A, B solution into the reaction kettle in a cocurrent manner, and simultaneously introducing CO into the reaction kettle2The synthesis of cobalt carbonate is carried out under stirring of gas, and the flow rate of A, B solution and CO are strictly controlled in the synthesis process2Flow rate, reaction temperature, stirring intensity and reaction time; step three, after the synthesis reaction is finished, stopping adding liquid and introducing CO2And aging; step four, carrying out solid-liquid separation and washing on the synthesized product; step five, drying and sieving the washed synthetic product to obtain a hollow shell ball cobalt carbonate synthetic product; step six, calcining the hollow shell ball cobalt carbonate product and collecting; and step seven, sending the obtained product into a rotary cooler, and cooling to obtain a hollow shell ball cobaltosic oxide product. The invention provides a preparation method of hollow shell ball cobaltosic oxide, which has a simple and easily-controlled production process.
Description
Technical Field
The invention belongs to the technical field of material synthesis, and particularly relates to a preparation method of hollow shell sphere cobaltosic oxide.
Background
Well crystallized Co3O4Belong to AB2O4Spinel structure, Co3+Occupy octahedral sites, Co2+Occupies tetrahedral positions, wherein Co (II) ion tetrahedrons are surrounded by oxygen atoms and Co (III) ion octahedrons are also surrounded by oxygen atoms, and has higher crystal field stabilization energy. Co3O4The framework is a three-dimensional network which is beneficial to ion diffusion and has tetrahedron and octahedron which are coplanar, and oxygen atoms are tightly packed as cubic crystals.
Co3O4The lithium cobalt oxide is a functional material with special structure and performance, and is a main raw material for preparing the lithium cobalt oxide which is the anode material of the lithium ion battery in the battery industry. In addition, the material can also be applied to lithium ion battery cathode materials, supercapacitors, hard alloys, pressure sensitive ceramics, inorganic pigments, catalysts and the like.
At present, hollow Co3O4The synthesis method mainly comprises a template method, and commonly used templates comprise carbon spheres and SiO2Small spheres, polystyrene spheres, metal oxide particles and the like, and the removal of the template agent is very difficult and the steps are complicated. Still other template-free methods require the addition of organic surfactants, ionic liquids, etc., which increases costs. And the reaction is carried out at the high temperature of 700-1000 ℃ by adopting an atomization mode, the reaction condition is harsh, the control is not easy, and the requirement on equipment is higher. Therefore, a method for preparing the hollow shell sphere cobaltosic oxide is needed.
Disclosure of Invention
The invention aims to provide a preparation method of hollow shell sphere cobaltosic oxide, which aims to solve the problems of the prior art, such as the hollow Co3O4The synthesis method mainly comprises a template method, and commonly used templates comprise carbon spheres and SiO2The method has the advantages that the removal of the template agent is very difficult due to small balls, polystyrene small balls, metal oxide particles and the like, the steps are complex, organic surfactants, ionic liquids and the like are required to be added in some template-free methods, so that the cost is increased, the reaction is carried out at the high temperature of 700-1000 ℃ in an atomization mode, the reaction conditions are harsh, the control is not easy, and the requirement on equipment is high.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of hollow shell sphere cobaltosic oxide comprises the following steps:
step one, cobalt chloride is used as a raw material, and a cobalt solution is prepared as an A solution; preparing a sodium carbonate solution as a B solution;
step two, when the synthesis reaction starts, A, B solution is added into the reaction kettle in a cocurrent way, and CO is introduced into the reaction kettle in a certain way2The synthesis of cobalt carbonate was carried out under stirring with gas. The A, B solution flow and CO are strictly controlled in the synthesis process2Flow rate, reaction temperature, stirring intensity and reaction time;
step three, after the synthesis reaction is finished, stopping adding liquid and introducing CO2And aging;
step four, carrying out solid-liquid separation and washing on the synthetic product after ageing is finished;
step five, drying and sieving the washed synthetic product to obtain a hollow shell ball cobalt carbonate synthetic product;
step six, calcining and collecting the hollow shell ball cobalt carbonate product;
and step seven, sending the obtained product into a rotary cooler, and cooling to obtain a hollow shell ball cobaltosic oxide product.
Preferably, the cobalt concentration of the cobalt solution in the first step is 50-70 g/L, and the concentration of the sodium carbonate solution is 100-120 g/L.
Preference is given toThe reaction kettle in the second step is a 30L reaction kettle, and CO is introduced into the reaction kettle2The gas is introduced from the bottom of the reaction kettle, and A, B solution flow and CO are generated in the reaction process2The flow rate of the solution A, the flow rate of the solution B, the flow rate of the solution A, the flow rate of the solution B, the flow rate of the solution A, the flow rate of the solution B, the stirring intensity and the reaction time are 8-10 mL/min, 12-16 mL/min, and CO2The flow rate is 1-2L/min, the reaction temperature is 43-47 ℃, the stirring intensity is 240-260 r/min, and the reaction time is 16-18 h.
Preferably, the aging time in the third step is 0.5-1 h.
Preferably, the solid-liquid separation and washing equipment in the fourth step is a Buchner funnel, a suction filtration pump and a suction filtration bottle, and the washing materials are deionized water at 80-90 ℃.
Preferably, the device for drying the materials in the fifth step is an oven, the drying temperature is 80-90 ℃, and a 200-mesh screen is adopted for sieving.
Preferably, in the sixth step, the calcining condition is calcining in a box-type atmosphere furnace, the calcining temperature is 700-720 ℃, and the calcining time is 2-3 h.
Preferably, the cooling time of the rotary cooler in the seventh step is 5-10 min, and the rotating speed of the rotary cooler is 110-120 r/min.
Preferably, the physicochemical index of the hollow shell sphere cobaltosic oxide product in the seventh step is the laser particle size D50The tap density is 1.0-1.2 g/cm at 12-14 mu m3The specific surface area is 0.5 to 1.5m2The shape is a hollow shell sphere.
Compared with the prior art, the invention has the beneficial effects that: the preparation method of the hollow-shell spherical cobaltosic oxide is simple and easy to control on simple equipment, the equipment is simple, the process is simple and feasible, and the synthesis time is short.
Drawings
FIG. 1 is a schematic diagram of SEM detection results of a product prepared according to an embodiment of the invention;
FIG. 2 is a schematic diagram of SEM test results of a product prepared by the second embodiment of the invention;
FIG. 3 is a schematic diagram of SEM detection results of products prepared by the third embodiment of the invention;
FIG. 4 is a schematic process flow diagram of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-4, the present invention provides an embodiment:
a preparation method of hollow shell sphere cobaltosic oxide comprises the following steps:
step one, cobalt chloride is used as a raw material, and a cobalt solution is prepared as an A solution; preparing a sodium carbonate solution as a B solution;
step two, when the synthesis reaction starts, A, B solution is added into the reaction kettle in a cocurrent way, and CO is introduced into the reaction kettle in a certain way2The synthesis of cobalt carbonate was carried out under stirring with gas. The A, B solution flow and CO are strictly controlled in the synthesis process2Flow rate, reaction temperature, stirring intensity and reaction time;
step three, after the synthesis reaction is finished, stopping adding liquid and introducing CO2And aging;
step four, sending the aged synthetic product into a grinder for grinding, sieving the ground synthetic product, and filtering impurities in the synthetic product to obtain the synthetic product;
washing and drying the synthetic product obtained in the step four to obtain a hollow shell sphere cobalt carbonate synthetic product;
step six, calcining the hollow shell sphere cobalt carbonate product obtained in the step five, and collecting the calcined product;
and step seven, collecting the product obtained in the step six, sending the product into a rotary cooler, and cooling to obtain the hollow shell ball cobaltosic oxide product.
Further, the cobalt concentration of the cobalt solution in the first step is 50-70 g/L, and the concentration of the sodium carbonate solution is 100-120 g/L.
Further, the reaction kettle in the second step is a 30L reaction kettle, and CO is introduced into the reaction kettle2The gas mode is that gas is introduced from the bottom of the reaction kettle, and A, B solution flow and CO are generated in the reaction process2The flow rate, the reaction temperature, the stirring intensity and the flow rate of the solution A for reaction time are respectively 8-10 mL/min, the flow rate of the solution B is 12-16 mL/min, the flow rate of CO2 is 1-2L/min, the reaction temperature is 43-47 ℃, the stirring intensity is 240-260 r/min, and the reaction time is 16-18 h.
Further, the aging time in the third step is 0.5-1 h, a Buchner funnel is adopted for washing, deionized water at 80-90 ℃ is adopted for washing materials, an oven is adopted for drying materials, and the drying temperature is 80-90 ℃.
Further, the calcination condition in the sixth step is calcination in a box-type atmosphere furnace, the calcination temperature is 700-720 ℃, and the calcination time is 2-3 h.
Further, the materialization index of the hollow shell ball cobaltosic oxide product in the step seven is the laser granularity D50The particle size is 12-14 mu m, the tap density is 1.0-1.2 g/cm3, the specific surface area is 0.5-1.5 m2/g, and the shape is a hollow shell sphere.
Further, the stirring time in the fourth step is 5-10 min, and the rotating speed of the motor is 110-120 r/min.
The first embodiment is as follows:
step one, preparing a solution A with a cobalt solution of 70g/L by taking cobalt chloride as a raw material; preparing a B solution of 120g/L of sodium carbonate solution;
step two, when the synthesis reaction starts, A, B solution is added into a 30L reaction kettle in a cocurrent way, and CO is added at the same time2Introducing gas into the reaction kettle from the bottom of the reaction kettle at a certain flow rate, and carrying out wet cobalt carbonate synthesis under stirring, wherein the flow rate of the solution A is strictly controlled to be 8mL/min, the flow rate of the solution B is controlled to be 12mL/min, and CO is strictly controlled in the reaction process2The flow rate is 2L/min, the reaction temperature is 43 ℃, the stirring intensity is 260r/min, and the reaction time is 18 h;
step three, obtaining a synthetic product after the synthesis reaction is finished, taking out the material and beginning to age for 1 hour;
step four, sending the aged synthetic product into a grinder for grinding, sieving the ground synthetic product, and filtering impurities in the synthetic product to obtain the synthetic product;
step five, performing suction filtration and washing on the synthesized product by using a Buchner funnel, wherein deionized water with the temperature of 80 ℃ is adopted for washing materials, the device for drying the materials is an oven, and the drying temperature is 90 ℃ to obtain the hollow shell spherical cobalt carbonate;
step six, calcining the obtained hollow shell ball cobalt carbonate in a box-type atmosphere furnace, wherein the calcining temperature is 720 ℃, and the calcining time is 2 hours;
and step seven, collecting the product obtained in the step six, sending the product into a rotary cooler, and cooling to obtain the hollow shell ball cobaltosic oxide product.
The partial physicochemical indices of example 1 are given in the following table:
| Co（%） | Na+（%） | D50(μm) | TD(g/cm3) | BET(m2/g) |
| 73.29 | ≤0.002 | 12.6 | 1.19 | 0.89 |
the micro-morphology index of the prepared product is shown in figure 1.
Example two:
step one, preparing a cobalt solution A with the concentration of 60g/L by taking cobalt chloride as a raw material; preparing a B solution of a sodium carbonate solution of 110 g/L;
step two, when the synthesis reaction starts, A, B solution is added into a 30L reaction kettle in a cocurrent way, and CO is added at the same time2Introducing gas into the reaction kettle from the bottom of the reaction kettle at a certain flow rate, and carrying out wet cobalt carbonate synthesis under stirring, wherein the flow rate of the solution A is strictly controlled to be 9mL/min, the flow rate of the solution B is strictly controlled to be 13mL/min, and CO is strictly controlled in the reaction process2The flow rate is 1.5L/min, the reaction temperature is 45 ℃, the stirring intensity is 250 r/min, and the reaction time is 17 h;
step three, obtaining a synthetic product after the synthesis reaction is finished, taking out the material and beginning to age for 0.8 h;
step four, sending the aged synthetic product into a grinder for grinding, sieving the ground synthetic product, and filtering impurities in the synthetic product to obtain the synthetic product;
step five, performing suction filtration and washing on the synthesized product by using a Buchner funnel, wherein deionized water with the temperature of 85 ℃ is adopted for washing materials, the device for drying the materials is an oven, and the drying temperature is 85 ℃ to obtain the hollow shell spherical cobalt carbonate;
step six, calcining the obtained hollow shell ball cobalt carbonate in a box-type atmosphere furnace, wherein the calcining temperature is 710 ℃, and the calcining time is 2.5 hours;
and step seven, collecting the product obtained in the step six, sending the product into a rotary cooler, and cooling to obtain the hollow shell ball cobaltosic oxide product.
The partial physicochemical indices of example 2 are given in the following table:
the micro-morphology index of the prepared product is shown in figure 2.
Example three:
step one, preparing a solution A with a cobalt solution of 50g/L by taking cobalt chloride as a raw material; preparing a B solution of 100g/L of sodium carbonate solution;
step two, when the synthesis reaction starts, A, B solution is added into a 30L reaction kettle in a cocurrent way, and CO is added at the same time2Introducing gas into the reaction kettle from the bottom of the reaction kettle at a certain flow rate, and carrying out wet cobalt carbonate synthesis under stirring, wherein the flow rate of the solution A is strictly controlled to be 10mL/min, the flow rate of the solution B is strictly controlled to be 14mL/min, and CO is strictly controlled in the reaction process2The flow rate is 1.0L/min, the reaction temperature is 47 ℃, the stirring intensity is 240 r/min, and the reaction time is 16 h;
step three, obtaining a synthetic product after the synthesis reaction is finished, taking out the material and beginning to age for 0.5 h;
step four, sending the aged synthetic product into a grinder for grinding, sieving the ground synthetic product, and filtering impurities in the synthetic product to obtain the synthetic product;
step five, performing suction filtration and washing on the synthesized product by using a Buchner funnel, wherein deionized water at 90 ℃ is adopted for washing materials, equipment for drying the materials is an oven, and the drying temperature is 90 ℃ to obtain the hollow shell spherical cobalt carbonate;
step six, calcining the obtained hollow shell ball cobalt carbonate in a box-type atmosphere furnace, wherein the calcining temperature is 700 ℃, and the calcining time is 3 hours;
and step seven, collecting the product obtained in the step six, sending the product into a rotary cooler, and cooling to obtain the hollow shell ball cobaltosic oxide product.
The physicochemical indexes of the product part of example 3 are as follows in Table 2:
the micro-morphology index of the prepared product is shown in figure 3
By comparing the three preparation methods of the hollow shell ball cobaltosic oxide, the three preparation methods of the hollow shell ball cobaltosic oxide can obtain the hollow shell ball cobaltosic oxide product, wherein the processing production time of the third embodiment is shortest.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (9)
1. The preparation method of the hollow shell sphere cobaltosic oxide is characterized by comprising the following steps of:
step one, cobalt chloride is used as a raw material, and a cobalt solution is prepared as an A solution; preparing a sodium carbonate solution as a B solution;
step two, when the synthesis reaction starts, A, B solution is added into the reaction kettle in a cocurrent way, and CO is introduced into the reaction kettle in a certain way2The synthesis of cobalt carbonate is carried out under stirring of gas, and the flow rate of A, B solution and CO are strictly controlled in the synthesis process2Flow rate, reaction temperature, stirring intensity and reaction time;
step three, after the synthesis reaction is finished, stopping adding liquid and introducing CO2And aging;
step four, carrying out solid-liquid separation and washing on the synthetic product after ageing is finished;
step five, drying and sieving the washed synthetic product to obtain a hollow shell ball cobalt carbonate synthetic product;
step six, calcining and collecting the hollow shell ball cobalt carbonate product;
and step seven, sending the obtained product into a rotary cooler, and cooling to obtain a hollow shell ball cobaltosic oxide product.
2. The method for preparing the hollow shell sphere cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the cobalt concentration of the cobalt solution in the first step is 50-70 g/L, and the concentration of the sodium carbonate solution is 100-120 g/L.
3. A hollow shell sphere four as claimed in claim 1The preparation method of the cobaltosic oxide is characterized by comprising the following steps: the reaction kettle in the second step is a 30L reaction kettle, and CO is introduced into the reaction kettle2The gas is introduced from the bottom of the reaction kettle, and A, B solution flow and CO are generated in the reaction process2The flow rate of the solution A, the flow rate of the solution B, the flow rate of the solution A, the flow rate of the solution B, the flow rate of the solution A, the flow rate of the solution B, the stirring intensity and the reaction time are 8-10 mL/min, 12-16 mL/min, and CO2The flow rate is 1-2L/min, the reaction temperature is 43-47 ℃, the stirring intensity is 240-260 r/min, and the reaction time is 16-18 h.
4. The method for preparing the hollow shell sphere cobaltosic oxide according to claim 1, wherein the method comprises the following steps: the aging time in the third step is 0.5-1 h.
5. The method for preparing the hollow shell sphere cobaltosic oxide according to claim 1, wherein the method comprises the following steps: and the solid-liquid separation and washing equipment in the fourth step is a Buchner funnel, a suction filtration pump and a suction filtration bottle, and the washing materials are deionized water at the temperature of 80-90 ℃.
6. The method for preparing the hollow shell sphere cobaltosic oxide according to claim 1, wherein the method comprises the following steps: and fifthly, drying the materials by using an oven at the drying temperature of 80-90 ℃, and sieving by using a 200-mesh sieve.
7. The method for preparing the hollow shell sphere cobaltosic oxide according to claim 1, wherein the method comprises the following steps: in the sixth step, the calcining condition is calcining in a box-type atmosphere furnace, the calcining temperature is 700-720 ℃, and the calcining time is 2-3 h.
8. The preparation method of hollow shell sphere cobaltosic oxide as claimed in claim 1, wherein: and in the seventh step, the cooling time of the rotary cooler is 5-10 min, and the rotating speed of the rotary cooler is 110-120 r/min.
9. According to the claimsThe preparation method of the hollow shell sphere cobaltosic oxide according to claim 1 is characterized by comprising the following steps: the materialization index of the hollow shell ball cobaltosic oxide product in the step seven is the laser granularity D50The tap density is 1.0-1.2 g/cm at 12-14 mu m3The specific surface area is 0.5 to 1.5m2The shape is a hollow shell sphere.
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