CN115784319B - Spherical cobalt carbonate particles and preparation method thereof - Google Patents
Spherical cobalt carbonate particles and preparation method thereof Download PDFInfo
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Abstract
The invention relates to spherical cobalt carbonate particles and a preparation method thereof, and belongs to the technical field of cobalt carbonate particle preparation, wherein the cobalt carbonate particles comprise the following raw materials: cobalt chloride hexahydrate, sodium bicarbonate, polyvinylpyrrolidone, ultrapure water, ethylene glycol and sericin; the preparation method of the spherical cobalt carbonate particles comprises the steps of (1) preparing a material to be aged; (2) preparing a material to be dried; (3) preparation of cobalt carbonate particles. According to the invention, sericin is used as a regulating agent, polyvinylpyrrolidone is added, and cobalt carbonate particles are guided to form into spheres; the preparation process is improved, in the preparation of the material to be dried, ultrapure water is firstly used for ultrasonic washing and then ethanol is used for washing, so that the agglomeration of the precipitate is helped to be destroyed; carbon dioxide gas is introduced to make the cobalt carbonate particles form more stable. The spherical cobalt carbonate with the particle diameter D50 of 6.0+/-0.2 mu m can be prepared by the method and is applied to the industries of cobalt salt production, magnetic materials, batteries and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of cobalt carbonate particles, and particularly relates to spherical cobalt carbonate particles and a preparation method thereof.
Background
Cobalt carbonate is widely used in the industries of cobalt salt production, catalysts, nickel-hydrogen battery additives, camouflage paint, chemical temperature indicators, feeds, ceramics and the like. Along with the continuous increase of the economy in China, particularly the rapid development of the communication industry in China in recent years, the demands of industries such as electroplating, catalysts, hard alloy, magnetic materials, batteries and the like on cobalt resources are continuously increased, cobalt carbonate is gradually known by the public, and therefore, the quality requirements of people are also higher and higher.
At present, when a plurality of factories prepare cobalt carbonate, the situation of severe local reaction of a system exists, and the prepared cobalt carbonate has different morphology and serious agglomeration of cobalt carbonate particles, which is not beneficial to producing more stable and high-quality products. Therefore, the cobalt carbonate particles with the spherical morphology are prepared, and particularly the spherical cobalt carbonate particles with uniform morphology and excellent dispersion performance can be prepared, so that the cobalt carbonate particles have practical significance and practical value.
Disclosure of Invention
The invention aims to provide spherical cobalt carbonate particles and a preparation method thereof, wherein sericin is used as a regulating agent, polyvinylpyrrolidone is added, interaction between sericin molecules and cobalt ions is enhanced, and the cobalt carbonate particles are guided to form into spheres; the preparation process is improved, in the preparation of the material to be dried, ultrapure water is firstly used for ultrasonic washing and then ethanol is used for washing, so that the agglomeration of the precipitate is destroyed, and the precipitate particles are better dispersed; in the preparation of the material to be aged and the material to be dried, carbon dioxide gas is introduced to help the formation of the cobalt carbonate particles, so that the morphology of the cobalt carbonate particles is more stable, and the problems of non-uniform morphology and serious particle agglomeration of the cobalt carbonate particles in the prior art are solved.
The aim of the invention can be achieved by the following technical scheme:
the spherical cobalt carbonate particles comprise the following raw materials in parts by weight:
further, the preparation method of the spherical cobalt carbonate particles comprises the following steps:
(1) Preparing a material to be aged: mixing cobalt chloride hexahydrate and 30% of ultrapure water according to a formula, heating to 80-90 ℃ to obtain a standby liquid A, mixing sodium bicarbonate and 30% of ultrapure water according to the formula, heating to 80-90 ℃ to obtain a standby liquid B, slowly pouring the standby liquid A, the standby liquid B and 80% of ethylene glycol into a high-pressure reaction kettle while stirring, adding the formula of polyvinylpyrrolidone and sericin into the high-pressure reaction kettle, introducing carbon dioxide gas, regulating the rotation speed of a stirrer in the high-pressure reaction kettle, stirring, starting a cooling water protection device in the high-pressure reaction kettle, regulating the temperature of the high-pressure reaction kettle, and carrying out heat preservation reaction to obtain a material to be aged;
(2) Preparing materials to be dried: placing the material to be aged prepared in the step (1) in an oven for temperature control and aging to obtain a precipitate, adding the rest ultrapure water into the precipitate under the carbon dioxide environment, ultrasonically washing, performing vacuum suction filtration to obtain a suction filtration substance, introducing carbon dioxide gas into the suction filtration substance, and stirring and washing with the rest of ethylene glycol in the formula amount to obtain the material to be dried;
(3) Preparation of cobalt carbonate particles: and (3) drying the material to be dried, which is prepared in the step (2), at a controlled temperature to obtain cobalt carbonate particles.
The cobalt carbonate is aged and washed under the condition of introducing carbon dioxide gas, so that the crystal form of the cobalt carbonate is more stable, and the carbon dioxide exists in the form of carbonate radical in water, thereby being beneficial to the crystallization of the cobalt carbonate.
Further, the rotation speed of the stirrer in the high-pressure reaction kettle in the step (1) is 250-310rmp, and the stirring time is 40-60min.
Further, the autoclave temperature in step (1) is 220-250 ℃.
Further, the incubation reaction time in step (1) is 7-9h.
Further, in the step (2), the temperature in the oven is controlled, the aging temperature is 110-115 ℃, and the aging time is 14-16h.
Further, the ultrasonic washing time in the step (2) is 10-12min.
Further, the stirring and washing time in the step (2) is 12-15min.
Further, in the step (3), the temperature control and drying temperature is 85-90 ℃ and the drying time is 10-11h.
The invention has the beneficial effects that:
(1) According to the invention, sericin is used as a regulating agent, polyvinylpyrrolidone is added, carbonyl bonds in the polyvinylpyrrolidone play a role of a bridge, cobalt ions are attracted from all directions, so that interaction between sericin molecules and the cobalt ions is enhanced, meanwhile, because sericin molecular chains can generate asymmetric and three-dimensional extensibility processes such as irregular curling or folding, the polyvinylpyrrolidone is adsorbed on the surfaces of cobalt carbonate particles, adjacent cobalt carbonate particles are guided by the sericin, the sericin molecular chains can be copied, the spontaneous assembly is carried out for orientation connection, and thus the cobalt carbonate particles are guided to form into spheres.
(2) The spherical cobalt carbonate particles are prepared through specific preparation sequences and reaction conditions, the used instruments are common, and the preparation method is simple.
(3) In the preparation of the material to be aged, carbon dioxide gas is introduced, and the carbon dioxide exists in the form of carbonate radical in water, so that the formation of cobalt carbonate particles is facilitated; and carbon dioxide gas is introduced in the preparation of the material to be dried for ageing and washing, so that the cobalt carbonate particles are more stable in shape.
(4) In the preparation of the material to be dried, ultra-pure water is firstly used for ultrasonic washing and then ethanol is used for washing. The ultrasonic washing is helpful for destroying the secondary agglomeration of the precipitate, better dispersing the precipitate particles, and then washing with ethanol, so that the water adsorbed on the surface of the particles is replaced by ethanol, the particle environment is improved, and meanwhile, the agglomeration is inhibited and the dispersion performance is improved.
(5) The spherical cobalt carbonate with the particle diameter D50 of 6.0+/-0.2 mu m can be prepared by the method, and the product has high sphericity and stable morphology, can be widely applied to industries such as cobalt salt production, catalysts, nickel-hydrogen battery additives, chemical temperature indicators, magnetic materials, batteries and the like, and has important practical significance and practical value.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in example 3 of the present invention;
FIG. 2 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 2 of the present invention;
FIG. 4 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 3 of the present invention;
FIG. 5 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 4 of the present invention;
FIG. 6 is a graph showing the particle size distribution of spherical cobalt carbonate particles prepared in example 3 of the present invention;
FIG. 7 is a particle size distribution diagram of spherical cobalt carbonate particles prepared in comparative example 1 of the present invention;
FIG. 8 is a particle size distribution diagram of spherical cobalt carbonate particles prepared in comparative example 2 of the present invention;
FIG. 9 is a particle size distribution diagram of spherical cobalt carbonate particles prepared in comparative example 3 of the present invention;
FIG. 10 is a particle size distribution diagram of spherical cobalt carbonate particles prepared in comparative example 4 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The spherical cobalt carbonate particles comprise the following raw materials in parts by weight:
the preparation method of the spherical cobalt carbonate particles comprises the following steps:
(1) Preparing a material to be aged: mixing cobalt chloride hexahydrate and 30% of ultrapure water according to a formula, heating to 85 ℃ to obtain a standby liquid A, mixing sodium bicarbonate and 30% of ultrapure water according to the formula, heating to 85 ℃ to obtain a standby liquid B, slowly pouring the standby liquid A, the standby liquid B and 80% of ethylene glycol according to the formula into a high-pressure reaction kettle while stirring, adding polyvinylpyrrolidone and sericin according to the formula into the high-pressure reaction kettle, screwing a cover of the high-pressure reaction kettle, introducing carbon dioxide gas into the high-pressure reaction kettle, adjusting the rotating speed of a stirrer in the high-pressure reaction kettle to 250rmp, stirring for 40min, starting a cooling water protection device in the high-pressure reaction kettle, adjusting the temperature of the high-pressure reaction kettle to 220 ℃, and carrying out heat preservation reaction for 7h to obtain a material to be aged;
(2) Preparing materials to be dried: placing the material to be aged prepared in the step (1) in an oven, controlling the temperature to be 110 ℃, aging for 14 hours to obtain a precipitate, adding the rest ultrapure water into the precipitate under the carbon dioxide environment, washing for 10 minutes by ultrasonic waves, performing vacuum suction filtration to obtain a suction-filtered material, introducing carbon dioxide gas into the suction-filtered material, and stirring and washing for a small amount of times by using the rest of the ethylene glycol in the formula amount, and performing vacuum suction filtration to obtain the material to be dried;
(3) Preparation of cobalt carbonate particles: and (3) controlling the temperature of the material to be dried, which is prepared in the step (2), to be 85 ℃ and drying for 10 hours to obtain cobalt carbonate particles.
Example 2
The spherical cobalt carbonate particles comprise the following raw materials in parts by weight:
the preparation method of the spherical cobalt carbonate particles comprises the following steps:
(1) Preparing a material to be aged: mixing cobalt chloride hexahydrate and 30% of ultrapure water according to a formula, heating to 85 ℃ to obtain a standby liquid A, mixing sodium bicarbonate and 30% of ultrapure water according to the formula, heating to 85 ℃ to obtain a standby liquid B, slowly pouring the standby liquid A, the standby liquid B and 80% of ethylene glycol according to the formula into a high-pressure reaction kettle while stirring, adding polyvinylpyrrolidone and sericin according to the formula into the high-pressure reaction kettle, screwing a cover of the high-pressure reaction kettle, introducing carbon dioxide gas into the high-pressure reaction kettle, adjusting the rotating speed of a stirrer in the high-pressure reaction kettle to 280rmp, stirring for 50min, starting a cooling water protection device in the high-pressure reaction kettle, adjusting the temperature of the high-pressure reaction kettle to 235 ℃, and carrying out heat preservation reaction for 8h to obtain a material to be aged;
(2) Preparing materials to be dried: placing the material to be aged prepared in the step (1) in an oven, controlling the temperature to be 113 ℃, aging for 15 hours to obtain a precipitate, adding the rest ultrapure water into the precipitate under the carbon dioxide environment, washing for 11 minutes by ultrasonic waves, performing vacuum suction filtration to obtain a suction-filtered material, introducing carbon dioxide gas into the suction-filtered material, and stirring and washing for a small amount of times by using the rest of the ethylene glycol in the formula amount, and performing vacuum suction filtration to obtain the material to be dried;
(3) Preparation of cobalt carbonate particles: and (3) controlling the temperature of the material to be dried, which is prepared in the step (2), to be 87 ℃ and drying for 10.5 hours to obtain cobalt carbonate particles.
Example 3
The spherical cobalt carbonate particles comprise the following raw materials in parts by weight:
the preparation method of the spherical cobalt carbonate particles comprises the following steps:
(1) Preparing a material to be aged: mixing cobalt chloride hexahydrate and 30% of ultrapure water according to a formula, heating to 85 ℃ to obtain a standby liquid A, mixing sodium bicarbonate and 30% of ultrapure water according to the formula, heating to 85 ℃ to obtain a standby liquid B, slowly pouring the standby liquid A, the standby liquid B and 80% of ethylene glycol according to the formula into a high-pressure reaction kettle while stirring, adding polyvinylpyrrolidone and sericin according to the formula into the high-pressure reaction kettle, screwing a cover of the high-pressure reaction kettle, introducing carbon dioxide gas into the high-pressure reaction kettle, adjusting the rotating speed of a stirrer in the high-pressure reaction kettle to 310rmp, stirring for 60min, starting a cooling water protection device in the high-pressure reaction kettle, adjusting the temperature of the high-pressure reaction kettle to 250 ℃, and carrying out heat preservation reaction for 9h to obtain a material to be aged;
(2) Preparing materials to be dried: placing the material to be aged prepared in the step (1) in an oven, controlling the temperature at 115 ℃ for 16 hours, aging to obtain a precipitate, adding the rest ultrapure water and ultrasonic washing for 12 minutes in a carbon dioxide environment, performing vacuum suction filtration to obtain a suction-filtered material, introducing carbon dioxide gas into the suction-filtered material, and stirring and washing a small amount of the rest glycol for multiple times to obtain the material to be dried;
(3) Preparation of cobalt carbonate particles: and (3) controlling the temperature of the material to be dried, which is prepared in the step (2), to be 90 ℃ and drying for 11 hours to obtain cobalt carbonate particles.
FIG. 1 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in example 3 of the present invention.
FIG. 6 is a graph showing the particle size distribution of spherical cobalt carbonate particles prepared in example 3 of the present invention, to obtain spherical cobalt carbonate having a particle diameter D50 ranging from 6.0.+ -. 0.2. Mu.m.
Comparative example 1
In comparison with example 3, 2 parts by weight of polyvinylpyrrolidone was added in step (1), and the other steps and parameters were the same.
FIG. 2 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 1 of the present invention;
FIG. 7 is a graph showing the particle size distribution of spherical cobalt carbonate particles prepared in comparative example 1 of the present invention, to obtain spherical cobalt carbonate having a particle diameter D50 ranging from 6.7.+ -. 0.2. Mu.m.
Comparative example 2
In comparison with example 3, 3.5 parts by weight of polyvinylpyrrolidone was added in step (1), and the other steps and parameters were the same.
FIG. 3 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 2 of the present invention.
FIG. 8 is a graph showing the particle size distribution of spherical cobalt carbonate particles prepared in comparative example 2 according to the present invention, to obtain spherical cobalt carbonate having a particle size D50 in the range of 6.7.+ -. 0.2. Mu.m.
Comparative example 3
In comparison with example 3, 10 parts by weight of sericin was added in step (1), and the remaining steps and parameters were the same.
FIG. 4 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 3 of the present invention.
FIG. 9 is a graph showing the particle size distribution of spherical cobalt carbonate particles prepared in comparative example 3 according to the present invention, to obtain spherical cobalt carbonate having a particle diameter D50 ranging from 6.7.+ -. 0.2. Mu.m.
Comparative example 4
In comparison with example 3, 19 parts by weight of sericin was added in step (1), and the remaining steps and parameters were the same.
FIG. 5 is a scanning electron microscope image of spherical cobalt carbonate particles prepared in comparative example 4 of the present invention.
FIG. 10 is a graph showing the particle size distribution of spherical cobalt carbonate particles prepared in comparative example 4 of the present invention, to obtain spherical cobalt carbonate having a particle diameter D50 ranging from 6.7.+ -. 0.2. Mu.m.
Comparative example 5
Compared with example 3, the nitrogen gas is introduced in the step (1) instead of the carbon dioxide gas, and the rest steps and parameters are the same.
Comparative example 6
Compared with example 3, the nitrogen gas is introduced in the step (2) instead of the carbon dioxide gas, and the rest steps and parameters are the same.
Comparative example 7
In contrast to example 3, step (2) is:
and (3) placing the material to be aged prepared in the step (1) in an oven, controlling the temperature to 115 ℃ and aging for 16 hours to obtain a precipitate, adding the rest ultrapure water into the precipitate in a carbon dioxide environment, washing for 12 minutes by ultrasonic waves, and carrying out vacuum suction filtration to obtain the material to be dried.
Comparative example 8
In contrast to example 3, step (2) is:
and (3) placing the material to be aged prepared in the step (1) in an oven, controlling the temperature to 115 ℃ and aging for 16 hours to obtain a precipitate, stirring and washing the precipitate for a plurality of times with the residual glycol in the formula amount under the carbon dioxide environment, and carrying out vacuum suction filtration to obtain the material to be dried.
The microscopic morphology of the cobalt carbonate particles prepared in examples 1-3 and comparative examples 1-4 was observed as follows:
the microscopic morphologies of the cobalt carbonate particles prepared in examples 1 to 3 and comparative examples 1 to 8 were observed by using a Hitachi S-4800 scanning electron microscope, the morphology of example 3 was shown in FIG. 1, the morphology of comparative examples 1 to 4 was shown in FIG. 2 to 5, the particle size distribution was shown in FIG. 6 to 10, and the detailed results were shown in Table 1.
TABLE 1
As is clear from Table 1, the cobalt carbonate particles prepared in examples 1 to 3 of the present invention have no agglomeration phenomenon, the particles are remarkable and the sphericity is high, whereas the cobalt carbonate particles prepared in comparative examples 1 to 4 are partially agglomerated and the morphology of the particles is elliptic and spheroid. Specifically, because the invention uses sericin as a regulating agent and polyvinylpyrrolidone is added, the sericin molecular chain can generate the symmetric and three-dimensional extensibility processes such as irregular curling or folding, and the carbonyl bond in the polyvinylpyrrolidone plays a role of a bridge, cobalt ions are attracted from all directions, so that the interaction between the sericin molecules and the cobalt ions is enhanced, simultaneously, the polyvinylpyrrolidone is adsorbed on the surface of cobalt carbonate, and adjacent particles are guided by the sericin, and the cobalt carbonate particles can replicate the curling and folding processes of the sericin molecular chain, and perform self-assembly to perform orientation connection, thereby being beneficial to the formation of the cobalt carbonate particles to spheres.
The morphology of the cobalt carbonate particles prepared in comparative examples 5 to 6 is elliptical, and in detail, in the processes of preparing the material to be aged and the material to be dried, comparative example 5 and comparative example 6 lack the introduction of carbon dioxide gas, that is, lack carbonate, so that the formation and the morphological stability of the cobalt carbonate particles are not facilitated.
The cobalt carbonate particles prepared in comparative examples 7 to 8 exhibited a slight agglomeration phenomenon, because the absence of ultrasonic washing was not conducive to dispersion of the precipitate, so that the precipitate particles were reagglomerated, whereas the absence of ethanol washing resulted in adsorption of water on the particle surfaces, and the agglomeration was large.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (7)
1. A preparation method of spherical cobalt carbonate particles, which is characterized in that the spherical cobalt carbonate particles comprise the following raw materials in parts by weight:
cobalt chloride hexahydrate 25-35 weight portions
27-33 parts by weight of sodium bicarbonate
2.1 to 3.4 parts by weight of polyvinylpyrrolidone
720-870 parts by weight of ultrapure water
320-390 parts by weight of ethylene glycol
12-17 parts by weight of sericin;
the preparation method of the spherical cobalt carbonate particles comprises the following steps:
(1) Preparing a material to be aged: mixing cobalt chloride hexahydrate and 30% of ultrapure water according to a formula, heating to 80-90 ℃ to obtain a standby liquid A, mixing sodium bicarbonate and 30% of ultrapure water according to the formula, heating to 80-90 ℃ to obtain a standby liquid B, slowly pouring the standby liquid A, the standby liquid B and 80% of ethylene glycol into a high-pressure reaction kettle while stirring, adding the formula of polyvinylpyrrolidone and sericin into the high-pressure reaction kettle, introducing carbon dioxide gas, regulating the rotation speed of a stirrer in the high-pressure reaction kettle, stirring, starting a cooling water protection device in the high-pressure reaction kettle, regulating the temperature of the high-pressure reaction kettle, and carrying out heat preservation reaction to obtain a material to be aged;
(2) Preparing materials to be dried: placing the material to be aged prepared in the step (1) in an oven for temperature control and aging to obtain a precipitate, adding the rest ultrapure water into the precipitate under the carbon dioxide environment, ultrasonically washing, performing vacuum suction filtration to obtain a suction filtration substance, introducing carbon dioxide gas into the suction filtration substance, and stirring and washing with the rest of ethylene glycol in the formula amount to obtain the material to be dried;
(3) Preparation of cobalt carbonate particles: drying the material to be dried, which is prepared in the step (2), at a controlled temperature to obtain cobalt carbonate particles;
in the step (2), the temperature in the oven is controlled, the aging temperature is 110-115 ℃, and the aging time is 14-16h.
2. The method for producing spherical cobalt carbonate particles according to claim 1, wherein the stirring time in the autoclave in step (1) is from 40 to 60 minutes at a stirrer rotation speed of from 250 to 310 rmp.
3. The method for producing spherical cobalt carbonate particles according to claim 1, wherein the autoclave temperature in step (1) is 220 to 250 ℃.
4. The method for producing spherical cobalt carbonate particles according to claim 1, wherein the incubation time in step (1) is 7 to 9 hours.
5. The method for producing spherical cobalt carbonate particles according to claim 1, wherein the ultrasonic washing time in step (2) is 10 to 12 minutes.
6. The method for producing spherical cobalt carbonate particles according to claim 1, wherein the stirring washing time in step (2) is 12 to 15 minutes.
7. The method for preparing spherical cobalt carbonate particles according to claim 1, wherein the temperature-controlled drying temperature in the step (3) is 85-90 ℃ and the drying time is 10-11h.
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