CN112723424A - Rod-shaped composite basic cobalt carbonate precursor and preparation method thereof - Google Patents
Rod-shaped composite basic cobalt carbonate precursor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a rod-shaped composite basic cobalt carbonate precursor, which comprises the following steps: 1) simultaneously adding a cobalt salt solution and an ammonium bicarbonate solution into a reaction device with a base solution, and controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow of the ammonium bicarbonate while stirring to perform a coprecipitation reaction to obtain a coprecipitation reactant; 2) and (3) carrying out centrifugal hot water washing and drying on the coprecipitation reactant to obtain a rod-shaped composite basic cobalt carbonate precursor. According to the invention, a deionized water solution containing 10-30 g/L ammonium bicarbonate is selected as a base solution in a reaction device, the stirring speed is controlled to be 250-350 r/min when reaction raw materials of cobalt salt and ammonium bicarbonate are added, and the reaction conditions that the pH value of a reaction system in the reaction device is controlled to be 7.3-7.5 and the temperature is kept at 50-65 ℃ are controlled by adjusting the flow of the ammonium bicarbonate, so that the prepared precursor is in a rod shape.
Description
Technical Field
The invention belongs to the technical field of basic cobalt carbonate precursors, and particularly relates to a rod-shaped composite basic cobalt carbonate precursor and a preparation method thereof.
Background
Cobalt powder is widely applied to the fields of hard alloy, batteries, catalysts, magnetic materials, wave-absorbing materials, ceramics and the like due to the special physical and chemical properties and good mechanical properties of the cobalt powder; the cobalt powder for producing hard alloy and battery is produced through the reduction of cobalt oxide and oxalate, thermal dissociation of oxalate, reduction of polyol cobalt salt, etc. In recent years, in order to prepare high-quality cobalt powder more easily, some domestic and foreign enterprises prepare cobalt powder by hydrogen reduction of cobalt oxalate, and obtain Co by precipitation-hydrogen reduction calcination with cobalt oxalate as a precursor. The morphology of the cobalt powder has inheritance to the raw material, so the quality of the performance of the cobalt powder also depends on the performance of the raw material. In the traditional method, cobalt powder prepared by reducing cobalt oxalate is generally needle-shaped or dendritic cobalt oxalate, and the cobalt powder is in irregular shapes such as dendritic shape. Disordered deposition of rod-shaped cobalt powder in the nickel-metal hydride battery can increase the conductivity of the positive electrode material; however, the price of preparing the cobalt powder by reducing the common cobalt oxalate is higher, and the rod-shaped composite basic cobalt carbonate precursor is prepared by simple low-temperature precipitation, so that the preparation of the rod-shaped cobalt powder is possible.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a bar-shaped composite basic cobalt carbonate precursor; the invention also aims to provide a preparation method of the rodlike composite basic cobalt carbonate precursor.
In order to achieve the purpose, the technical scheme of the invention is realized as follows: a bar-shaped composite basic cobalt carbonate precursor has the chemical expression as follows: (NH)4)2CO8(CO3)6(OH)6·4H2O。
The other technical scheme of the invention is realized as follows: a preparation method of a rod-shaped composite basic cobalt carbonate precursor comprises the following steps:
step 1, simultaneously adding a cobalt salt solution and an ammonium bicarbonate solution into a reaction device with deionized water, and controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow of the ammonium bicarbonate while stirring to perform a coprecipitation reaction to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing and drying on the coprecipitation reactant obtained in the step 1 to obtain a rod-shaped composite basic cobalt carbonate precursor.
Preferably, in the step 1, the concentration of cobalt ions in the cobalt salt is 80-140 g/L; the concentration of the ammonium bicarbonate solution is 150-260 g/L.
Preferably, in the step 1, the base solution is a deionized water solution containing 10-30 g/L ammonium bicarbonate.
Preferably, in the step 1, the cobalt salt is at least one of cobalt chloride and cobalt sulfate.
Preferably, in the step 1, the flow ratio of the cobalt salt solution and the ammonium bicarbonate solution added into the reaction device is 1 (0.99-3).
Preferably, in the step 1, the stirring speed is 250-350 r/min; the reaction temperature of the coprecipitation reaction is 50-65 ℃.
Preferably, in the step 2, the washing process is stopped when the co-precipitation reactant is centrifugally washed with hot water until the content of chloride ions is less than 100 ppm.
Preferably, in the step 2, the drying temperature is 100-120 ℃.
Compared with the prior art, the method disclosed by the invention has the advantages that the deionized water solution containing 10-30 g/L of ammonium bicarbonate is selected as the base solution in the reaction device, the stirring speed is controlled to be 250-350 r/min when the reaction raw materials of cobalt salt and ammonium bicarbonate are added, and the reaction condition that the pH value of a reaction system in the reaction device is controlled to be 7.3-7.5 is realized by adjusting the flow of the ammonium bicarbonate, so that the prepared composite basic cobalt carbonate precursor is rod-shaped, and the rod-shaped composite basic cobalt carbonate precursor lays a solid foundation for preparing rod-shaped cobalt powder; in addition, when the rod-shaped cobalt powder prepared by the rod-shaped composite basic cobalt carbonate precursor is applied to the preparation process of an active material of a nickel-metal hydride battery, the disordered precipitation of the rod-shaped cobalt powder can increase the conductivity of a positive electrode material.
Drawings
FIG. 1 is an SEM image of a rod-like composite basic cobalt carbonate precursor obtained in example 1 of the present invention;
FIG. 2 is an SEM image of a rod-like composite basic cobalt carbonate precursor obtained in example 2 of the present invention;
FIG. 3 is an SEM image of a rod-like composite basic cobalt carbonate precursor obtained in example 6 of the present invention;
FIG. 4 is an SEM image of a rod-like composite basic cobalt carbonate precursor obtained by a comparative example of the present invention;
fig. 5 is XRD charts of the rod-shaped composite basic cobalt carbonate precursor obtained in examples 1 to 4, 6 and 8 of the present invention and the cobalt carbonate precursor obtained in comparative example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a rod-shaped composite basic cobalt carbonate precursor, which has the chemical expression as follows: (NH)4)2CO8(CO3)6(OH)6·4H2O。
The embodiment of the invention also provides a preparation method of the rodlike composite basic cobalt carbonate precursor, which comprises the following steps:
step 1, adding a cobalt salt solution with the cobalt ion concentration of 80-140 g/L into a reaction device containing a deionized water solution of 10-30 g/L ammonium bicarbonate according to an ammonium bicarbonate solution with the cobalt ion concentration of 150-260 g/L, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow of the ammonium bicarbonate at a stirring speed of 250-350 r/min, and carrying out a coprecipitation reaction at 50-65 ℃ to obtain a coprecipitation reactant; wherein, the cobalt salt is at least one of cobalt chloride and cobalt sulfate; the flow ratio of the cobalt salt solution and the ammonium bicarbonate solution added into the reaction device is 1 (0.99-3);
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 100-120 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 1
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 130g/L of cobalt ions into a reaction device containing a deionized water solution of 25g/L of ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 4.1L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow rate of the ammonium bicarbonate at the stirring speed of 250r/min, and carrying out coprecipitation reaction at the temperature of 60 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 110 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 2
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 130g/L of cobalt ions into a reaction device containing a deionized water solution of 25g/L of ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 4.1L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow rate of the ammonium bicarbonate at the stirring speed of 300r/min, and carrying out coprecipitation reaction at the temperature of 60 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 110 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 3
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 130g/L of cobalt ions into a reaction device containing a deionized water solution of 25g/L of ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 4.1L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow rate of the ammonium bicarbonate at the stirring speed of 350r/min, and carrying out coprecipitation reaction at the temperature of 60 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 110 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 4
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of cobalt ions of 80g/L into a reaction device containing a deionized water solution of 10g/L ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 4.0L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow of the ammonium bicarbonate at the stirring speed of 350r/min, and carrying out coprecipitation reaction at 55 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 100 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 5
Rod-like composite basic cobalt carbonate precursorBody (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 140g/L of cobalt ions into a reaction device containing a deionized water solution of 30g/L of ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 3.46L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow rate of the ammonium bicarbonate at the stirring speed of 250r/min, and carrying out coprecipitation reaction at the temperature of 60 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 120 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 6
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 130g/L of cobalt ions into a reaction device containing a deionized water solution of 25g/L of ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 4.1L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow rate of the ammonium bicarbonate at the stirring speed of 350r/min, and carrying out coprecipitation reaction at the temperature of 60 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 100 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 7
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of cobalt ions of 80g/L into a reaction device containing a deionized water solution of 10g/L ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 4.0L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow of the ammonium bicarbonate at the stirring speed of 250r/min, and carrying out coprecipitation reaction at 55 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 120 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Example 8
Rod-shaped composite basic cobalt carbonate precursor (NH)4)2CO8(CO3)6(OH)6·4H2The O is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 140g/L of cobalt ions into a reaction device containing a deionized water solution of 30g/L of ammonium bicarbonate at the same time according to the feeding speed of 2L/h and the feeding speed of 3.5L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow of the ammonium bicarbonate at the stirring speed of 350r/min, and carrying out coprecipitation reaction at 65 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 110 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
Comparative example
The composite basic cobalt carbonate precursor is prepared by the following steps:
step 1, adding a cobalt chloride solution with the concentration of 130g/L of cobalt ions into a reaction device of deionized water at the same time according to the feeding speed of 2L/h and the feeding speed of an ammonium bicarbonate solution with the concentration of 200g/L of 4.1L/h, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 by adjusting the flow rate of the ammonium bicarbonate solution at the stirring speed of 250r/min, and carrying out coprecipitation reaction at 45 ℃ to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing on the coprecipitation reactant obtained in the step 1 until the content of chloride ions is less than 100ppm, stopping washing, and drying at 110 ℃ to obtain a rod-shaped composite basic cobalt carbonate precursor.
In addition, the reaction apparatus in examples 1 to 8 and comparative example are preferably a reaction vessel.
Detection example 1
1) PDS detection was performed on the bar-shaped composite basic cobalt carbonate precursors obtained in examples 1 to 8, and the detection results are detailed in Table 1;
table 1 PDS test results of the bar-shaped composite basic cobalt carbonate precursors obtained in examples 1 to 8:
as can be seen from the detection data in Table 1 above, the rod-like composite basic cobalt carbonate precursor CoCO prepared by the method of the present invention3·(NH4)2CO8(CO3)6·4H2The particle size of O is intensively distributed between 10 and 17 mu m, and the average particle size is reduced due to the existence of the particles.
Detection example 2
1) Performing electron microscope Scanning (SEM) detection on the composite basic cobalt carbonate precursors obtained in the examples 1, 2, 6 and the comparative example, wherein the detection results are shown in accompanying figures 1-4;
as can be seen from fig. 1 and 2: the composite basic cobalt carbonate precursor prepared by the method in the embodiment of the invention is rod-shaped, and the dispersibility of a sample can be improved by properly increasing the rotating speed;
as can be seen from fig. 3 and 4, the composite basic cobalt carbonate precursor prepared by the method of the present example with different base solution concentrations is rod-like and sphere-like or spherical, the sample produced at 20g/L is rod-like and has a large aspect ratio, and when it exceeds 25g/L, small particles begin to appear, and the morphology becomes poor.
2) XRD detection is carried out on the rod-shaped composite basic cobalt carbonate precursors obtained in examples 1-4, 6 and 8 and the comparative example, and the detection result is shown in the attached figure 5:
as can be seen from FIG. 5, the higher the speed, the (NH) produced4)2Co8(CO3)6(OH)64H2The purer the O phase, the more than 30g/L the concentration of the base solution, and the generated products are all CoCO3The concentration of the base solution is more than 40g/L, and the generated products are all CoCO3And (NH)4)2Co8(CO3)6(OH)64H2And O. At a temperature below 60 ℃, the products are all CoCO3The product formed at 70 ℃ is Co (CO)3)0.5(OH)0.11H2O。
In conclusion, the method disclosed by the invention selects a deionized water solution containing 10-30 g/L of ammonium bicarbonate as a base solution in a reaction device, controls the stirring speed to be 250-350 r/min when adding reaction raw materials of cobalt salt and ammonium bicarbonate and controls the reaction condition that the pH value of a reaction system in the reaction device is 7.3-7.5 by adjusting the flow of the ammonium bicarbonate, so that the prepared precursor is a rod-shaped composite basic cobalt carbonate precursor, and the rod-shaped composite basic cobalt carbonate precursor lays a solid foundation for preparing rod-shaped cobalt powder; in addition, when the rod-shaped cobalt powder prepared by the rod-shaped composite basic cobalt carbonate precursor is applied to the preparation process of an active material of a nickel-metal hydride battery, the disordered precipitation of the rod-shaped cobalt powder can increase the conductivity of the positive electrode material, and meanwhile, the preparation efficiency is improved, the production cost is reduced, and the method is worthy of vigorous popularization and application.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A bar-shaped composite basic cobalt carbonate precursor is characterized by high length-diameter ratio, and the chemical expression is as follows: (NH)4)2CO8(CO3)6(OH)6·4H2O。
2. A preparation method of a rod-shaped composite basic cobalt carbonate precursor is characterized by high length-diameter ratio, and comprises the following steps:
step 1, simultaneously adding a cobalt salt solution and an ammonium bicarbonate solution into a reaction device with a base solution, controlling the pH value of a reaction system in the reaction device to be 7.3-7.5 and keeping the temperature at 50-65 ℃ for coprecipitation reaction by adjusting the flow rate of the ammonium bicarbonate while stirring to obtain a coprecipitation reactant;
and 2, carrying out centrifugal hot water washing and drying on the coprecipitation reactant obtained in the step 1 to obtain a rod-shaped composite basic cobalt carbonate precursor.
3. The preparation method of the rod-shaped composite basic cobalt carbonate precursor according to claim 2, wherein the length-diameter ratio is high, and in the step 1, the concentration of cobalt ions in the cobalt salt is 80-140 g/L; the concentration of the ammonium bicarbonate solution is 150-260 g/L.
4. The method for preparing the rod-shaped composite basic cobalt carbonate precursor according to claim 3, wherein the aspect ratio is high, and in the step 1, the cobalt salt is at least one of cobalt chloride and cobalt sulfate.
5. The method for preparing the rod-shaped composite basic cobalt carbonate precursor according to claim 2, wherein in the step 1, the base solution is a deionized water solution containing 10-30 g/L ammonium bicarbonate.
6. The preparation method of the rod-shaped composite basic cobalt carbonate precursor according to claim 2, wherein the length-diameter ratio is high, and in the step 1, the flow ratio of the cobalt salt solution and the ammonium bicarbonate solution added into the reaction device is 1 (0.99-3).
7. The preparation method of the rod-shaped composite basic cobalt carbonate precursor according to claim 2, wherein in the step 1, the stirring speed is 250-350 r/min; the reaction temperature of the coprecipitation reaction is 50-65 ℃.
8. The method for preparing the rod-shaped composite basic cobalt carbonate precursor according to claim 2, wherein the aspect ratio is high, and in the step 2, when the co-precipitation reactant is subjected to centrifugal hot water washing until the content of chloride ions is less than 100ppm, the washing process is stopped.
9. The preparation method of the rod-shaped composite basic cobalt carbonate precursor according to any one of claims 2 to 8, wherein the length-to-diameter ratio is high, and the drying temperature in the step 2 is 100 to 120 ℃.
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