CN110961648A - Preparation method of titanium-doped superfine nickel powder - Google Patents
Preparation method of titanium-doped superfine nickel powder Download PDFInfo
- Publication number
- CN110961648A CN110961648A CN201811139424.0A CN201811139424A CN110961648A CN 110961648 A CN110961648 A CN 110961648A CN 201811139424 A CN201811139424 A CN 201811139424A CN 110961648 A CN110961648 A CN 110961648A
- Authority
- CN
- China
- Prior art keywords
- powder
- nickel
- tio
- nickel salt
- titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Abstract
The invention discloses a method for preparing titanium-doped superfine nickel powder, which comprises the steps of mixing a first precipitator and TiO2Adding powder into a reaction kettle, heating the reaction kettle, adding nickel salt, a second precipitator and a surfactant into the reaction kettle, controlling the feeding flow of the nickel salt and the second precipitator to keep the pH value of a reaction system at 7.2-9.2, and obtaining the wrapped TiO2Then wrapping TiO with the basic nickel salt precursor2Carrying out high-temperature hydrogen reduction on the basic nickel salt powder to obtain titanium-doped superfine nickel powder; thus, the invention is doped in the process of preparing the basic nickel salt precursor and then wraps TiO2The basic nickel salt precursor is calcined at high temperature, so that the phenomenon of uneven mixing of the titanium-nickel composite powder can be effectively avoided, the obtained titanium-doped superfine nickel powder has good uniformity, and the plasticity, wear resistance, corrosion resistance, high damping, superelasticity and the like of the nickel powder in alloy application can be enhanced.
Description
Technical Field
The invention belongs to the technical field of nickel powder preparation, and particularly relates to a preparation method of titanium-doped superfine nickel powder.
Background
The superfine nickel powder is a good electric and magnetic heat sensitive material, and has wide application prospect in the aspects of catalysts, magnetic materials, sintering activators, conductive slurry, battery materials, hard alloy binders and the like.
At present, in many alloy aspects, titanium powder is mixed for use, the traditional manufacturing method of titanium-nickel composite powder comprises a mechanical mixing method and an atomization method, and the titanium-nickel composite powder manufactured by the two methods is not uniformly mixed, so that more defects exist in the alloy easily, and the service life of the alloy is influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of titanium-doped superfine nickel powder.
The invention provides a preparation method of titanium-doped superfine nickel powder, which is implemented by the following steps:
step 1, adding a first precipitator into a reaction kettle to serve as a base solution, stirring the base solution at a stirring frequency of 25Hz, and adding TiO into the first precipitator2Powder is stirred for 30-60 min until the TiO2Dispersing powder into a first precipitator, heating the reaction kettle to 60-70 ℃ and keeping the temperature constant, adding nickel salt, a second precipitator and a surfactant into the reaction kettle, controlling the feeding flow of the nickel salt and the second precipitator to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3-5 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, adopting pure water to wrap the TiO obtained in the step 12The basic nickel salt precursor is washed and then dried to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22The basic nickel salt powder is crushed by airflow and then is reduced by high-temperature hydrogen to obtain the titanium-doped superfine nickel powder.
In the scheme, the TiO added in the step 12The mass ratio of the powder to the nickel salt is 1: 500-2: 500.
In the above scheme, the nickel salt in step 1 is one of a nickel nitrate solution, a nickel sulfate solution or a nickel chloride solution.
In the scheme, the nickel content of the nickel salt in the step 1 is 2mol/L, and the feeding flow rate of the nickel salt is 200L/H.
In the above scheme, in step 1, the first precipitant and the second precipitant are both one of sodium carbonate, ammonium bicarbonate, ammonium carbonate or sodium hydroxide.
In the scheme, the volume of the first precipitator added in the step 1 is 400-500L, and the concentration of the first precipitator is 0.05 mol/L.
In the scheme, the volume ratio of the second precipitator to the nickel salt added in the step 1 is 1.8: 1-2.5: 1, the concentration of the second precipitator is 2mol/L, and the feeding flow rate of the second precipitator is 400L/H.
In the above scheme, the surfactant in step 1 is one of (L) -tartaric acid, citric acid or oxalic acid.
In the scheme, the volume of the surfactant added in the step 1 is 8-16L.
In the scheme, the reduction temperature of the high-temperature hydrogen reduction in the step 3 is 600-700 ℃, and the reduction time is 2-3 h.
Compared with the prior art, the method is used for doping in the process of preparing the basic nickel salt precursor to obtain the wrapped TiO2The basic nickel salt precursor is coated with TiO2The basic nickel salt precursor is calcined at high temperature to obtain wrapped TiO2The basic nickel salt powder can effectively avoid the phenomenon of uneven mixing of the titanium-nickel composite powder, the obtained titanium-doped superfine nickel powder has good uniformity, and the plasticity and the wear resistance of the nickel powder in alloy application can be enhancedDamage, corrosion resistance, high damping, super elasticity and the like.
Drawings
Fig. 1 is a scanning electron microscope image of a method for preparing titanium-doped ultrafine nickel powder according to embodiment 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments and the accompanying drawings. 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 preparation method of titanium-doped superfine nickel powder, which is implemented by the following steps:
step 1, adding 400L-500L of first precipitator with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the first precipitator2Powder, added TiO2The mass ratio of the powder to the nickel salt is 1: 500-2: 500, and the mixture is stirred for 30-60 min to TiO2Dispersing the powder in a first precipitator, heating a reaction kettle to 60-70 ℃ and keeping the temperature constant, adding nickel salt with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding a second precipitator with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the second precipitator to the nickel salt is 1.8: 1-2.5: 1, simultaneously adding 8-16L of surfactant to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3-5H to obtain the coated TiO2The basic nickel salt precursor;
wherein the nickel salt is one of nickel nitrate solution, nickel sulfate solution or nickel chloride solution; the first precipitator and the second precipitator are both one of sodium carbonate, ammonium bicarbonate, ammonium carbonate or sodium hydroxide; the surfactant is one of (L) -tartaric acid, citric acid or oxalic acid;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is placed in a two-in-one washing machine, washed for 4-6 times by pure water at the temperature of 60-80 ℃, placed in a flash evaporation machine after washing, and washed for 6 timesDrying at 0-80 ℃ to obtain coated TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the alkali nickel salt powder by airflow, then putting the crushed alkali nickel salt powder into a reduction furnace, reducing the crushed alkali nickel salt powder for 2 to 3 hours by high-temperature hydrogen at the reduction temperature of 600 to 700 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
The invention is doped in the process of preparing basic nickel salt precursor to obtain wrapped TiO2The basic nickel salt precursor is coated with TiO2The basic nickel salt precursor is calcined at high temperature to obtain wrapped TiO2The basic nickel salt powder can effectively avoid the phenomenon of uneven mixing of the titanium-nickel composite powder, and the obtained titanium-doped superfine nickel powder has good uniformity and can enhance the plasticity, wear resistance, corrosion resistance, high damping, superelasticity and the like of the nickel powder in alloy application. The method of twice precipitating agents can effectively control the particle size distribution of the precursor of the prepared nickel powder, thereby controlling the particle size distribution of the nickel powder; the obtained product can be directly used for alloy mixing by controlling the mass ratio of the titanium to the nickel, so that the application range of the titanium-nickel powder is enlarged; the TiO is greatly enhanced by adding a small amount of surfactant2And the nickel powder precursor, thereby avoiding a large amount of agglomeration, enhancing the applicability of the Ti-doped nickel powder in the alloy tool industry, and effectively weakening the limitation of the alloy tool performance caused by uneven mixing in the alloy production process.
Example 1
Embodiment 1 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of sodium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the sodium carbonate2Powder, added TiO2The mass ratio of the powder to the nickel nitrate solution is 1:500, and the mixture is stirred for 30min until TiO2Dispersing the powder in sodium carbonate, heating the reaction kettle to 60 ℃ and keeping the temperature constant, and adding a nickel nitrate solution with the nickel content of 2mol/L into the reaction kettle by adopting a metering pump at the feeding flow rate of 200L/H so as toAdding sodium carbonate with the concentration of 2mol/L into a reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the sodium carbonate to the nickel nitrate solution is 2:1, simultaneously adding 12L of (L) -tartaric acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 4H to obtain coated TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 70 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the basic nickel salt powder by airflow, then putting the crushed basic nickel salt powder into a reduction furnace, reducing the crushed basic nickel salt powder for 2.8 hours by high-temperature hydrogen at the reduction temperature of 660 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
As shown in fig. 1, it can be seen from a scanning electron microscope image of the method for preparing titanium-doped ultrafine nickel powder provided in embodiment 1 that the Ti-Ni powder is uniformly mixed and distributed without separate agglomeration.
Example 2
Embodiment 2 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 450L of sodium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the sodium carbonate2Powder, added TiO2The mass ratio of the powder to the nickel nitrate solution is 1.5:500, and the mixture is stirred for 45min until TiO2Dispersing the powder in sodium carbonate, heating a reaction kettle to 66 ℃ and keeping the temperature constant, adding a nickel nitrate solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding sodium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the sodium carbonate to the nickel nitrate solution is 2:1, simultaneously adding 12L of (L) -tartaric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 4 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, packaging the obtained packages in the step 1TiO2The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 70 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the basic nickel salt powder by airflow, then putting the crushed basic nickel salt powder into a reduction furnace, reducing the crushed basic nickel salt powder for 2.8 hours by high-temperature hydrogen at the reduction temperature of 660 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 3
Embodiment 3 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of sodium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the sodium carbonate2Powder, added TiO2The mass ratio of the powder to the nickel nitrate solution is 2:500, and the mixture is stirred for 60min until TiO2Dispersing the powder in sodium carbonate, heating a reaction kettle to 70 ℃ and keeping the temperature constant, adding a nickel nitrate solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding sodium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the sodium carbonate to the nickel nitrate solution is 2:1, simultaneously adding 12L of (L) -tartaric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 4 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 70 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22The basic nickel salt powder is crushed by airflow and then is put into a reduction furnace, and the reduction temperature is 660 DEG CReducing the mixture for 2.8h by high-temperature hydrogen, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 4
Embodiment 4 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of ammonium bicarbonate with the concentration of 0.05mol/L into a reaction kettle to be used as a base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the ammonium bicarbonate2Powder, added TiO2The mass ratio of the powder to the nickel sulfate solution is 1:500, and the mixture is stirred for 40min to TiO2Dispersing the powder in ammonium bicarbonate, heating a reaction kettle to 68 ℃ and keeping the temperature constant, adding a nickel sulfate solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow of 200L/H by using a metering pump, adding ammonium bicarbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow of 400L/H, wherein the volume ratio of the ammonium bicarbonate to the nickel sulfate solution is 1.8:1, simultaneously adding 8L of citric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 70 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the alkali nickel salt powder by airflow, then putting the crushed alkali nickel salt powder into a reduction furnace, reducing the crushed alkali nickel salt powder for 3 hours by high-temperature hydrogen at the reduction temperature of 640 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 5
Embodiment 5 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of ammonium bicarbonate with the concentration of 0.05mol/L into a reaction kettle to be used as a base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the ammonium bicarbonate2Powder, added TiO2The mass ratio of the powder to the nickel sulfate solution is 1:500, and the mixture is stirred for 40min to TiO2Dispersing the powder in ammonium bicarbonate, heating a reaction kettle to 68 ℃ and keeping the temperature constant, adding a nickel sulfate solution with the nickel content of 2mol/L into the reaction kettle at a feeding flow rate of 200L/H by using a metering pump, adding ammonium bicarbonate with the concentration of 2mol/L into the reaction kettle at a feeding flow rate of 400L/H, wherein the volume ratio of the ammonium bicarbonate to the nickel sulfate solution is 2.3:1, simultaneously adding 12L of citric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 4 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 70 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the alkali nickel salt powder by airflow, then putting the crushed alkali nickel salt powder into a reduction furnace, reducing the crushed alkali nickel salt powder for 3 hours by high-temperature hydrogen at the reduction temperature of 640 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 6
Embodiment 6 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 500L of ammonium bicarbonate with the concentration of 0.05mol/L into a reaction kettle to be used as a base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the ammonium bicarbonate2Powder, added TiO2The mass ratio of the powder to the nickel sulfate solution is 1:500, and the mixture is stirred for 40min to TiO2Dispersing the powder in ammonium bicarbonate, heating a reaction kettle to 68 ℃ and keeping the temperature constant, adding a nickel sulfate solution with the nickel content of 2mol/L into the reaction kettle at a feeding flow rate of 200L/H by using a metering pump, adding ammonium bicarbonate with the concentration of 2mol/L into the reaction kettle at a feeding flow rate of 400L/H, wherein the volume ratio of the ammonium bicarbonate to the nickel sulfate solution is 2.5:1, simultaneously adding 16L of citric acid to keep the pH value of a reaction system at 7.2-9.2, and reacting for 5 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 70 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the alkali nickel salt powder by airflow, then putting the crushed alkali nickel salt powder into a reduction furnace, reducing the crushed alkali nickel salt powder for 3 hours by high-temperature hydrogen at the reduction temperature of 640 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 7
Embodiment 7 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of ammonium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the ammonium carbonate2Powder, added TiO2The mass ratio of the powder to the nickel chloride solution is 2:500, and the mixture is stirred for 60min until TiO2Dispersing the powder in ammonium carbonate, heating the reaction kettle to 65 ℃ and keeping the temperature constant, adding a nickel chloride solution with the nickel content of 2mol/L into the reaction kettle at a feeding flow rate of 200L/H by using a metering pump, adding ammonium carbonate with the concentration of 2mol/L into the reaction kettle at a feeding flow rate of 400L/H, wherein the volume ratio of the ammonium carbonate to the nickel chloride solution is 2:1, and simultaneously adding 12L of oxalic acid to ensure that the reaction kettle is enabled to have the nickel chloride solution and the ammonium carbonate solution have the same volume ratioThe pH value of the reaction system is kept between 7.2 and 9.2, and the reaction is carried out for 3.6 hours to obtain the wrapped TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 6 times by pure water at 60 ℃, then put into a flash evaporation machine after washing, and dried at 60 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the basic nickel salt powder by airflow, putting the crushed basic nickel salt powder into a reduction furnace, reducing the crushed basic nickel salt powder for 3 hours by high-temperature hydrogen at the reduction temperature of 600 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 8
Embodiment 8 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of ammonium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the ammonium carbonate2Powder, added TiO2The mass ratio of the powder to the nickel chloride solution is 2:500, and the mixture is stirred for 60min until TiO2Dispersing the powder in ammonium carbonate, heating a reaction kettle to 65 ℃ and keeping the temperature constant, adding a nickel chloride solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow rate of 200L/H by using a metering pump, adding ammonium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow rate of 400L/H, wherein the volume ratio of the ammonium carbonate to the nickel chloride solution is 2:1, simultaneously adding 12L of oxalic acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 3.6 hours to obtain the wrapped TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 5 times by pure water at 72 ℃, put into a flash evaporation machine after washing, and dried at 72 ℃ to obtain the wrapped TiO2Basic nickel salt powder ofGrinding;
step 3, wrapping the wrapped TiO obtained in the step 22The alkali nickel salt powder is crushed by airflow and then is put into a reduction furnace, the high-temperature hydrogen is reduced for 2.2 hours at the reduction temperature of 640 ℃, and finally, iron is removed to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
Example 9
Embodiment 9 of the present invention provides a method for preparing titanium-doped ultrafine nickel powder, which is implemented by the following steps:
step 1, adding 400L of ammonium carbonate with the concentration of 0.05mol/L into a reaction kettle to be used as base solution, stirring the base solution at the stirring frequency of 25Hz, and adding TiO into the ammonium carbonate2Powder, added TiO2The mass ratio of the powder to the nickel chloride solution is 2:500, and the mixture is stirred for 60min until TiO2Dispersing the powder in ammonium carbonate, heating a reaction kettle to 65 ℃ and keeping the temperature constant, adding a nickel chloride solution with the nickel content of 2mol/L into the reaction kettle at the feeding flow rate of 200L/H by using a metering pump, adding ammonium carbonate with the concentration of 2mol/L into the reaction kettle at the feeding flow rate of 400L/H, wherein the volume ratio of the ammonium carbonate to the nickel chloride solution is 2:1, simultaneously adding 12L of oxalic acid to keep the pH value of the reaction system at 7.2-9.2, and reacting for 3.6 hours to obtain the wrapped TiO2The basic nickel salt precursor;
step 2, wrapping the wrapped TiO obtained in the step 12The basic nickel salt precursor is put into a two-in-one washing machine, washed for 4 times by pure water at the temperature of 80 ℃, put into a flash evaporation machine after washing, and dried at the temperature of 80 ℃ to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22And crushing the basic nickel salt powder by airflow, then putting the crushed basic nickel salt powder into a reduction furnace, reducing the crushed basic nickel salt powder for 2 hours by high-temperature hydrogen at the reduction temperature of 700 ℃, and finally removing iron to obtain the titanium-doped superfine nickel powder.
Compared with the prior art, the titanium-doped superfine nickel powder obtained by the preparation process has uniform Ti-Ni powder mixing distribution and no independent agglomeration.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (10)
1. The preparation method of the titanium-doped superfine nickel powder is characterized by comprising the following steps:
step 1, adding a first precipitator into a reaction kettle to serve as a base solution, stirring the base solution at a stirring frequency of 25Hz, and adding TiO into the first precipitator2Powder is stirred for 30-60 min until the TiO2Dispersing powder into a first precipitator, heating the reaction kettle to 60-70 ℃ and keeping the temperature constant, adding nickel salt, a second precipitator and a surfactant into the reaction kettle, controlling the feeding flow of the nickel salt and the second precipitator to keep the pH value of a reaction system at 7.2-9.2, and reacting for 3-5 hours to obtain coated TiO2The basic nickel salt precursor;
step 2, adopting pure water to wrap the TiO obtained in the step 12The basic nickel salt precursor is washed and then dried to obtain the wrapped TiO2The basic nickel salt powder of (4);
step 3, wrapping the wrapped TiO obtained in the step 22The basic nickel salt powder is crushed by airflow and then is reduced by high-temperature hydrogen to obtain the titanium-doped superfine nickel powder.
2. The method of claim 1, wherein the TiO added in step 1 is added2The mass ratio of the powder to the nickel salt is 1: 500-2: 500.
3. The method of claim 2, wherein the nickel salt in step 1 is one of a nickel nitrate solution, a nickel sulfate solution, or a nickel chloride solution.
4. The method of claim 3, wherein the nickel content of the nickel salt in step 1 is 2mol/L, and the feeding flow rate of the nickel salt is 200L/H.
5. The method of claim 4, wherein the first precipitant and the second precipitant are selected from sodium carbonate, ammonium bicarbonate, ammonium carbonate and sodium hydroxide in step 1.
6. The method of claim 5, wherein the volume of the first precipitant added in step 1 is 400-500L, and the concentration of the first precipitant is 0.05 mol/L.
7. The method for preparing titanium-doped ultrafine nickel powder according to claim 6, wherein the volume ratio of the second precipitator to the nickel salt added in step 1 is 1.8: 1-2.5: 1, the concentration of the second precipitator is 2mol/L, and the feeding flow rate of the second precipitator is 400L/H.
8. The method of claim 7, wherein the surfactant in step 1 is one of (L) -tartaric acid, citric acid, and oxalic acid.
9. The method for preparing titanium-doped ultrafine nickel powder according to claim 8, wherein the volume of the surfactant added in step 1 is 8 to 16L.
10. The method for preparing titanium-doped ultrafine nickel powder according to any one of claims 1 to 9, wherein the reduction temperature of the high-temperature hydrogen reduction in step 3 is 600 to 700 ℃ and the reduction time is 2 to 3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811139424.0A CN110961648A (en) | 2018-09-28 | 2018-09-28 | Preparation method of titanium-doped superfine nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811139424.0A CN110961648A (en) | 2018-09-28 | 2018-09-28 | Preparation method of titanium-doped superfine nickel powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110961648A true CN110961648A (en) | 2020-04-07 |
Family
ID=70026853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811139424.0A Withdrawn CN110961648A (en) | 2018-09-28 | 2018-09-28 | Preparation method of titanium-doped superfine nickel powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110961648A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830606A (en) * | 2006-04-14 | 2006-09-13 | 北京科技大学 | Method of preparing ultrafine alloy powder by coprecipitation coreduction |
| CN101332515A (en) * | 2008-08-05 | 2008-12-31 | 中南大学 | Preparation method of fibrous iron-nickel alloy powder |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN101797650A (en) * | 2010-04-22 | 2010-08-11 | 昆明贵金属研究所 | Method for producing surface-activated superfine nickel powder |
| CN102728852A (en) * | 2012-07-10 | 2012-10-17 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of oxide or meta-coated nickel ultrafine powder |
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN107088660A (en) * | 2017-07-03 | 2017-08-25 | 张成亮 | A kind of preparation method of ultra-fine cobalt nickel powder |
-
2018
- 2018-09-28 CN CN201811139424.0A patent/CN110961648A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830606A (en) * | 2006-04-14 | 2006-09-13 | 北京科技大学 | Method of preparing ultrafine alloy powder by coprecipitation coreduction |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN101332515A (en) * | 2008-08-05 | 2008-12-31 | 中南大学 | Preparation method of fibrous iron-nickel alloy powder |
| CN101797650A (en) * | 2010-04-22 | 2010-08-11 | 昆明贵金属研究所 | Method for producing surface-activated superfine nickel powder |
| CN102728852A (en) * | 2012-07-10 | 2012-10-17 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of oxide or meta-coated nickel ultrafine powder |
| CN105921762A (en) * | 2016-06-17 | 2016-09-07 | 陕西理工学院 | Densification formation type preparation method of nickel-based alloy powder |
| CN107088660A (en) * | 2017-07-03 | 2017-08-25 | 张成亮 | A kind of preparation method of ultra-fine cobalt nickel powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112357974B (en) | Preparation method of ternary cathode material NCA precursor | |
| CN111682197B (en) | Single crystal type anion and cation co-doped nickel-magnesium binary cobalt-free precursor, positive electrode material and preparation method | |
| CN110534732A (en) | A kind of preparation method of nickel-cobalt-manganese ternary persursor material | |
| CN110961647A (en) | Preparation method of molybdenum-doped superfine nickel powder | |
| CN109546144A (en) | The preparation method and applications of ternary precursor | |
| CN110510593A (en) | A kind of preparation method of ferric phosphate presoma and LiFePO4 | |
| CN109987646B (en) | Continuous reaction method for synthesizing large-particle-size cobalt carbonate | |
| CN104478699B (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN110961652A (en) | Preparation method of lanthanum-doped superfine nickel powder | |
| CN113314707B (en) | Modified nickel-cobalt lithium aluminate anode material and preparation method and application thereof | |
| CN113659129A (en) | Multi-element doped ternary precursor and preparation method thereof | |
| CN109546126A (en) | A kind of transition metal element doped carbon coating lithium titanate, preparation method and application | |
| CN106816579B (en) | Method for preparing lithium nickel cobalt manganese oxide lithium ion battery positive electrode material by freezing crystallization method | |
| CN110961655A (en) | Preparation method of tungsten-doped superfine nickel powder | |
| CN110961648A (en) | Preparation method of titanium-doped superfine nickel powder | |
| CN111634935A (en) | Microwave preparation method of nano rare earth oxide | |
| CN113800574B (en) | Nickel-manganese-iron-aluminum-lithium positive electrode material and preparation method thereof | |
| CN114843458B (en) | High-nickel monocrystal cobalt-free positive electrode material and preparation method thereof | |
| CN114361448B (en) | Lithium iron phosphate, preparation method thereof and lithium ion battery | |
| CN109346711A (en) | A kind of carbon coating lithium titanate, the preparation method and application of thulium doping | |
| CN110961650A (en) | Preparation method of zirconium-doped superfine nickel powder | |
| CN110961651A (en) | Preparation method of chromium-doped superfine nickel powder | |
| CN110961654A (en) | Preparation method of tin-doped superfine nickel powder | |
| CN110961649A (en) | Preparation method of cobalt-doped superfine nickel powder | |
| CN110961658A (en) | Preparation method of iron-doped superfine nickel powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200407 |
|
| WW01 | Invention patent application withdrawn after publication |