CN114394578A - Vanadium nitride precursor and preparation method thereof - Google Patents
Vanadium nitride precursor and preparation method thereof Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
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Abstract
The invention relates to a precursor of vanadium nitride and a preparation method thereof. The technical scheme is as follows: adding a carbonaceous reducing agent into the vanadium-containing solution under the stirring condition to obtain slurry I, wherein the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent is 1 to (0.2-1); according to the ratio of V to NH3Adding a precipitator into the slurry I under the stirring condition to obtain slurry II, wherein the molar ratio of the precipitant to the slurry I is 1: 3-9; adjusting the pH value of the slurry II to 1.5-3.0, placing the slurry II in a microwave chemical reactor, stirring for 10-50 min under the conditions of microwave power of 250-600W, stirring speed of 100-600 r/min and temperature of 80-100 ℃, and carrying out solid-liquid separation to obtain filter residue; and drying the filter residue at the temperature of 80-150 ℃ for 0.5-6 h to prepare a precursor of the vanadium nitride. The preparation method has the advantages of short preparation time and simple preparation process, the prepared vanadium nitride precursor has the characteristics of full mixing of vanadium and carbon, uniform particle size and large specific surface area, and the prepared vanadium nitride has high nitrogen content.
Description
Technical Field
The invention belongs to the technical field of precursors of vanadium nitride. In particular to a precursor of vanadium nitride and a preparation method thereof.
Background
Vanadium nitride is a novel alloy additive, improves the comprehensive mechanical properties of toughness, strength, ductility, wear resistance and the like of steel by refining crystal grains and strengthening precipitation in the steel, and can effectively improve the welding performance of the steel. Compared with ferrovanadium, the addition of vanadium nitride can save the addition of vanadium, thereby reducing the cost. The precursor of vanadium nitride is used as an intermediate product for preparing vanadium nitride, the preparation process of the precursor attracts great attention, and the good precursor can effectively optimize the preparation process of vanadium nitride and improve the comprehensive performance of vanadium nitride.
Most of the existing precursors for preparing vanadium nitride use vanadium oxide as a vanadium source, and are milled and mixed uniformly with a carbonaceous reducing agent, and a binder is added for agglomeration, so that the problem of uneven mixing of raw materials exists. Dissolving ammonium vanadate in deionized water and adding a carbonaceous reducing agent to prepare a precursor in an improved technology, wherein the preparation process is complex; and a carbonaceous reducing agent is added into the vanadium-containing solution, and a precursor is prepared by a vanadium precipitation method, wherein the method has the problems of long vanadium precipitation time, uneven particle size of the precursor, small specific surface area and the like.
"a simple vanadium nitride production method" (CN102173395A) patent technique, using V2O5Fully mixing the powder and graphite in a dry mixer according to the mass ratio of 4: 1, adding 4% polyvinyl alcohol aqueous solution into the mixed powder according to the mass ratio of 100: 15, mixing in a wet mixer, and pressing balls to obtain a precursor; and then pre-reducing the precursor at 800 ℃ for 5h, heating to 1350 ℃ for deep reduction for 6h, heating to 1600 ℃ again, nitriding and sintering for 6-10 h, and cooling to obtain vanadium nitride. The precursor is prepared by two mixing processes, the mixing process is complex, and the mixing is not uniform.
Preparing nano vanadium nitride powder by a precursor carbonization/nitridation method (Chinese ceramics [ J ].2009, 45 (11): 59-61.doi:10.16521/J. cnki. issn.1001-9642.2009.11.010), dissolving powdery ammonium metavanadate and nano carbon black in deionized water, stirring to prepare a mixed solution, heating and drying the mixed solution to obtain the precursor powder. And carbonizing/nitriding the obtained precursor to obtain the nano vanadium nitride powder. The process precursor is prepared by dissolving powdery ammonium metavanadate and nano carbon black in deionized water, stirring to prepare a mixed solution, and heating and drying the mixed solution, and has the advantages of complex preparation process and high preparation cost.
"A novel method to synthesis of vanadium nitride nanoparticles from synthesis of combustion precursors" (Journal of Alloys and compounds.2019,772,808-813.https:// doi.org/10.1016/j.jallcom.2018.09.112), ammonium metavanadate is used as vanadium source, ammonium nitrate is used as oxidant, glycine is used as fuel VO, and ultrafast SCS method is used to prepare ammonium vanadate from synthesis of vanadium nitride precursors2And preparing vanadium nitride from the precursor through reduction nitridation reaction. The method prepares VO2The precursor needs to be added with oxidant and fuel to generate heat, the process is complex, and the preparation cost is increased.
The patent technology of 'a method for preparing vanadium-nitrogen alloy by using vanadium-containing solution' (CN107058855A) is characterized in that the vanadium-containing solution is used as a vanadium source, a carbonaceous reducing agent is added into the vanadium-containing solution to precipitate vanadium for 1h, and a vanadium precipitation product is dried to obtain a precursor; then the vanadium-nitrogen alloy is prepared by high-temperature reduction nitridation, cooling and discharging, crushing and grinding and briquetting. The vanadium precipitation time in the process of preparing the precursor by the process is longer, and the prepared particles have larger particle size, wide particle distribution range and smaller specific surface area.
In summary, the existing precursor for preparing vanadium nitride still has the problem of uneven mixing after being mixed for many times, and the precursor prepared by the vanadium precipitation method has the problems of long vanadium precipitation time, uneven particle size and small specific surface area.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the preparation method of the precursor of the vanadium nitride, which has short preparation time and simple preparation process.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
step one, adding a carbonaceous reducing agent into a vanadium-containing solution under the stirring condition according to the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent of 1 to (0.2-1) to obtain slurry I.
The vanadium-containing solution is a pentavalent vanadium solution, the concentration of V ions is more than or equal to 5.0g/L, and the concentration of other impurity ions is less than or equal to 5.5 mol/L;
step two, according to V in the vanadium-containing solution and NH in the precipitator3The molar ratio of the precipitant to the slurry I is 1: 3-9, and the precipitant is added into the slurry I under the stirring condition to obtain slurry II.
Regulating the pH value of the slurry II to 1.5-3.0 to obtain slurry III; and (3) placing the slurry III in a microwave chemical reactor, stirring for 10-50 min under the conditions that the microwave power is 250-600W, the stirring speed is 100-600 r/min and the temperature is 80-100 ℃, and performing solid-liquid separation to obtain filter residues.
And step four, drying the filter residue for 0.5-6 h at the temperature of 80-150 ℃ to prepare a precursor of the vanadium nitride.
The C content of the carbonaceous reducing agent is more than or equal to 94 wt%.
The precipitant is one or more of ammonia water, ammonium bicarbonate, ammonium chloride and ammonium sulfate.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
(1) according to the invention, the carbonaceous reducing agent is added into the vanadium-containing solution, the solution is rapidly stirred, the carbonaceous reducing agent is dispersed in the solution to form slurry, vanadium and carbon in the slurry are uniformly mixed, and then the slurry is subjected to vanadium precipitation in the microwave chemical reactor to prepare the vanadium nitride precursor with uniform components.
(2) According to the invention, vanadium is precipitated in the microwave chemical reactor, and the time for preparing the precursor is 10-50 min, so that the time for preparing the precursor of the vanadium nitride is 17-83% of the time for directly precipitating the vanadium to prepare the precursor, and the preparation time is short.
(3) According to the invention, vanadium precipitation is carried out in the microwave chemical reactor, the prepared vanadium nitride precursor particles are fine and uniform, and the average particle size is reduced by 13-35% compared with the precursor particles of vanadium nitride prepared by a direct vanadium precipitation method. The surface appearance is the mixture of layers and porous, the specific surface area is increased by 36-47%, and the specific surface area is large.
(4) The nitrogen content of the vanadium nitride prepared by the method is increased by 0.5-1.4 wt% compared with the nitrogen content of the vanadium nitride prepared by the precursor of the vanadium nitride prepared by a direct vanadium precipitation method through reduction nitridation reaction, and the nitrogen content of the prepared vanadium nitride is high.
Therefore, the preparation time is short and the preparation process is simple; the prepared vanadium nitride precursor has the characteristics of full mixing of vanadium and carbon, uniform particle size and large specific surface area, and the prepared vanadium nitride has high nitrogen content.
Drawings
FIG. 1 is a graph showing the comparison of the particle size distribution of a vanadium nitride precursor prepared by the present invention and a vanadium nitride precursor prepared by a direct vanadium precipitation method;
FIG. 2 is a SEM image of a precursor of vanadium nitride prepared according to the present invention shown in FIG. 1;
FIG. 3 is an enlarged view of a portion of FIG. 2;
FIG. 4 is an SEM image of a precursor of vanadium nitride prepared by the direct vanadium precipitation method shown in FIG. 1;
fig. 5 is a partially enlarged view of B in fig. 4.
Detailed Description
The invention is further described with reference to the following figures and detailed description, without limiting its scope.
In this embodiment:
the C content of the carbonaceous reducing agent is more than or equal to 94 wt%.
The detailed description is omitted in the embodiments.
Example 1
A precursor of vanadium nitride and a preparation method thereof. The method of the embodiment comprises the following specific steps:
step one, adding a carbonaceous reducing agent into a vanadium-containing solution under the stirring condition according to the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent of 1 to (0.2-0.5), and obtaining slurry I.
The vanadium-containing solution is a pentavalent vanadium solution, the concentration of V ions is more than or equal to 5.0g/L, and the concentration of other impurity ions is less than or equal to 5.5 mol/L.
Step two, according to V in the vanadium-containing solution and NH in the precipitator3In a molar ratio of 1 to (3-5) under stirringAnd adding the precipitant into the slurry I to obtain slurry II.
Regulating the pH value of the slurry II to 1.5-2.0 to obtain slurry III; and (3) placing the slurry III in a microwave chemical reactor, stirring for 10-20 min under the conditions that the microwave power is 250-300W, the stirring speed is 100-300 r/min and the temperature is 80-850 ℃, and performing solid-liquid separation to obtain filter residues.
And step four, drying the filter residue for 4.5-6 hours at the temperature of 80-100 ℃ to obtain a precursor of the vanadium nitride.
The precipitant is one of ammonia water, ammonium bicarbonate, ammonium chloride and ammonium sulfate.
Compared with the precursor of vanadium nitride prepared by a direct vanadium precipitation method, the precursor of vanadium nitride prepared by the embodiment has the following advantages: the average particle size is reduced by 24-35%; the specific surface area is increased by 40-47%; the nitrogen content of the respectively prepared vanadium nitride is increased by 0.8-1.4 wt%.
Example 2
A precursor of vanadium nitride and a preparation method thereof. The method of the embodiment comprises the following specific steps:
step one, adding a carbonaceous reducing agent into a vanadium-containing solution under the stirring condition according to the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent of 1 to (0.5-0.6), and obtaining slurry I.
The vanadium-containing solution is a pentavalent vanadium solution, the concentration of V ions is more than or equal to 5.0g/L, and the concentration of other impurity ions is less than or equal to 5.5 mol/L.
Step two, according to V in the vanadium-containing solution and NH in the precipitator3The molar ratio of the precipitant to the slurry I is 1: 5-6, and the precipitant is added into the slurry I under the stirring condition to obtain slurry II.
Regulating the pH value of the slurry II to 1.8-2.3 to obtain slurry III; and (3) placing the slurry III in a microwave chemical reactor, stirring for 20-30 min under the conditions that the microwave power is 300-400W, the stirring speed is 200-400 r/min and the temperature is 85-90 ℃, and performing solid-liquid separation to obtain filter residues.
And step four, drying the filter residue for 3.0-4.5 hours at the temperature of 100-120 ℃ to obtain a precursor of the vanadium nitride.
The precipitant is a mixture of any two of ammonia water, ammonium bicarbonate, ammonium chloride and ammonium sulfate.
Compared with the precursor of vanadium nitride prepared by a direct vanadium precipitation method, the precursor of vanadium nitride prepared by the embodiment has the following advantages: the average particle size is reduced by 20-30%; the specific surface area is increased by 39-47%; the nitrogen content of the respectively prepared vanadium nitride is increased by 0.7-1.3 wt%.
Example 3
A precursor of vanadium nitride and a preparation method thereof. The method of the embodiment comprises the following specific steps:
step one, adding a carbonaceous reducing agent into a vanadium-containing solution under the stirring condition according to the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent of 1 to (0.6-0.8), and obtaining slurry I.
The vanadium-containing solution is a pentavalent vanadium solution, the concentration of V ions is more than or equal to 5.0g/L, and the concentration of other impurity ions is less than or equal to 5.5 mol/L.
Step two, according to V in the vanadium-containing solution and NH in the precipitator3The molar ratio of the precipitant to the slurry I is 1: 6-8, and the precipitant is added into the slurry I under the stirring condition to obtain slurry II.
Regulating the pH value of the slurry II to 2.2-2.8 to obtain slurry III; and (3) placing the slurry III in a microwave chemical reactor, stirring for 30-40 min under the conditions that the microwave power is 400-500W, the stirring speed is 3000-500 r/min and the temperature is 90-95 ℃, and performing solid-liquid separation to obtain filter residues.
And step four, drying the filter residue for 1.5-3.0 hours at the temperature of 120-140 ℃ to prepare a precursor of the vanadium nitride.
The precipitant is a mixture of any three of ammonia water, ammonium bicarbonate, ammonium chloride and ammonium sulfate.
Compared with the precursor of vanadium nitride prepared by a direct vanadium precipitation method, the precursor of vanadium nitride prepared by the embodiment has the following advantages: the average particle size is reduced by 17-25%; the specific surface area is increased by 37-44%; the nitrogen content of the respectively prepared vanadium nitride is increased by 0.7-1.2 wt%.
Example 4
A precursor of vanadium nitride and a preparation method thereof. The method of the embodiment comprises the following specific steps:
step one, adding a carbonaceous reducing agent into a vanadium-containing solution under the stirring condition according to the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent of 1 to (0.8-1) to obtain slurry I.
The vanadium-containing solution is a pentavalent vanadium solution, the concentration of V ions is more than or equal to 5.0g/L, and the concentration of other impurity ions is less than or equal to 5.5 mol/L.
Step two, according to V in the vanadium-containing solution and NH in the precipitator3The molar ratio of the precipitant to the slurry I is 1: 8-9, and the precipitant is added into the slurry I under the stirring condition to obtain slurry II.
Regulating the pH value of the slurry II to 2.5-3.0 to obtain slurry III; and (3) placing the slurry III in a microwave chemical reactor, stirring for 40-50 min under the conditions that the microwave power is 500-600W, the stirring rotating speed is 400-600 r/min and the temperature is 95-100 ℃, and carrying out solid-liquid separation to obtain filter residues.
And step four, drying the filter residue for 0.5-1.5 h at the temperature of 140-150 ℃ to prepare a precursor of the vanadium nitride.
The precipitant is a mixture of ammonia water, ammonium bicarbonate, ammonium chloride and ammonium sulfate.
Compared with the precursor of vanadium nitride prepared by a direct vanadium precipitation method, the precursor of vanadium nitride prepared by the embodiment has the following advantages: the average particle size is reduced by 13-21%; the specific surface area is increased by 36-41%; the nitrogen content of the respectively prepared vanadium nitride is increased by 0.5-1.0 wt%.
Compared with the prior art, the specific implementation mode has the following positive effects:
(1) according to the specific embodiment, the carbonaceous reducing agent is added into the vanadium-containing solution, the solution is rapidly stirred, the carbonaceous reducing agent is dispersed in the solution to form slurry, vanadium and carbon in the slurry are uniformly mixed, and then the slurry is subjected to vanadium precipitation in a microwave chemical reactor to prepare the vanadium nitride precursor with uniform components.
(2) According to the embodiment, vanadium is precipitated in the microwave chemical reactor, the time for preparing the precursor is 10-50 min, the time for preparing the precursor of the vanadium nitride prepared by the embodiment is 17-83% of the time for directly precipitating the vanadium to prepare the precursor, and the preparation time is short.
(3) The particle size distribution of the vanadium nitride precursor prepared by the present embodiment is shown in the accompanying drawing, and fig. 1 is a comparison graph of the particle size distribution of the vanadium nitride precursor prepared in example 1 and the vanadium nitride precursor prepared by the direct vanadium precipitation method; FIG. 2 is a SEM image of a precursor of vanadium nitride prepared in example 1 shown in FIG. 1; FIG. 3 is an enlarged view of a portion of FIG. 2; FIG. 4 is an SEM image of a precursor of vanadium nitride prepared by the direct vanadium precipitation method shown in FIG. 1; fig. 5 is a partially enlarged view of B in fig. 4. Analysis of FIG. 1 shows that the average particle size is reduced by 14.86%; comparing with fig. 4, it can be seen from fig. 2 that the particle size of the precursor particles of the vanadium nitride prepared in example 1 is significantly reduced and more uniform, and the precursor particles do not have significant agglomeration phenomenon; comparing with fig. 5, it can be seen from fig. 3 that the precursor structure of the vanadium nitride prepared in example 1 has a porous structure, and the specific surface area is increased by 37.58%; the nitrogen content of the vanadium nitride prepared by the precursor through the reduction nitridation process is increased by 0.55 percent.
According to the specific embodiment, vanadium precipitation is carried out in the microwave chemical reactor, the prepared vanadium nitride precursor particles are fine and uniform, and the average particle size is reduced by 13-35% compared with the precursor particles of vanadium nitride prepared by a direct vanadium precipitation method. The surface appearance is the mixture of layers and porous, the specific surface area is increased by 36-47%, and the specific surface area is large.
(4) The nitrogen content of the vanadium nitride prepared by the precursor of the vanadium nitride prepared by the specific embodiment is increased by 0.5-1.4 wt% compared with the nitrogen content of the vanadium nitride prepared by the precursor prepared by the direct vanadium precipitation method, and the using effect is good.
Therefore, the preparation time of the specific embodiment is short and the preparation process is simple; the prepared vanadium nitride precursor has the characteristics of full mixing of vanadium and carbon, uniform particle size and large specific surface area, and the prepared vanadium nitride has high nitrogen content.
Claims (4)
1. A preparation method of a precursor of vanadium nitride is characterized by comprising the following steps:
step one, adding a carbonaceous reducing agent into a vanadium-containing solution under the stirring condition according to the mass ratio of V in the vanadium-containing solution to C in the carbonaceous reducing agent of 1 to (0.2-1) to obtain slurry I;
the vanadium-containing solution is a pentavalent vanadium solution, the concentration of V ions is more than or equal to 5.0g/L, and the concentration of other impurity ions is less than or equal to 5.5 mol/L;
step two, according to V in the vanadium-containing solution and NH in the precipitator3The molar ratio of the precipitant to the slurry I is 1: 3-9, and the precipitant is added into the slurry I under the stirring condition to obtain slurry II;
regulating the pH value of the slurry II to 1.5-3.0 to obtain slurry III; placing the slurry III in a microwave chemical reactor, stirring for 10-50 min under the conditions that the microwave power is 250-600W, the stirring speed is 100-600 r/min and the temperature is 80-100 ℃, and carrying out solid-liquid separation to obtain filter residues;
and step four, drying the filter residue for 0.5-6 h at the temperature of 80-150 ℃ to prepare a precursor of the vanadium nitride.
2. The method for preparing the precursor of vanadium nitride according to claim 1, wherein the carbonaceous reducing agent has a C content of 94 wt% or more.
3. The method of claim 1, wherein the precipitating agent is one or more of ammonia, ammonium bicarbonate, ammonium chloride, and ammonium sulfate.
4. A precursor of vanadium nitride, characterized in that the precursor of vanadium nitride is a precursor of vanadium nitride prepared according to the preparation method of any one of claims 1 to 3.
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Citations (6)
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|---|---|---|---|---|
| US4562057A (en) * | 1984-03-29 | 1985-12-31 | Union Carbide Corporation | Preparation of low-carbon vanadium nitride |
| CN103708429A (en) * | 2013-12-19 | 2014-04-09 | 河南工业大学 | Preparation method of nano vanadium nitride/chromium nitride composite powder |
| CN104016314A (en) * | 2014-06-26 | 2014-09-03 | 济南顺源新材料科技有限公司 | Preparation method of vanadium nitride |
| CN106498266A (en) * | 2016-12-01 | 2017-03-15 | 武汉科技大学 | A kind of preparation method of VN alloy |
| CN107058855A (en) * | 2017-04-12 | 2017-08-18 | 武汉科技大学 | It is a kind of with the method that VN alloy is prepared containing vanadium solution |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
-
2021
- 2021-12-06 CN CN202111475935.1A patent/CN114394578A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4562057A (en) * | 1984-03-29 | 1985-12-31 | Union Carbide Corporation | Preparation of low-carbon vanadium nitride |
| CN103708429A (en) * | 2013-12-19 | 2014-04-09 | 河南工业大学 | Preparation method of nano vanadium nitride/chromium nitride composite powder |
| CN104016314A (en) * | 2014-06-26 | 2014-09-03 | 济南顺源新材料科技有限公司 | Preparation method of vanadium nitride |
| CN106498266A (en) * | 2016-12-01 | 2017-03-15 | 武汉科技大学 | A kind of preparation method of VN alloy |
| CN107058855A (en) * | 2017-04-12 | 2017-08-18 | 武汉科技大学 | It is a kind of with the method that VN alloy is prepared containing vanadium solution |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
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