CN111232980A - Preparation method of vanadium carbide powder - Google Patents
Preparation method of vanadium carbide powder Download PDFInfo
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- CN111232980A CN111232980A CN202010208854.4A CN202010208854A CN111232980A CN 111232980 A CN111232980 A CN 111232980A CN 202010208854 A CN202010208854 A CN 202010208854A CN 111232980 A CN111232980 A CN 111232980A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a preparation method of vanadium carbide powder, belonging to the technical field of vanadium metallurgy. The invention provides a novel method for preparing vanadium carbide powder, which comprises the steps of taking vanadium-containing powder as a vanadium source, taking chlorine as a chlorination medium, taking a fluidized bed as a reaction carrier, carrying out boiling chlorination, and distilling an obtained vanadium chloride primary product at 110-140 ℃ and 160-180 ℃ in two steps to obtain a high-purity vanadium chloride intermediate product; heating and gasifying the intermediate product, and mixing with high-purity CH4And H2Mixing, then contacting with a reaction carrier to carry out carbonization reaction, and obtaining the high-purity superfine vanadium metal powder. The method can realize the preparation of high-purity vanadium chloride with low content of interstitial impurities, can also perform gas-gas reaction at relatively low temperature to obtain vanadium carbide powder with nano size, and is favorable for industrial production and application.
Description
Technical Field
The invention belongs to the technical field of vanadium metallurgy, and particularly relates to a preparation method of vanadium carbide powder.
Background
Vanadium carbide has the general characteristics of transition metal carbides with higher hardness, melting point, high-temperature strength and the like, and has good electric conductivity and thermal conductivity, so that the vanadium carbide can be widely applied to the fields of ferrous metallurgy, hard alloys, electronic products, catalysts, high-temperature coating materials and the like. The vanadium carbide can improve the comprehensive performances of the steel such as wear resistance, corrosion resistance, toughness, strength, ductility, thermal fatigue resistance and the like, and can be used as a wear-resistant material in different cutting and wear-resistant tools. In addition, the vanadium carbide can be used as a grain inhibitor or used as a hard alloy independently to be applied to the fields of hard alloy and metal ceramic, so that the growth of hard alloy grains in the sintering process is prevented, and the mechanical properties of the hard alloy and the metal ceramic are improved. Meanwhile, vanadium carbide is widely used as a novel catalyst due to its high activity, selectivity, stability and resistance to catalyst poisoning in hydrocarbon reactions. With the wider application of the hard alloy in high and new technology weaponry, advanced science and technology and nuclear energy, the preparation of the ultrafine vanadium carbide powder and the market demand are more urgent.
CN200610021329 has powdered ammonium vanadate, carbon reducer and catalyst dissolved in deionized water or distilled water in certain proportion, and through heating and drying, vanadium and carbon containing precursor powder is obtained, which is carbonized in high temperature reactor at certain temperature and atmosphere to obtain vanadium carbide powder with average grain size smaller than 100nm and homogeneous grain size distribution. CN201410785489 volatilizes, concentrates and decomposes a solution prepared from a vanadium source, a carbon source and an auxiliary agent according to a certain proportion to obtain precursor powder, and reacts the precursor powder for a certain time at the temperature of 700-1300 ℃ to obtain vanadium carbide powder with good dispersibility and granularity smaller than 50 nm. CN201710498523 discloses a method for preparing nano vanadium carbide powder, which comprises mixing and grinding a carbon source and ammonium metavanadate according to a certain proportion, and then carrying out heat preservation reaction in a tube furnace under a certain condition to obtain the nano vanadium carbide powder with uniform chemical composition, uniform morphology and size and high stability.
It can be known from the above publications and patents that the preparation process of vanadium carbide mainly comprises carbothermic reduction, gas phase reduction, precursor method, etc., wherein the preparation process of nano vanadium carbide powder is mainly prepared by precursor method, and the main idea is to mix and dissolve different vanadium sources and carbon sources in a liquid carrier, obtain precursor powder containing vanadium and carbon by heating and drying, etc., and sinter the obtained precursor powder under certain conditions to finally obtain vanadium carbide product. However, carbothermic, gas phase reduction processes generally do not allow the obtainment of vanadium carbide powders of higher purity and finer particle size; the precursor method has the problems of long process flow, difficult control of the particle size, sintering temperature and sintering time of precursor powder, and difficult control of the quality of large-proportion non-stoichiometric components and large-powder particle size distribution range lamp products.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of vanadium carbide powder, which comprises the following steps:
A. chlorination of vanadium-containing powder: boiling and chlorinating by taking vanadium-containing powder as a vanadium source and chlorine as a chlorination medium to obtain a primary vanadium chloride product;
B. primary purification of vanadium chloride: performing two-step distillation on the primary vanadium chloride product at 110-140 ℃ and 160-180 ℃, and collecting distillate obtained during distillation at 160-180 ℃ to obtain a high-purity vanadium chloride intermediate product;
C. high-temperature carbonization of vanadium chloride: heating and gasifying vanadium chloride intermediate product, and mixing with high-purity CH4And H2The mixed gas is mixed and then contacts with a reaction carrier to carry out carbonization reaction, and high-purity superfine vanadium powder is obtained.
In the preparation method of the vanadium carbide powder, in the step A, the high-purity vanadium-containing powder is vanadium-containing intermediate alloy powder, the purity of the vanadium-containing intermediate alloy powder is more than or equal to 99.0%, the granularity of the vanadium-containing intermediate alloy powder is less than or equal to 50 meshes, the contents of non-metallic inclusions of O, Si, C, P and S are respectively not higher than 0.20%, 0.40%, 0.10%, 0.05% and 0.05%, and the contents of other impurities are not higher than 0.2%.
Preferably, in the preparation method of the vanadium carbide powder, in the step a, the high-purity vanadium-containing powder is high-grade vanadium-containing intermediate alloy powder such as FeV80, AlV85 and the like.
In the preparation method of the vanadium carbide powder, in the step A, the purity of the chlorine is more than or equal to 99.8%.
In the preparation method of the vanadium carbide powder, in the step A, the boiling chlorination temperature is 400-700 ℃.
In the preparation method of the vanadium carbide powder, in the step C, the temperature for heating and gasifying the vanadium chloride is 500-700 ℃.
In the preparation method of the vanadium carbide powder, in the step C, vanadium chloride gas and high-purity CH are mixed by a spray gun4And H2The temperature of the wall of the spray gun is 500-700 ℃, and the pressure is 0.5-2.0 MPa.
In the preparation method of the vanadium carbide powder, in the step C, CH is added before mixing4And H2The mixed gas is preheated to 300-500 ℃.
Wherein, in the step C, the CH is used as the raw material for preparing the vanadium carbide powder4And H2Is 1: 1-5: 1.
in the preparation method of the vanadium carbide powder, in the step C, the reaction carrier is a multilayer inert metal high-temperature net, and the temperature of the reaction carrier is 1200-1500 ℃.
The invention has the beneficial effects that:
the invention takes high-purity vanadium-containing intermediate alloy as a raw material, converts all vanadium in the raw material into vanadium chloride by a chlorination process, avoids introducing process oxygen from the source, obtains a high-purity vanadium chloride intermediate by two-step distillation, realizes the molecular mixing of the raw materials by the gas phase contact between the gasified vanadium chloride and a reducing agent, reduces the reaction diffusion distance, is beneficial to the rapid nucleation of a product in a non-equilibrium state, accelerates the reaction process, can realize the preparation of high-purity vanadium chloride with low content of interstitial impurities, can also carry out gas-gas reaction at a relatively low temperature to obtain vanadium carbide powder with a nano size, and is beneficial to industrial production and application.
Detailed Description
Specifically, the preparation method of the vanadium carbide powder comprises the following steps:
A. chlorination of vanadium-containing powder: boiling and chlorinating by taking vanadium-containing powder as a vanadium source and chlorine as a chlorination medium to obtain a primary vanadium chloride product;
B. primary purification of vanadium chloride: performing two-step distillation on the primary vanadium chloride product at 110-140 ℃ and 160-180 ℃, and collecting distillate obtained during distillation at 160-180 ℃ to obtain a high-purity vanadium chloride intermediate product;
C. high-temperature carbonization of vanadium chloride: heating and gasifying vanadium chloride intermediate product, and mixing with high-purity CH4And H2Mixing, then contacting with a reaction carrier to carry out carbonization reaction, and obtaining the high-purity superfine vanadium metal powder.
The method provides a high-quality intermediate raw material for the subsequent preparation of vanadium carbide, and in the step A, the high-purity vanadium-containing intermediate alloy is used as the raw material, and vanadium in the raw material is completely converted into vanadium chloride through a chlorination process, so that the introduction of process oxygen is avoided from the source. Wherein, the high-purity vanadium-containing powder is high-grade vanadium-containing intermediate alloy powder, the purity of the high-purity vanadium-containing powder is more than or equal to 99.0 percent, the granularity of the high-purity vanadium-containing intermediate alloy powder is less than or equal to 50 meshes, the non-metal inclusion contents of O, Si, C, P and S are respectively not higher than 0.20 percent, 0.40 percent, 0.10 percent, 0.05 percent and 0.05 percent, and the contents of other impurities are not higher than 0.2; the high-grade alloy can reduce chlorine consumption and control the later separation effect, so that the high-grade alloy such as FeV80, AlV85 and the like has the best effect. Boiling chlorination has no strict requirements on the reactor, but the fluidized bed is the best choice for powder chlorination effect.
In the step A, the purity of the chlorine is more than or equal to 99.8 percent; the temperature of the boiling chlorination is 400-700 ℃.
Chlorination products obtained in the chlorination process are different metal chlorides, the boiling points and the saturated vapor pressures of the different metal chlorides are obviously different, wherein the boiling point of the vanadium chloride is 140-160 ℃, low-boiling-point chlorides in the mixed chlorides can be removed through low-temperature distillation, then high-temperature distillation and two-step distillation are carried out to obtain high-purity vanadium chloride, and the residual substances in the fluidized bed are high-melting-point metal chlorides (the boiling points are more than or equal to 180 ℃); the purity of the obtained high-purity vanadium chloride can reach more than 99.5 percent.
In the step C, vanadium chloride is heated and gasified at 500-700 ℃, and then the vanadium chloride is mixed with CH under the pressure of 0.5-2.0 MPa by a spray gun with the wall temperature of 500-700 DEG C4And H2The volume ratio is 1: 1-5: 1, mixing the mixed gas; the main purpose of controlling the wall temperature is to ensure that the feedstock is in a vaporized state,meanwhile, a certain preheating effect is achieved; the pressure is controlled to mainly ensure the flow rate in the reaction process and the temperature of a reaction interface to be stable; meanwhile, the mixed gas is preheated to 300-500 ℃, the gasification state of the vanadium chloride is ensured, and the phenomenon that the vanadium chloride is liquefied by cooling due to the entering of the mixed gas at normal temperature is avoided.
And C, performing carbonization reaction on the reaction system on a reaction carrier of a multilayer inert metal high-temperature net at the temperature of 1200-1500 ℃. The multilayer inert metal high-temperature net has the effects that firstly, the stable temperature condition required by reduction is met, and firstly, the contact reaction area of gas under the high-temperature condition is increased; in addition, the invention realizes the molecular mixing among the raw materials and reduces the reaction diffusion distance by the gas phase contact between the gasified vanadium chloride and the reducing agent, thereby being beneficial to the rapid nucleation of the product in a non-equilibrium state and accelerating the reaction process; the carbonization temperature is lower than that of the conventional carbonization temperature.
In the present invention, unless otherwise specified, the purity and the content are both in mass percent.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
Performing chlorination reaction on vanadium-aluminum alloy powder with the purity of 99.6 percent, the average particle size of 50 meshes and the vanadium mass fraction of 84.9 percent and chlorine with the purity of 99.5 percent in a fluidized bed at the temperature of 400 ℃, performing distillation operation twice on the obtained liquid chlorination product at the temperature of 110 ℃ and 180 ℃ respectively, and collecting the obtained liquid chlorination product at a second distillation condensation port to obtain a vanadium chloride intermediate product. Heating and vaporizing the obtained vanadium chloride intermediate product at 500 ℃, and passing through a spray gun with the wall temperature of 500 ℃ and the spray gun pressure of 0.5MPa, a preheating temperature of 300 ℃ and a volume ratio of 1: high purity CH of 14And H2Mixing the mixed gas, and then carrying out contact reaction with a reaction carrier with the surface temperature of 1000 ℃ to obtain a reaction product, namely vanadium carbide powder.
Through the operation, the purity of the obtained high-purity vanadium chloride intermediate product is 99.5 percent, and the loss rate of vanadium chloride is 39.8 percent; the purity of the obtained vanadium carbide powder is 99.6 percent, the average particle size of the powder is 25nm, and the vanadium loss rate in the carbonization process is 38.2 percent. The comprehensive vanadium yield is 37.2 percent (the reduction temperature is low, the reduction effect is poor, the yield is low, but the powder granularity is finest, the raw material purity is low, the secondary distillation temperature difference is large, and the product purity is relatively low).
Example 2
Performing chlorination reaction on vanadium-aluminum alloy powder with the purity of 99.9 percent, the average particle size of 200 meshes and the vanadium mass fraction of 85.1 percent and chlorine with the purity of 99.9 percent in a fluidized bed at the temperature of 600 ℃, performing distillation operation twice on the obtained liquid chlorination product at the temperature of 125 ℃ and 170 ℃ respectively, and collecting the obtained liquid chlorination product at a second distillation condensation port to obtain a vanadium chloride intermediate product. Heating and vaporizing the obtained vanadium chloride intermediate product at 600 ℃, and passing through a spray gun with the wall temperature of 700 ℃ and the spray gun pressure of 1.0MPa, a preheating temperature of 500 ℃ and a volume ratio of 3: high purity CH of 14And H2Mixing the mixed gas, and then carrying out contact reaction with a reaction carrier with the surface temperature of 1300 ℃ to obtain a reaction product, namely vanadium carbide powder.
Through the operation, the purity of the obtained high-purity vanadium chloride intermediate product is 99.9 percent, and the loss rate of vanadium chloride is 4.5 percent; the purity of the obtained vanadium carbide powder is 99.9 percent, the average particle size of the powder is 35nm, and the vanadium loss rate in the carbonization process is 12.8 percent. The overall vanadium yield was 83.3%.
Example 3
Performing chlorination reaction on vanadium-aluminum alloy powder with the purity of 99.9 percent, the average particle size of 200 meshes and the vanadium mass fraction of 85.1 percent and chlorine with the purity of 99.9 percent in a fluidized bed at the temperature of 600 ℃, performing distillation operation twice on the obtained liquid chlorination product at the temperature of 140 ℃ and 160 ℃ respectively, and collecting the obtained liquid chlorination product at a second distillation condensation port to obtain a vanadium chloride intermediate product. Heating and vaporizing the obtained vanadium chloride intermediate product at 700 ℃, and passing through a spray gun with the wall temperature of 700 ℃ and the spray gun pressure of 2.0MPa, a preheating temperature of 500 ℃ and a volume ratio of 5: high purity CH of 14And H2Mixing the mixed gas, and then carrying out contact reaction with a reaction carrier with the surface temperature of 1500 ℃ to obtain a reaction product, namely vanadium carbide powder.
Through the operation, the purity of the obtained high-purity vanadium chloride intermediate product is 99.9 percent, and the loss rate of vanadium chloride is 4.5 percent; the purity of the obtained vanadium carbide powder is 99.9 percent, the average particle size of the powder is 55nm, and the vanadium loss rate in the carbonization process is 4.8 percent. The comprehensive vanadium yield is 90.9%.
Example 4
Performing chlorination reaction on vanadium-aluminum alloy powder with the purity of 99.8 percent, the average particle size of 200 meshes and the vanadium mass fraction of 85.1 percent and chlorine with the purity of 99.9 percent in a fluidized bed at the temperature of 500 ℃, performing distillation operation twice on the obtained liquid chlorination product at the temperature of 125 ℃ and 170 ℃ respectively, and collecting the obtained liquid chlorination product at a second distillation condensation port to obtain a vanadium chloride intermediate product. Heating and vaporizing the obtained vanadium chloride intermediate product at 600 ℃, and passing through a spray gun with the wall temperature of 600 ℃ and the spray gun pressure of 1.0MPa, a preheating temperature of 400 ℃ and a volume ratio of 3: high purity CH of 14And H2Mixing the mixed gas, and then carrying out contact reaction with a reaction carrier with the surface temperature of 1300 ℃ to obtain a reaction product, namely vanadium carbide powder.
Through the operation, the purity of the obtained high-purity vanadium chloride intermediate product is 99.8 percent, and the loss rate of vanadium chloride is 9.8 percent; the purity of the obtained vanadium carbide powder is 99.9 percent, the average particle size of the powder is 35nm, and the vanadium loss rate in the carbonization process is 11.8 percent. The overall vanadium yield was 79.5%.
Example 5
Performing chlorination reaction on ferrovanadium powder with the purity of 99.8 percent, the average particle size of 200 meshes and the vanadium mass fraction of 80.8 percent and chlorine with the purity of 99.9 percent in a fluidized bed at 700 ℃, performing distillation operation twice on the obtained liquid chlorination products at 140 ℃ and 160 ℃ respectively, and collecting the high-purity vanadium chloride intermediate product at a second distillation condensation port. Heating and vaporizing the obtained vanadium chloride intermediate product at 700 ℃, and passing through a spray gun with the wall temperature of 700 ℃ and the spray gun pressure of 2.0MPa, a preheating temperature of 500 ℃ and a volume ratio of 5: high purity CH of 14And H2Mixing the mixed gas, and then carrying out contact reaction with a reaction carrier with the surface temperature of 1500 ℃ to obtain a reaction product, namely vanadium carbide powder.
Through the operation, the purity of the obtained high-purity vanadium chloride intermediate product is 99.9 percent, and the loss rate of vanadium chloride is 5.3 percent; the purity of the obtained vanadium carbide powder is 99.9 percent, the average particle size of the powder is 60nm, and the vanadium loss rate in the carbonization process is 7.5 percent. The overall vanadium yield was 87.6%.
Claims (9)
1. The preparation method of the vanadium carbide powder is characterized by comprising the following steps: the method comprises the following steps:
A. chlorination of vanadium-containing powder: boiling and chlorinating by taking vanadium-containing powder as a vanadium source and chlorine as a chlorination medium to obtain a primary vanadium chloride product;
B. primary purification of vanadium chloride: performing two-step distillation on the primary vanadium chloride product at 110-140 ℃ and 160-180 ℃, and collecting distillate obtained during distillation at 160-180 ℃ to obtain a high-purity vanadium chloride intermediate product;
C. high-temperature carbonization of vanadium chloride: heating and gasifying vanadium chloride intermediate product, and mixing with high-purity CH4And H2The mixed gas is mixed and then contacts with a reaction carrier to carry out carbonization reaction, and high-purity superfine vanadium powder is obtained.
2. The method for producing vanadium carbide powder according to claim 1, characterized in that: in the step A, the high-purity vanadium-containing powder is vanadium-containing intermediate alloy powder, the purity of the vanadium-containing intermediate alloy powder is more than or equal to 99.0%, the granularity of the vanadium-containing intermediate alloy powder is less than or equal to 50 meshes, the non-metal impurity contents of O, Si, C, P and S are respectively not higher than 0.20%, 0.40%, 0.10%, 0.05% and 0.05%, and the contents of other impurities are not higher than 0.2%.
3. The method for producing vanadium carbide powder according to claim 1, characterized in that: in the step A, the purity of the chlorine is more than or equal to 99.8 percent.
4. The method for producing vanadium carbide powder according to claim 1, characterized in that: in the step A, the boiling chlorination temperature is 400-700 ℃.
5. The method for producing vanadium carbide powder according to claim 1, characterized in that: in the step C, the heating and gasifying temperature of the vanadium chloride is 500-700 ℃.
6. According to the claimsThe method for producing a vanadium carbide powder according to claim 1, characterized in that: in the step C, vanadium chloride gas and high-purity CH are sprayed by a spray gun4And H2The temperature of the wall of the spray gun is 500-700 ℃, and the pressure is 0.5-2.0 MPa.
7. The method for producing vanadium carbide powder according to claim 1, characterized in that: in step C, high purity H is added before mixing2And CH4The mixed gas is preheated to 300-500 ℃.
8. The method for producing vanadium carbide powder according to claim 1, characterized in that: in step C, the CH4And H2Is 1: 1-5: 1.
9. the method for producing a vanadium carbide powder according to any one of claims 1 to 8, characterized in that: in the step C, the reaction carrier is a multilayer inert metal high-temperature net, and the temperature of the reaction carrier is 1200-1500 ℃.
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Application publication date: 20200605 |