CN110964962A - Preparation method of 50 ferrovanadium and 50 ferrovanadium prepared by using same - Google Patents
Preparation method of 50 ferrovanadium and 50 ferrovanadium prepared by using same Download PDFInfo
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- CN110964962A CN110964962A CN201911338576.8A CN201911338576A CN110964962A CN 110964962 A CN110964962 A CN 110964962A CN 201911338576 A CN201911338576 A CN 201911338576A CN 110964962 A CN110964962 A CN 110964962A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
- C22C27/025—Alloys based on vanadium, niobium, or tantalum alloys based on vanadium
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0066—Preliminary conditioning of the solid carbonaceous reductant
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/006—Making ferrous alloys compositions used for making ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C35/00—Master alloys for iron or steel
- C22C35/005—Master alloys for iron or steel based on iron, e.g. ferro-alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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Abstract
The invention relates to a preparation method of 50 ferrovanadium and 50 ferrovanadium prepared by the same. The preparation method comprises the following steps: (1) uniformly mixing a vanadium-containing raw material, a carbon-containing raw material and an iron-containing raw material; (2) and (3) putting the mixed raw material obtained in the step (1) into a pushed slab kiln filled with protective gas for carbon-thermal solid-phase reduction to obtain 50 ferrovanadium. The preparation method does not need to be vacuumized, can prepare the qualified 50 ferrovanadium in the pushed slab kiln under the protective gas environment, has the recovery rate of vanadium of more than 98 percent, has the advantages of simple flow, low production cost and easily obtained raw materials, and can realize continuous large-scale production by utilizing the common pushed slab kiln.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a preparation method of 50 ferrovanadium and 50 ferrovanadium prepared by the same.
Background
Ferrovanadium is a vanadium microalloyed intermediate alloy which is most widely applied in the steel industry at present, and is widely applied to the industries of mechanical manufacturing, aerospace, construction of roads and bridges and the like.
Ferrovanadium is an important alloy additive in the steel industry, mainly plays a role in refining grains, increasing the strength of steel and inhibiting the aging effect of steel, and is specifically represented as follows: in the alloy structural steel, ferrovanadium has the function of refining grains and increasing the strength and toughness of the steel; in spring steel, ferrovanadium is used in combination with chromium or manganese, so that the elastic limit of the steel is increased, and the quality of the steel is improved; in the tool steel, the ferrovanadium has the functions of refining the structure and the crystal grains of the steel, increasing the tempering stability of the steel, enhancing the secondary hardening effect of the steel, improving the wear resistance of the steel and prolonging the service life of the tool; vanadium added into cast iron promotes the formation of pearlite due to the formation of carbide, so that cementite is stable, the shape of graphite particles is fine and uniform, and the crystal grains of a matrix are refined, thereby improving the hardness, tensile strength and wear resistance of a casting.
The preparation principle of the ferrovanadium alloy is mainly that a reducing agent is used for reducing vanadium-containing oxide and other vanadium-containing raw materials, and the vanadium-containing oxide and other vanadium-containing raw materials are mutually dissolved with an iron melt in a high-temperature molten state to obtain the ferrovanadium alloy. The traditional 50 ferrovanadium smelting methods include an aluminothermic method, an electric silicothermic method and a vacuum furnace smelting method. (1) The aluminothermic process adopts a strong reducing agent aluminum, so that a large amount of heat can be generated in the process of reducing vanadium oxide, the heat requirement of the aluminothermic smelting process can be met, the reaction temperature is reduced by adding return ferrovanadium scraps, and the slag viscosity is reduced by adding lime, magnesia and fluorite, so that the smelting recovery rate of vanadium is only 90-95%. Therefore, the aluminothermic method has the advantages of low vanadium recovery rate, intermittent production and higher price of the reducing agent aluminumAnd (4) the defect. (2) The electro-silicothermic process uses a mixed reductant of ferrosilicon and aluminum to produce ferrovanadium containing 40-60% V in an improved three-phase alkaline electric arc furnace. The raw materials used by the method comprise vanadium pentoxide fuse pieces, aluminum blocks, lime and steel scraps or steel scraps of plain carbon steel. Since the vanadium suboxides are basic compounds, which adversely affect the reduction of vanadium, lime is added to increase the basicity of the slag and promote the reduction of the vanadium oxides. The smelting process of the method comprises two steps of reduction and refining: 1) in the reduction period, ferrosilicon and aluminum are used for reducing vanadium oxide to obtain vanadium-silicon-iron alloy with high silicon content; 2) in the refining stage, use V2O5The high slag refines the ferrovanadium-silicon alloy, and reduces silicon to obtain ferrovanadium. The method can generate a large amount of SiO byproduct2And the smelting recovery rate is only 90-95%, and the method has the defects of low vanadium recovery rate, intermittent production, complex operation and higher price of a reducing agent. (3) The vacuum furnace smelting method comprises the steps of adding water into vanadium oxide, a reducing agent and iron powder for mixing, then pressing into blocks, drying, carrying out vacuum smelting, and finally reacting to generate ferrovanadium. Although the method can adopt cheap carbon powder as a reducing agent and improve the smelting recovery rate to more than 95 percent, the method still has the defects of complex process, high production cost of a vacuum furnace, intermittent production and the like, and can not meet the continuous large-scale production requirement.
CN108165781A discloses a preparation method of FeV50 with low Mn content, which still adopts an aluminothermic method, and only adjusts parameters of a process for smelting FeV50 by a conventional tilting furnace electro-aluminothermic method, specifically adjusts arc striking voltage and current, slag-poor voltage and current, and refining voltage and current. Although the preparation method can prepare FeV50 with low Mn content, the thermit method with high energy consumption, high cost and high pollution is still adopted, so that the application range of the preparation method is limited, and the continuous large-scale production requirement cannot be met.
CN110042238A discloses a production method of a high-quality FeV50 alloy, which mainly comprises the steps of electro-aluminothermic smelting, casting and cooling, and specifically comprises the steps of tapping FeV50 alloy liquid which meets the requirements, casting the FeV50 alloy liquid into an ingot mold, starting a water cooling system after 14-16min, closing the water cooling system after 110-130min, and removing the furnace after 20-24h to obtain the high-quality FeV50 alloy. Although the production method can prepare the high-quality FeV50 alloy required by the grade A, the aluminothermic method with high energy consumption, high cost and high pollution is still adopted, so that the application range of the preparation method is limited, and the continuous large-scale production requirement cannot be met.
CN106854700A discloses a method for preparing a ferrovanadium alloy, which comprises the steps of preparing mixed pellets, carrying out reduction roasting to obtain metallized pellets, and continuously charging and smelting to obtain the ferrovanadium alloy. Although the method comprehensively utilizes iron in the vanadium slag to replace steel scraps to smelt the ferrovanadium, compared with the existing ferrovanadium smelting process, the method saves the comprehensive energy consumption by more than 20 percent, reduces the consumption of aluminum particles by more than 70 percent and reduces the consumption of the steel scraps by 100 percent, but still adopts an aluminothermic method with high energy consumption, high cost and high pollution, so that the application range of the preparation method is limited, and the continuous large-scale production requirement cannot be met.
CN105838971A discloses a preparation method of FeV50 alloy, which adopts a two-stage smelting process of silicon for pre-reduction and aluminum for refining reduction, and adopts ferrosilicon as a smelting mixture of a main reducing agent for electro-silicothermic reduction reaction in the first stage of smelting; in the second smelting stage, smelting mixture with metal aluminum as main reductant is used for electro-aluminothermic reduction reaction. The preparation method improves the comprehensive recovery rate of ferrovanadium smelting and reduces the use proportion of unit reducing agent metal aluminum, but still has the defects of complex process, higher cost and intermittent production.
CN109722581A discloses 85-90 ferrovanadium and a preparation method thereof, the preparation method comprises the steps of adding powder vanadium oxide, carbon powder, iron oxide powder and a composite binder into a mixer, adding water into the mixer for mixing uniformly, adding the mixed raw materials into a ball press or a briquetting machine for ball pressing or briquetting, drying the wet pressed balls or briquettes in a dryer, then filling the dried pressed balls or briquettes into a vacuum resistance furnace or a vacuum intermediate frequency electric furnace, vacuumizing in a closed manner, heating, and performing carbothermic solid phase reduction, thereby producing the 85-90 ferrovanadium alloy. Although the preparation method improves the recovery rate of vanadium to 98% or above, the preparation method still has the defects of complex process, high production cost of a vacuum furnace, intermittent production and the like, and cannot meet the continuous large-scale production requirement.
Therefore, there is a need to develop a new method for preparing 50 ferrovanadium.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a preparation method of 50 ferrovanadium and 50 ferrovanadium prepared by the same. The preparation method comprises the following steps: (1) uniformly mixing a vanadium-containing raw material, a carbon-containing raw material and an iron-containing raw material; (2) and (3) putting the mixed raw material obtained in the step (1) into a pushed slab kiln filled with protective gas for carbon-thermal solid-phase reduction to obtain 50 ferrovanadium. The preparation method does not need to be vacuumized, can prepare the qualified 50 ferrovanadium in the pushed slab kiln under the protective gas environment, has the recovery rate of vanadium of more than 98 percent, has the advantages of simple flow, low production cost and easily obtained raw materials, and can realize continuous large-scale production by utilizing the common pushed slab kiln.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) uniformly mixing a vanadium-containing raw material, a carbon-containing raw material and an iron-containing raw material;
(2) and (3) putting the mixed raw material obtained in the step (1) into a pushed slab kiln filled with protective gas for carbon-thermal solid-phase reduction to obtain 50 ferrovanadium.
The preparation method of the invention does not adopt high-valence aluminum in an aluminothermic method and an electro-silicothermic method as a reducing agent, and does not adopt a vacuum furnace with high production cost in a vacuum furnace smelting method, but further simplifies the preparation method into two steps of uniformly mixing raw materials and carrying out carbothermic solid-phase reduction in a pushed slab kiln filled with protective gas, does not need to be vacuumized, can improve the recovery rate of vanadium to more than 98 percent, not only has the advantages of simple flow, low production cost and easily obtained raw materials, but also can realize continuous large-scale production by utilizing a common pushed slab kiln.
As a preferable technical scheme of the invention, the vanadium-containing raw material, the carbon-containing raw material and the iron-containing raw material in the step (1) are proportioned according to the mass ratio of elements.
Preferably, the element mass ratio is V: c: fe 1000 (620) -300 (800) -1100, such as 1000:620:800, 1000:600:850, 1000:500:900, 1000:400:1000, or 1000:300:1100, etc., but is not limited to the values listed, and other values not listed within the range of values are also applicable.
As a preferred technical solution of the present invention, in the step (1), the vanadium-containing raw material is any one or a mixture of at least two of vanadium dioxide, vanadium trioxide, vanadium pentoxide, ammonium metavanadate or ammonium polyvanadate, and typical but non-limiting examples of the mixture are: mixtures of vanadium dioxide and vanadium trioxide, mixtures of vanadium trioxide and vanadium pentoxide, mixtures of ammonium metavanadate and ammonium polyvanadate or mixtures of vanadium dioxide, vanadium trioxide and vanadium pentoxide, and the like.
Preferably, the vanadium-containing raw material in step (1) has a particle size of 50 to 300 mesh, such as 50 mesh, 70 mesh, 100 mesh, 120 mesh, 150 mesh, 180 mesh, 200 mesh, 230 mesh, 250 mesh, 280 mesh or 300 mesh, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred technical scheme of the invention, the carbonaceous raw material in the step (1) is any one or a mixture of at least two of graphite, coke, tar or asphalt, and typical but non-limiting examples of the mixture are as follows: a mixture of graphite and coke, a mixture of coke and tar or a mixture of tar and pitch, etc.
The invention adopts the carbon-containing raw material with low price as the reducing agent, and the carbon-containing raw material can be not only graphite or coke with high C purity, even carbon powder, but also hydrocarbon mixture tar or asphalt with lower C purity, and the like, thereby further reducing the production cost.
As a preferred technical scheme of the invention, the iron-containing raw material in the step (1) is any one or a mixture of at least two of iron, ferric oxide and ferroferric oxide, and typical but non-limiting examples of the mixture are as follows: mixtures of iron and ferric oxide, mixtures of ferric oxide and ferroferric oxide or mixtures of iron and ferroferric oxide, and the like.
Preferably, the iron-containing material of step (1) has a particle size of 50 to 300 mesh, such as 50 mesh, 70 mesh, 100 mesh, 120 mesh, 150 mesh, 180 mesh, 200 mesh, 230 mesh, 250 mesh, 280 mesh or 300 mesh, but not limited to the recited values, and other values not recited in this range are equally applicable.
As a preferred technical solution of the present invention, the shielding gas in step (2) is any one or a mixture of at least two of nitrogen, helium, neon or argon, and typical but non-limiting examples of the mixture are: a mixture of nitrogen and helium, a mixture of helium and neon, or a mixture of neon and argon, and the like.
Preferably, the pressure of the shielding gas in step (2) is 0 to 80Pa, such as 0Pa, 10Pa, 20Pa, 30Pa, 40Pa, 50Pa, 60Pa, 70Pa, or 80Pa, but is not limited to the recited values, and other values not recited within the range are equally applicable.
The pressure of the protective gas belongs to micro-positive pressure, can be consistent with the pressure of external atmospheric pressure, and can also be slightly higher than the pressure of the external atmospheric pressure, so that extra requirements on the tightness in the existing equipment can not be generated, and unnecessary waste of the protective gas can not be caused.
In a preferred embodiment of the present invention, the reaction time of the carbothermic solid phase reduction in step (2) is 6 to 70 hours, for example, 6 hours, 10 hours, 15 hours, 20 hours, 25 hours, 30 hours, 35 hours, 40 hours, 50 hours, 60 hours, or 70 hours, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, preferably 20 to 40 hours.
Preferably, the carbothermic solid phase reduction of step (2) is heated to 1500-.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) uniformly mixing a vanadium-containing raw material with the granularity of 50-300 meshes, a carbon-containing raw material and an iron-containing raw material with the granularity of 50-300 meshes, wherein the vanadium-containing raw material, the carbon-containing raw material and the iron-containing raw material are mixed according to the mass ratio of elements V: c: fe 1000 (620) and 300 (800) and 1100;
(2) and (2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln filled with protective gas for carbon thermal solid-phase reduction, wherein the pressure of the protective gas is 0-80Pa, the reaction time of the carbon thermal solid-phase reduction is 6-70h, and the temperature is heated to 1500-1800 ℃ to obtain 50 ferrovanadium.
The second purpose of the invention is to provide 50 ferrovanadium prepared by the preparation method of the first purpose, wherein the 50 ferrovanadium comprises 48-55% of V and 0.1-5% of C by mass percent, and the balance is iron.
As a preferred technical scheme of the invention, the 50 ferrovanadium is a compact block.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the 50 ferrovanadium preparation method adopts the carbon-containing raw material with low price and wide source as the reducing agent, and does not adopt a vacuum furnace for reaction, thereby greatly reducing the production cost;
(2) the 50 ferrovanadium preparation method can improve the recovery rate of vanadium to more than 98 percent;
(3) the preparation method of the 50 ferrovanadium utilizes a common pushed slab kiln to carry out reaction, has the advantages of simple flow, low production cost and easy operation, and can realize continuous large-scale production.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) uniformly mixing 1000kg of vanadium pentoxide with the granularity of 100 meshes and the purity of 98.5 percent, 255kg of carbon powder with the purity of 99.2 percent and 550kg of iron powder with the granularity of 200 meshes and the purity of 95.8 percent;
(2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln with the length of 46 meters, wherein 32 temperature zones are arranged in the pushed slab kiln, each temperature zone of 1-7 temperature zones is 1 meter long, each temperature zone of 8-21 temperature zones is 2 meters long, and each temperature zone of 22-32 temperature zones is 1 meter; introducing nitrogen as protective gas into the pushed slab kiln, wherein the pressure of the nitrogen is 20 Pa; the temperature of the pushed slab kiln is set to be 1-13 temperature zone, which is gradually heated from 300 ℃ to 1600 ℃, 14-21 temperature zone, which is constant at 1700 ℃, and 22-32 temperature zone, which is gradually cooled from 1600 ℃ to 100 ℃; the mixed raw materials enter a temperature zone 1 from the kiln head of the pushed slab kiln and then come out from the kiln tail of the pushed slab kiln after 18 hours to obtain 50 ferrovanadium.
The 50 ferrovanadium obtained in this example comprises, in mass%, 50.2% V and 0.3% C, with the balance being iron and unavoidable impurities. The vanadium recovery of this example was 98.9%.
Example 2
The embodiment provides a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) mixing 1000kg of vanadium pentoxide with the granularity of 200 meshes and the purity of 99%, 270kg of graphite with the purity of 95.7% and 545kg of iron powder with the granularity of 300 meshes and the purity of 96.2% uniformly;
(2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln with the length of 46 meters, wherein 32 temperature zones are arranged in the pushed slab kiln, each temperature zone of 1-7 temperature zones is 1 meter long, each temperature zone of 8-21 temperature zones is 2 meters long, and each temperature zone of 22-32 temperature zones is 1 meter; introducing argon as a protective gas into the pushed slab kiln, wherein the pressure of the argon is 80 Pa; the temperature of the pushed slab kiln is set to be 1-13 temperature zone, which is gradually heated from 200 ℃ to 1500 ℃, 14-21 temperature zone, which is constant at 1600 ℃, and 22-32 temperature zone, which is gradually cooled from 1500 ℃ to 80 ℃; the mixed raw materials enter a temperature zone 1 from the kiln head of the pushed slab kiln and then come out from the kiln tail of the pushed slab kiln after 18 hours to obtain 50 ferrovanadium.
The 50 ferrovanadium obtained in this example comprises, in mass%, 50.4% V and 2.2% C, with the balance being iron and unavoidable impurities. The vanadium recovery of this example was 99.1%.
Example 3
The embodiment provides a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) uniformly mixing 1000kg of vanadium trioxide with the granularity of 150 meshes and the purity of 98.5%, 255kg of coke with the purity of 90.6% and 820kg of ferroferric oxide with the granularity of 50 meshes and the purity of 95.9%;
(2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln with the length of 34 meters, wherein 24 temperature zones are arranged in the pushed slab kiln, each temperature zone of 1-6 temperature zones is 1 meter long, each temperature zone of 7-16 temperature zones is 2 meters long, and each temperature zone of 17-24 temperature zones is 1 meter; introducing argon as a protective gas into the pushed slab kiln, wherein the pressure of the argon is 0Pa, namely the pressure is consistent with the pressure of the external atmospheric pressure; the temperature of the pushed slab kiln is set to be 1-8 temperature zone, which is gradually heated from 200 ℃ to 1400 ℃, 9-17 temperature zone, which is constant at 1500 ℃, and 18-24 temperature zone, which is gradually cooled from 1400 ℃ to 100 ℃; the mixed raw materials enter a temperature zone 1 from the kiln head of the pushed slab kiln and then come out from the kiln tail of the pushed slab kiln after 24 hours, so that 50 ferrovanadium is obtained.
The 50 ferrovanadium obtained in this example comprises, by mass, 49.4% V and 1.3% C, with the balance being iron and unavoidable impurities. The vanadium recovery of this example was 98.7%.
Example 4
The embodiment provides a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) mixing 1000kg of vanadium dioxide with granularity of 50 meshes and purity of 98.3%, 245kg of activated carbon with purity of 97.8% and 852kg of ferric oxide with granularity of 100 meshes and purity of 96.7% uniformly;
(2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln with the length of 46 meters, wherein 32 temperature zones are arranged in the pushed slab kiln, each temperature zone of 1-7 temperature zones is 1 meter long, each temperature zone of 8-21 temperature zones is 2 meters long, and each temperature zone of 22-32 temperature zones is 1 meter; introducing argon as a protective gas into the pushed slab kiln, wherein the pressure of the argon is 30 Pa; the temperature of the pushed slab kiln is set to be 1-13 temperature zone, which is gradually heated from 200 ℃ to 1700 ℃, 14-21 temperature zone, which is constant at 1800 ℃, and 22-32 temperature zone, which is gradually cooled from 1700 ℃ to 100 ℃; the mixed raw materials enter a temperature zone 1 from the kiln head of the pushed slab kiln and then come out from the kiln tail of the pushed slab kiln after 20 hours to obtain 50 ferrovanadium.
The 50 ferrovanadium obtained in this example comprises, in mass%, 50.2% V and 0.22% C, with the balance being iron and unavoidable impurities. The vanadium recovery of this example was 98.8%.
Example 5
The embodiment provides a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) mixing 1000kg of ammonium metavanadate with granularity of 300 meshes and purity of 98.5%, 276kg of carbon powder with purity of 99.1% and 650kg of ferric oxide with granularity of 100 meshes and purity of 96.7% uniformly;
(2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln with the length of 42 meters, wherein the pushed slab kiln is provided with 29 temperature zones, each temperature zone of 1-7 temperature zones is 1 meter long, each temperature zone of 8-20 temperature zones is 2 meters long, and each temperature zone of 21-29 temperature zones is 1 meter; introducing argon as a protective gas into the pushed slab kiln, wherein the nitrogen pressure is 50 Pa; the temperature of the pushed slab kiln is set to be 1-11 temperature zone, which is gradually heated from 200 ℃ to 1300 ℃, 12-21 temperature zone, which is constant at 1400 ℃, and 22-29 temperature zone, which is gradually cooled from 1300 ℃ to 100 ℃; the mixed raw materials enter a temperature zone 1 from the kiln head of the pushed slab kiln and then come out from the kiln tail of the pushed slab kiln after 40 hours to obtain 50 ferrovanadium.
The 50 ferrovanadium obtained in this example comprises 48.8% V and 5% C by mass, the balance being iron and unavoidable impurities. The vanadium recovery of this example was 98.2%.
Example 6
The embodiment provides a preparation method of 50 ferrovanadium, which comprises the following steps:
(1) uniformly mixing 1000kg of vanadium trioxide with the granularity of 150 meshes and the purity of 98.5%, 255kg of coke with the purity of 90.6% and 820kg of ferroferric oxide with the granularity of 50 meshes and the purity of 95.9%;
(2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln with the length of 36 meters, wherein the pushed slab kiln is provided with 26 temperature zones, each temperature zone of 1-7 temperature zones is 1 meter long, each temperature zone of 8-17 temperature zones is 2 meters long, and each temperature zone of 18-26 temperature zones is 1 meter; introducing argon as a protective gas into the pushed slab kiln, wherein the pressure of the argon is 60 Pa; the temperature of the pushed slab kiln is set to be 1-8 temperature zone, the temperature of which is gradually increased from 200 ℃ to 1700 ℃, 9-18 temperature zone, the temperature of which is constant at 1800 ℃, and 19-26 temperature zone, the temperature of which is gradually decreased from 1700 ℃ to 100 ℃; the mixed raw materials enter a temperature zone 1 from the kiln head of the pushed slab kiln and then come out from the kiln tail of the pushed slab kiln after 42 hours to obtain 50 ferrovanadium.
The 50 ferrovanadium obtained in this example comprises, in mass%, 52.3% V and 3.3% C, with the balance being iron and unavoidable impurities. The vanadium recovery of this example was 98.5%.
The embodiment shows that the preparation method can prepare qualified 50 ferrovanadium in the pushed slab kiln under the protective gas environment without vacuumizing, the recovery rate of vanadium is up to more than 98 percent, and the method has the advantages of simple flow, low production cost and easily obtained raw materials and can realize continuous large-scale production by utilizing the common pushed slab kiln.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of 50 ferrovanadium is characterized by comprising the following steps:
(1) uniformly mixing a vanadium-containing raw material, a carbon-containing raw material and an iron-containing raw material;
(2) and (3) putting the mixed raw material obtained in the step (1) into a pushed slab kiln filled with protective gas for carbon-thermal solid-phase reduction to obtain 50 ferrovanadium.
2. The preparation method according to claim 1, wherein the vanadium-containing raw material, the carbon-containing raw material and the iron-containing raw material in the step (1) are proportioned according to the mass ratio of elements;
preferably, the element mass ratio is V: c: fe 1000 (620-.
3. The preparation method according to claim 1 or 2, wherein the vanadium-containing raw material in step (1) is any one or a mixture of at least two of vanadium dioxide, vanadium trioxide, vanadium pentoxide, ammonium metavanadate or ammonium polyvanadate;
preferably, the vanadium-containing raw material in the step (1) has a particle size of 50-300 meshes.
4. The method according to any one of claims 1 to 3, wherein the carbonaceous raw material in step (1) is any one or a mixture of at least two of graphite, coke, tar and pitch.
5. The preparation method according to any one of claims 1 to 4, wherein the iron-containing raw material in the step (1) is any one of iron, ferric oxide and ferroferric oxide or a mixture of at least two of the iron, the ferric oxide and the ferroferric oxide;
preferably, the iron-containing raw material of step (1) has a particle size of 50-300 mesh.
6. The production method according to any one of claims 1 to 5, wherein the shielding gas in step (2) is any one or a mixture of at least two of nitrogen, helium, neon or argon;
preferably, the pressure of the protective gas in the step (2) is 0-80 Pa.
7. The process according to any one of claims 1 to 6, wherein the carbothermic solid phase reduction of step (2) is carried out for a reaction time of 6 to 70 hours, preferably 20 to 40 hours;
preferably, the carbothermic solid phase reduction of step (2) is heated to 1500-.
8. The production method according to any one of claims 1 to 7, characterized by comprising the steps of:
(1) uniformly mixing a vanadium-containing raw material with the granularity of 50-300 meshes, a carbon-containing raw material and an iron-containing raw material with the granularity of 50-300 meshes, wherein the vanadium-containing raw material, the carbon-containing raw material and the iron-containing raw material are mixed according to the mass ratio of elements V: c: fe 1000 (620) and 300 (800) and 1100;
(2) and (2) putting the mixed raw material obtained in the step (1) into a pushed slab kiln filled with protective gas for carbon thermal solid-phase reduction, wherein the pressure of the protective gas is 0-80Pa, the reaction time of the carbon thermal solid-phase reduction is 6-70h, and the temperature is heated to 1500-1800 ℃ to obtain 50 ferrovanadium.
9. 50 vanadium iron produced by the production method according to any one of claims 1 to 8, wherein the 50 vanadium iron comprises 48 to 55% by mass of V and 0.1 to 5% by mass of C, with the balance being iron.
10. The 50 ferrovanadium according to claim 9 wherein the 50 ferrovanadium is a dense cake.
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