CN113930662A - Preparation method of chromium nitride ferrovanadium alloy - Google Patents
Preparation method of chromium nitride ferrovanadium alloy Download PDFInfo
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- CN113930662A CN113930662A CN202111122501.3A CN202111122501A CN113930662A CN 113930662 A CN113930662 A CN 113930662A CN 202111122501 A CN202111122501 A CN 202111122501A CN 113930662 A CN113930662 A CN 113930662A
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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
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/056—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using gas
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
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Abstract
The invention relates to the technical field of ferroalloy, in particular to a preparation method of chromium vanadium iron nitride, which comprises the following steps: uniformly mixing vanadium oxide powder, chromium mud, iron oxide powder and a reducing agent, adding a binder and water, and uniformly mixing to prepare pellets; step two, drying the pellets at the temperature of 80-150 ℃; and step three, heating the dried pellets in an ammonia atmosphere for pre-reduction, heating for nitridation, and cooling to obtain the chromium nitride ferrovanadium nitride. The preparation method of the invention takes the byproduct chromium mud for producing vanadium pentoxide as the raw material, which can reduce the production cost of the chromium nitride ferrovanadium alloy, increase the nitrogen content in the alloy, improve the ratio of nitrogen to vanadium and improve the performance of steel. The preparation method has simple flow, few raw material types required by the reaction, recyclable gas generated in the production process and no waste residue in the whole production process.
Description
Technical Field
The invention relates to the technical field of ferroalloy, in particular to a preparation method of chromium vanadium iron nitride alloy.
Background
The ferrovanadium nitride is used as a novel vanadium-nitrogen alloy additive of high-strength microalloy steel, the performance of the ferrovanadium nitride is superior to that of ferrovanadium and vanadium nitride, and the ferrovanadium nitride has higher specific gravity and higher absorptivity than vanadium nitride, and has the functions of refining grains, improving strength, toughness, ductility and the like. The addition of nitrided ferrovanadium to steel not only improves the strength, toughness and ductility of steel, but also enhances the wear resistance, corrosion resistance and thermal fatigue resistance of steel, and enables the steel to have excellent weldability, so that nitrided ferrovanadium is widely used for products such as high-strength twisted steel, high-strength pipeline steel, high-strength section steel and the like.
At present, the main method for preparing nitrided ferrovanadium alloy at home and abroad is to crush ferrovanadium raw materials, place the crushed and ball-milled raw materials in a high-pressure synthesizer for sealing, fill high-purity nitrogen after vacuumizing to reach a specified pressure, start an ignition device to ignite self-propagating combustion synthesis reaction, and induce adjacent materials to continue chemical reaction under the support of self-exothermic reaction until all the materials are subjected to self-sustaining reaction to obtain a nitrided ferrovanadium product. However, the preparation method of the ferrovanadium nitride in the prior art has the advantages of high raw material cost, complex production process, long reaction time and high energy consumption, and the prepared ferrovanadium nitride has low nitrogen content and low nitrogen-vanadium ratio.
Disclosure of Invention
Based on the problems in the prior art, the invention provides the preparation method of the chromium nitride vanadium iron alloy, which can reduce the production cost and the energy consumption, and the chromium nitride vanadium iron alloy with high nitrogen content and high nitrogen-vanadium ratio can be prepared by the preparation method, so that the defects in the prior art are overcome.
In order to achieve the purpose, the invention adopts the following technical scheme:
the embodiment of the invention provides a preparation method of chromium nitride vanadium iron alloy, which comprises the following steps:
uniformly mixing vanadium oxide powder, chromium mud, iron oxide powder and a reducing agent, adding a binder and water, and uniformly mixing to prepare pellets;
step two, drying the pellets at the temperature of 80-150 ℃;
and thirdly, heating the dried pellets to 400-650 ℃ in an ammonia atmosphere for pre-reduction for 1-5 hours, heating to 1000-1300 ℃ for reduction, carrying out reduction reaction for 4-8 hours, heating to 1400-1600 ℃ for nitridation for 1-3 hours, and cooling after the nitridation is finished to obtain the chromium nitride ferrovanadium.
The preparation method of the chromium nitride ferrovanadium alloy provided by the invention takes the byproduct chromium mud for producing vanadium pentoxide as a raw material to prepare the chromium nitride ferrovanadium alloy, the chromium mud contains both vanadium and chromium, the addition of vanadium oxide can be reduced by fully utilizing the vanadium in the chromium mud, and the production cost of the chromium nitride ferrovanadium alloy is greatly reduced; by fully utilizing the reaction of chromium and nitrogen in the chromium mud, the nitrogen content in the alloy is increased, the nitrogen-vanadium ratio in the alloy is improved, the increase of the nitrogen content in the alloy can obviously improve the toughness and the plasticity of the steel, the heat resistance strength and the creep deformation capability of the steel, the interphase distribution of vanadium can be changed, the endurance strength of the steel is improved, and the performance of the steel is further improved. The method takes vanadium oxide powder, chromium mud and iron oxide powder as raw materials, and carries out pre-reduction, reduction and nitridation reactions by sectional heating in the atmosphere of ammonia gas to obtain vanadium-chromium-iron nitride alloy powder, wherein the ammonia gas not only can be used as a nitrogen source, but also can be used as a reducing agent in the process, so that the full progress of the reduction reaction is ensured. The temperature ranges of the pre-reduction, the reduction and the nitridation of the materials can be accurately controlled by heating the dried pellets in sections for pre-reduction, reduction and nitridation reactions, the time consumed by the whole preparation period is shortened by controlling the time of the section heating, and the energy consumption is reduced. The preparation method has simple flow, few raw material types required by the reaction, recyclable gas generated in the production process, no waste residue generated in the whole production process, capability of realizing green production of chromium nitride vanadium iron, reduction of the production cost, increase of the nitrogen content in the alloy, improvement of the nitrogen-vanadium ratio in the alloy, improvement of the performance of steel and overcoming of the defects of the prior art. The chromium nitride ferrovanadium alloy prepared by the preparation method has the nitrogen content of 25-30%, the vanadium content of 45-50% and the ratio of nitrogen to vanadium of 0.565-0.620.
Preferably, in the first step, the mass ratio of the vanadium oxide, the chromium mud, the iron oxide and the reducing agent is 1: 0.3-0.5: 0.1-0.3: 0.25 to 0.4.
Preferably, in the first step, the vanadium oxide is at least one of vanadium pentoxide, ammonium metavanadate, vanadium dioxide and vanadium trioxide.
Preferably, in the step one, the chromium mud is a byproduct for producing vanadium pentoxide, the content of vanadium is 7% -9.5%, and the content of chromium is 20% -25%.
The method takes the byproduct chromium mud for producing vanadium pentoxide as a raw material, and the chromium mud contains both vanadium and chromium, so that the addition amount of vanadium oxide can be reduced, the efficient utilization of solid wastes is realized, and the production cost of chromium nitride ferrovanadium alloy is greatly reduced; by fully utilizing the reaction between chromium and nitrogen in the chromium mud, the nitrogen content in the alloy is increased, the nitrogen-vanadium ratio in the alloy is improved, and the performance of the steel is improved. Compared with the traditional method for preparing the nitrogen-nitrided ferrovanadium alloy, the method has the advantages that the using amount of vanadium source compounds is greatly reduced, and the nitrogen content and the nitrogen-vanadium ratio in the alloy are obviously improved.
Preferably, in the first step, the iron oxide is at least one of ferric oxide and ferroferric oxide.
After vanadium oxide powder, chromium mud, iron oxide powder, a reducing agent, a binder and water are uniformly mixed, because ferric oxide or ferroferric oxide has a large specific surface area, a mixture with a pore structure can be formed with the vanadium oxide and the chromium mud, and ammonia can enter the solid mixture with the pore structure and fully contact with raw materials in the reduction nitridation process, so that the reduction rate can be further improved, and the nitrogen content of the alloy can be increased.
Preferably, in the first step, the binder is one or two of polyvinyl alcohol and starch glue, the mass of the binder is 25% -50% of the total mass of all the raw materials, and the mass of the water is 93-95 times of the total mass of all the raw materials.
Preferably, in the second step, the drying temperature is 90-110 ℃, and the drying time is 4-6 hours.
The drying process in the second step is a dehydration drying process and a preheating process, and the temperature rise time from the subsequent temperature rise to the low-temperature heat treatment temperature can be shortened through the preheating of the second step. And the moisture in the pellets can be fully removed by controlling the drying temperature and the drying time.
Preferably, in the third step, the temperature of pre-reduction is 450-550 ℃, the time of pre-reduction is 3-5 hours, the temperature of reduction is 1100-1200 ℃, and the time of reduction reaction is 4-6 hours.
The temperature ranges of the pre-reduction, the reduction and the nitridation of the materials can be accurately controlled by heating the dried pellets in sections for pre-reduction, reduction and nitridation reactions, the time consumed by the whole preparation period is shortened by controlling the time of the section heating, and the energy consumption is reduced.
The preparation method of the chromium nitride vanadium iron alloy provided by the invention takes vanadium oxide powder, chromium mud and iron oxide powder as raw materials to prepare the chromium nitride vanadium iron alloy, the use of the chromium mud can reduce the addition of vanadium oxide, and the production cost of the chromium nitride vanadium iron alloy is greatly reduced; by fully utilizing the reaction between chromium and nitrogen in the chromium mud, the nitrogen content in the alloy is increased, the nitrogen-vanadium ratio in the alloy is improved, and the performance of the steel is improved. When the iron oxide powder is at least one of ferric oxide or ferroferric oxide powder, the larger specific surface area of the iron oxide powder can enable the iron oxide powder, vanadium oxide and chromium mud to form a mixture with a pore structure, and ammonia gas can enter the solid mixture with the pore structure and fully contact with the raw materials in the reduction nitridation process, so that the reduction rate can be further improved, and the nitrogen content of the alloy can be increased. During the pre-reduction, reduction and nitridation reaction processes, ammonia gas can be used as a nitrogen source to increase the nitrogen content of the alloy, and can also be used as a reducing agent to ensure that the reduction reaction is fully carried out. The temperature range and the heating time of each step of reaction can be accurately controlled by heating the dried pellets in sections for pre-reduction, reduction and nitridation reaction, so that the time consumption of the whole preparation period is shortened, and the energy consumption is reduced. The preparation method has simple flow, few raw material types required by the reaction, recyclable gas generated in the production process, no waste residue generated in the whole production process, capability of realizing green production of chromium nitride vanadium iron, reduction of the production cost, increase of the nitrogen content in the alloy, improvement of the nitrogen-vanadium ratio in the alloy and improvement of the performance of steel. The chromium nitride ferrovanadium alloy prepared by the preparation method disclosed by the invention has the nitrogen content of 25-30%, the vanadium content of 45-50% and the ratio of nitrogen to vanadium of 0.565-0.620.
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 with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment provides a preparation method of chromium nitride vanadium iron alloy, which comprises the following steps:
(1) 1kg of vanadium pentoxide powder, 0.5kg of chromium mud (the content of vanadium in the chromium mud is 7 percent, and the content of chromium in the chromium mud is 25 percent), 0.1kg of ferric oxide powder and 0.4kg of graphite carbon powder are mixed uniformly, 0.5kg of polyvinyl alcohol and 186.8kg of water are added, and the mixture is mixed uniformly to prepare pellets.
(2) The pellets were dried at 80 ℃ for 6 hours.
(3) Heating the dried pellets to 400 ℃ in an ammonia atmosphere for pre-reduction, wherein the pre-reduction time is 5 hours, heating to 1000 ℃ for reduction, the reduction reaction time is 8 hours, heating to 1400 ℃ for nitridation, wherein the nitridation time is 3 hours, cooling to normal temperature after the nitridation is finished, crushing to obtain chromium-vanadium-iron nitride, and detecting that the vanadium content in the prepared chromium-vanadium-iron nitride alloy is 45.2%, the nitrogen content is 25.56%, and the nitrogen-vanadium ratio in the chromium-vanadium-iron nitride alloy is 0.565.
Example 2
The embodiment provides a preparation method of chromium nitride vanadium iron alloy, which comprises the following steps:
(1) 1kg of ammonium metavanadate powder, 0.3kg of chromium mud (the content of vanadium in the chromium mud is 9.5 percent, and the content of chromium in the chromium mud is 20 percent), 0.3kg of ferroferric oxide powder and 0.25kg of graphite carbon powder are mixed uniformly, 0.92kg of starch glue and 175.75kg of water are added, and the mixture is mixed uniformly to prepare pellets.
(2) The pellets were dried at 150 ℃ for 4 hours.
(3) Heating the dried pellets to 650 ℃ in an ammonia atmosphere for pre-reduction for 1 hour, heating to 1300 ℃ for reduction, carrying out reduction reaction for 4 hours, heating to 1600 ℃ for nitridation for 1 hour, cooling to normal temperature after the nitridation is finished, crushing to obtain chromium-vanadium-iron nitride, and detecting that the vanadium content in the prepared chromium-vanadium-iron nitride alloy is 46.8%, the nitrogen content is 26.96%, and the nitrogen-vanadium ratio in the chromium-vanadium-iron nitride alloy is 0.576.
Example 3
The embodiment provides a preparation method of chromium nitride vanadium iron alloy, which comprises the following steps:
(1) 1kg of vanadium pentoxide and vanadium dioxide powder, 0.45kg of chromium mud (the vanadium content in the chromium mud is 8 percent, and the chromium content in the chromium mud is 21 percent), 0.2kg of ferric oxide and ferroferric oxide powder and 0.3kg of graphite carbon powder are mixed uniformly, 0.59kg of polyvinyl alcohol and 183.3kg of starch glue are added, and the mixture is mixed uniformly to prepare pellets.
(2) The pellets were dried at 90 ℃ for 5 hours.
(3) Heating the dried pellets to 450 ℃ in an ammonia atmosphere for pre-reduction, wherein the pre-reduction time is 3 hours, heating to 1100 ℃ for reduction, the reduction reaction time is 5 hours, heating to 1500 ℃ for nitridation, wherein the nitridation time is 2 hours, cooling to normal temperature after the nitridation is finished, crushing to obtain chromium-vanadium-iron nitride, and detecting that the vanadium content in the prepared chromium-vanadium-iron nitride alloy is 48.3%, the nitrogen content is 29.34%, and the nitrogen-vanadium ratio in the chromium-vanadium-iron nitride alloy is 0.607.
Example 4
The embodiment provides a preparation method of chromium nitride vanadium iron alloy, which comprises the following steps:
(1) 1kg of vanadium trioxide and ammonium metavanadate powder, 0.45kg of chromium mud (the content of vanadium in the chromium mud is 9 percent, and the content of chromium in the chromium mud is 24 percent), 0.25kg of ferric oxide and ferroferric oxide powder and 0.35kg of graphite carbon powder are mixed uniformly, 0.82kg of polyvinyl alcohol and starch glue are added, and 194.75kg of water are added and mixed uniformly to prepare pellets.
(2) The pellets were dried at 110 ℃ for 4.5 hours.
(3) Heating the dried pellets to 600 ℃ in an ammonia atmosphere for pre-reduction, wherein the pre-reduction time is 2 hours, heating to 1200 ℃ for reduction, the reduction reaction time is 6 hours, heating to 1550 ℃ for nitridation, wherein the nitridation time is 1.5 hours, cooling to normal temperature after the nitridation is finished, crushing to obtain chromium-vanadium-iron nitride, and detecting that the vanadium content in the prepared chromium-vanadium-iron nitride alloy is 47.9%, the nitrogen content is 29.72%, and the nitrogen-vanadium ratio in the chromium-vanadium-iron nitride alloy is 0.620.
Example 5
The embodiment provides a preparation method of chromium nitride vanadium iron alloy, which comprises the following steps:
(1) 1kg of vanadium pentoxide and ammonium metavanadate powder, 0.4kg of chromium mud (the content of vanadium in the chromium mud is 9 percent, and the content of chromium in the chromium mud is 23 percent), 0.27kg of ferric oxide powder and 0.33kg of graphite carbon powder are mixed uniformly, 1kg of starch glue and 188.2kg of water are added, and the mixture is mixed uniformly to prepare pellets.
(2) The pellets were dried at 130 ℃ for 5.5 hours.
(3) Heating the dried pellets to 550 ℃ in an ammonia atmosphere for prereduction, wherein the prereduction time is 5 hours, heating to 1100 ℃ for reduction, the reduction reaction time is 4 hours, heating to 1450 ℃ for nitridation, wherein the nitridation time is 2.5 hours, cooling to normal temperature after the nitridation is finished, crushing to obtain chromium-vanadium-iron nitride, and detecting that the vanadium content in the prepared chromium-vanadium-iron nitride alloy is 49.3%, the nitrogen content is 28.95%, and the nitrogen-vanadium ratio in the chromium-vanadium-iron nitride alloy is 0.587.
Examples of effects
The chromium nitride ferrovanadium alloy prepared in examples 1 to 5 was added to steel to prepare a bar, and both ends of the bar were subjected to tensile strength and specified plastic elongation strength performance tests at room temperature according to the GB/T228-2010 metallic material tensile test method, and the test results are shown in table 1 below:
TABLE 1 tensile test results of metallic materials
The data in the table show that the chromium nitride vanadium iron alloy provided by the invention can obviously improve the toughness and plasticity of steel, improve the heat resistance strength and creep resistance of steel and improve the endurance strength of steel.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The preparation method of the chromium nitride vanadium iron alloy is characterized by comprising the following steps of:
uniformly mixing vanadium oxide powder, chromium mud, iron oxide powder and a reducing agent, adding a binder and water, and uniformly mixing to prepare pellets;
step two, drying the pellets at the temperature of 80-150 ℃;
and thirdly, heating the dried pellets to 400-650 ℃ in an ammonia atmosphere for pre-reduction for 1-5 hours, heating to 1000-1300 ℃ for reduction, carrying out reduction reaction for 4-8 hours, heating to 1400-1600 ℃ for nitridation for 1-3 hours, and cooling after the nitridation is finished to obtain the chromium nitride ferrovanadium.
2. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the first step, the mass ratio of the vanadium oxide to the chromium mud to the iron oxide to the reducing agent is 1: 0.3-0.5: 0.1-0.3: 0.25-0.4.
3. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the first step, the vanadium oxide is at least one of vanadium pentoxide, ammonium metavanadate, vanadium dioxide and vanadium trioxide.
4. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the first step, the chromium mud is a byproduct for producing vanadium pentoxide, the content of vanadium is 7% -9.5%, and the content of chromium is 20% -25%.
5. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the first step, the iron oxide is at least one of ferric oxide and ferroferric oxide.
6. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the first step, the reducing agent is graphite carbon powder.
7. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the first step, the binder is one or two of polyvinyl alcohol and starch glue, the mass of the binder is 25% -50% of the total mass of the vanadium oxide, the chromium mud, the iron oxide and the reducing agent, and the mass of the water is 93-95 times of the total mass of the vanadium oxide, the chromium mud, the iron oxide and the reducing agent.
8. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the second step, the drying temperature is 90-110 ℃, and the drying time is 4-6 hours.
9. The method of preparing a chromium nitride ferrovanadium alloy as claimed in claim 1, wherein: in the third step, the temperature of the pre-reduction is 450-550 ℃, the time of the pre-reduction is 3-5 hours, the temperature of the reduction is 1100-1200 ℃, and the time of the reduction reaction is 4-6 hours.
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Cited By (1)
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| CN115572888A (en) * | 2022-09-29 | 2023-01-06 | 中色（宁夏）东方集团有限公司 | Ferrovanadium alloy and preparation method thereof |
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