CN111020106A - Vanadium-nitrogen alloy additive and preparation method thereof - Google Patents
Vanadium-nitrogen alloy additive and preparation method thereof Download PDFInfo
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- CN111020106A CN111020106A CN201911286439.4A CN201911286439A CN111020106A CN 111020106 A CN111020106 A CN 111020106A CN 201911286439 A CN201911286439 A CN 201911286439A CN 111020106 A CN111020106 A CN 111020106A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/0006—Adding metallic additives
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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
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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
- 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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Abstract
The invention relates to a vanadium-nitrogen alloy additive and a preparation method thereof, wherein the vanadium-nitrogen alloy additive mainly comprises the following raw materials in parts by weight: 30-40 parts of vanadium compound, 8-11 parts of iron powder, 12-16 parts of graphite powder, 6-10 parts of silicide and 6-8 parts of aluminum oxide. The invention also comprises a preparation method of the vanadium-nitrogen alloy additive. According to the invention, through the speed of accelerating the carbonization reaction by alumina, the mixed gas of carbon dioxide and nitrogen is firstly introduced for reduction; and then mixed gas of nitrogen and ammonia gas is introduced for nitridation, so that the nitrogen content in the vanadium-nitrogen alloy can be increased, and the reaction speed is accelerated.
Description
Technical Field
The invention relates to the field of vanadium-nitrogen alloy additive manufacturing, in particular to a vanadium-nitrogen alloy additive and a preparation method thereof.
Background
The vanadium-nitrogen alloy is mainly used as an alloy additive in the metallurgical industry, the industrial development is rapid in recent years, and a large amount of industrial scale application data show that the addition of vanadium into steel brings benefits for steelmaking production and improves the performance of the steel, so that the cost is reduced.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a vanadium-nitrogen alloy additive with higher nitrogen content and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problem is that,
the vanadium-nitrogen alloy additive mainly comprises the following raw materials in parts by weight: 30-40 parts of vanadium compound, 8-11 parts of iron powder, 12-16 parts of graphite powder, 6-10 parts of silicide and 6-8 parts of aluminum oxide.
Further, the vanadium compound is at least one of vanadium trioxide, vanadium pentoxide and ammonium metavanadate.
Further, the silicide is ferrosilicon powder or silicon dioxide.
The preparation method of the vanadium-nitrogen alloy additive comprises the following steps:
the method comprises the following steps: putting iron powder into a high-temperature calcining kiln, carrying out high-temperature firing at 800 ℃ in 600-plus-one temperature, continuously introducing air to enable the iron powder to react completely to generate iron oxide, and crushing and grinding the iron oxide into 240-mesh iron oxide powder with the particle size of 180-plus-one temperature;
step two: crushing and grinding the vanadium compound into powder with the particle size of 180-240 meshes, and drying to obtain vanadium compound powder;
step three: uniformly mixing the iron oxide powder obtained in the step (1), the vanadium compound powder obtained in the step (2), silicide and aluminum oxide, and adding into a high-temperature calcining kiln;
step four, evacuating the air of the high-temperature calcining kiln added with the mixed materials, spraying graphite powder, filling mixed gas of carbon dioxide and nitrogen, and carrying out primary reduction reaction for more than 6 hours (preferably 8-12 hours) by high-temperature calcining;
the volume percentage of carbon dioxide in the mixed gas of carbon dioxide and nitrogen is 5-8%.
The temperature of the primary reduction reaction is 600-800 ℃.
Step five, after the reduction reaction is finished, continuously introducing mixed gas of nitrogen and ammonia, raising the calcination temperature, and carrying out secondary nitridation reaction for more than 12 hours;
the volume percentage of ammonia gas in the mixed gas of nitrogen and ammonia gas is 3-5%.
The temperature of the secondary nitridation reaction is 700-1200 ℃.
And step six, placing the reacted mixture into a vacuum environment for natural cooling to form the vanadium-nitrogen alloy additive.
According to the invention, through the speed of accelerating the carbonization reaction by alumina, the mixed gas of carbon dioxide and nitrogen is firstly introduced for reduction; and then mixed gas of nitrogen and ammonia gas is introduced for nitridation, so that the nitrogen content in the vanadium-nitrogen alloy can be increased, and the reaction speed is accelerated.
Detailed Description
The present invention will be described in further detail with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting.
Example 1
The vanadium-nitrogen alloy additive of the embodiment mainly comprises the following raw materials in parts by weight: 30 parts of vanadium trioxide, 8 parts of iron powder, 12 parts of graphite powder, 6 parts of ferrosilicon powder and 6 parts of aluminum oxide.
The preparation method of the vanadium-nitrogen alloy additive of the embodiment comprises the following steps:
the method comprises the following steps: putting iron powder into a high-temperature calcining kiln, calcining at 600 ℃, continuously introducing air to completely react to generate iron oxide, and crushing and grinding the iron oxide into 240-mesh iron oxide powder with the particle size of 180-;
step two: vanadium trioxide is crushed and ground into powder with the particle size of 180 meshes and 240 meshes, and the powder is dried to obtain vanadium trioxide powder;
step three: uniformly mixing the iron oxide powder obtained in the step (1), the vanadium trioxide powder obtained in the step (2), the ferrosilicon powder and the aluminum oxide, and adding the mixture into a high-temperature calcining kiln;
step four, evacuating the air of the high-temperature calcining kiln added with the mixed materials, spraying graphite powder, filling mixed gas of carbon dioxide and nitrogen, and carrying out primary reduction reaction for 6 hours through high-temperature calcining;
the volume percentage of carbon dioxide in the mixed gas of carbon dioxide and nitrogen is 5%.
The temperature of the primary reduction reaction was 600 ℃.
Step five, after the reduction reaction is finished, continuously introducing mixed gas of nitrogen and ammonia, raising the calcination temperature, and carrying out secondary nitridation reaction for 12 hours;
the volume percentage of ammonia gas in the mixed gas of nitrogen and ammonia gas is 3%.
The temperature of the secondary nitridation reaction was 700 ℃.
And step six, placing the reacted mixture into a vacuum environment for natural cooling to form the vanadium-nitrogen alloy additive.
The vanadium content in the obtained vanadium-nitrogen alloy additive is 80.0 percent, the nitrogen content is 19.0 percent, the oxygen content is 0.42 percent, and the contents of other elements are all in the national standard range.
Example 2
The vanadium-nitrogen alloy additive of the embodiment mainly comprises the following raw materials in parts by weight: 35 parts of vanadium pentoxide, 9 parts of iron powder, 15 parts of graphite powder, 8 parts of silicon dioxide and 7 parts of aluminum oxide.
The preparation method of the vanadium-nitrogen alloy additive of the embodiment comprises the following steps:
the method comprises the following steps: putting iron powder into a high-temperature calcining kiln, calcining at the high temperature of 700 ℃, continuously introducing air to enable the iron powder to react completely to generate iron oxide, and crushing and grinding the iron oxide into 240-mesh iron oxide powder with the particle size of 180-;
step two: crushing and grinding vanadium pentoxide into powder with the particle size of 180-240 meshes, and drying to obtain vanadium pentoxide powder;
step three: uniformly mixing the iron oxide powder obtained in the step (1), the vanadium pentoxide powder obtained in the step (2), silicon dioxide and aluminum oxide, and adding into a high-temperature calcining kiln;
step four, evacuating the air of the high-temperature calcining kiln added with the mixed materials, spraying graphite powder, filling mixed gas of carbon dioxide and nitrogen, and carrying out primary reduction reaction for 8 hours through high-temperature calcining;
the volume percentage of carbon dioxide in the mixed gas of carbon dioxide and nitrogen was 6%.
The temperature of the primary reduction reaction was 700 ℃.
Step five, after the reduction reaction is finished, continuously introducing mixed gas of nitrogen and ammonia, raising the calcination temperature, and carrying out secondary nitridation reaction for 15 hours;
the volume percentage of ammonia in the mixed gas of nitrogen and ammonia is 4%.
The temperature of the secondary nitridation reaction was 1000 ℃.
And step six, placing the reacted mixture into a vacuum environment for natural cooling to form the vanadium-nitrogen alloy additive.
The vanadium-nitrogen alloy additive contains 79.0 percent of vanadium, 19.5 percent of nitrogen and 0.43 percent of oxygen, and the contents of other elements are all in the national standard range.
Example 3
The vanadium-nitrogen alloy additive of the embodiment mainly comprises the following raw materials in parts by weight: 40 parts of ammonium metavanadate, 11 parts of iron powder, 16 parts of graphite powder, 10 parts of silicon dioxide and 8 parts of aluminum oxide.
The preparation method of the vanadium-nitrogen alloy additive of the embodiment comprises the following steps:
the method comprises the following steps: putting iron powder into a high-temperature calcining kiln, calcining at 800 ℃, continuously introducing air to completely react to generate iron oxide, and crushing and grinding the iron oxide into 240-mesh iron oxide powder with the particle size of 180-;
step two: crushing and grinding ammonium metavanadate into powder with the particle size of 180-240 meshes, and drying to obtain ammonium metavanadate powder;
step three: uniformly mixing the iron oxide powder obtained in the step (1), the ammonium metavanadate powder obtained in the step (2), silicon dioxide and aluminum oxide, and adding the mixture into a high-temperature calcining kiln;
step four, evacuating the air of the high-temperature calcining kiln added with the mixed materials, spraying graphite powder, filling mixed gas of carbon dioxide and nitrogen, and carrying out primary reduction reaction for 12 hours through high-temperature calcining;
the volume percentage of carbon dioxide in the mixed gas of carbon dioxide and nitrogen is 8%.
The temperature of the primary reduction reaction was 800 ℃.
Step five, after the reduction reaction is finished, continuously introducing mixed gas of nitrogen and ammonia, raising the calcination temperature, and carrying out secondary nitridation reaction for 16 hours;
the volume percentage of ammonia in the mixed gas of nitrogen and ammonia is 5%.
The temperature of the secondary nitridation reaction was 1200 ℃.
And step six, placing the reacted mixture into a vacuum environment for natural cooling to form the vanadium-nitrogen alloy additive.
The vanadium content in the obtained vanadium-nitrogen alloy additive is 80.5 percent, the nitrogen content is 19.0 percent, the oxygen content is 0.40 percent, and the contents of other elements are all in the national standard range
Comparative example 1
In this comparative example, nitrogen was introduced in the fourth step, and the other parameters were the same as in example 1.
The vanadium content in the obtained vanadium-nitrogen alloy additive is 75.0 percent, the nitrogen content is 12.0 percent, and the oxygen content is 0.65 percent.
Comparative example 2
In this comparative example, nitrogen was introduced in the fifth step, and the other parameters were the same as in example 2.
The vanadium content in the obtained vanadium-nitrogen alloy additive is 74.0 percent, the nitrogen content is 12.5 percent, and the oxygen content is 0.63 percent.
Claims (4)
1. The vanadium-nitrogen alloy additive is characterized by mainly comprising the following raw materials in parts by weight: 30-40 parts of vanadium compound, 8-11 parts of iron powder, 12-16 parts of graphite powder, 6-10 parts of silicide and 6-8 parts of aluminum oxide.
2. The vanadium-nitrogen alloy additive according to claim 1, wherein the vanadium compound is at least one of vanadium trioxide, vanadium pentoxide and ammonium metavanadate.
3. The vanadium-nitrogen alloy additive according to claim 1 or 2, wherein the silicide is ferrosilicon powder or silicon dioxide.
4. A method for preparing a vanadium-nitrogen alloy additive according to any one of claims 1 to 3, characterized by comprising the following steps:
the method comprises the following steps: putting iron powder into a high-temperature calcining kiln, carrying out high-temperature firing at 800 ℃ in 600-plus-one temperature, continuously introducing air to enable the iron powder to react completely to generate iron oxide, and crushing and grinding the iron oxide into 240-mesh iron oxide powder with the particle size of 180-plus-one temperature;
step two: crushing and grinding the vanadium compound into powder with the particle size of 180-240 meshes, and drying to obtain vanadium compound powder;
step three: uniformly mixing the iron oxide powder obtained in the step (1), the vanadium compound powder obtained in the step (2), silicide and aluminum oxide, and adding into a high-temperature calcining kiln;
step four, evacuating the air of the high-temperature calcining kiln added with the mixed materials, spraying graphite powder, filling mixed gas of carbon dioxide and nitrogen, and carrying out primary reduction reaction for more than 6 hours through high-temperature calcining;
in the mixed gas of carbon dioxide and nitrogen, the volume percentage of carbon dioxide is 5-8%;
the temperature of the primary reduction reaction is 600-800 ℃;
step five, after the reduction reaction is finished, continuously introducing mixed gas of nitrogen and ammonia, raising the calcination temperature, and carrying out secondary nitridation reaction for more than 12 hours;
in the mixed gas of nitrogen and ammonia, the volume percentage of ammonia is 3-5%;
the temperature of the secondary nitridation reaction is 700-1200 ℃;
and step six, placing the reacted mixture into a vacuum environment for natural cooling to form the vanadium-nitrogen alloy additive.
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Cited By (3)
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| CN113333739A (en) * | 2021-05-29 | 2021-09-03 | 湖南众鑫新材料科技股份有限公司 | Method for increasing nitrogen content in powdery vanadium-nitrogen alloy |
| CN114164371A (en) * | 2021-12-07 | 2022-03-11 | 九江市钒宇新材料股份有限公司 | Activating agent for preparing vanadium-nitrogen alloy and preparation method thereof |
| CN115927947A (en) * | 2022-12-12 | 2023-04-07 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of vanadium-nitrogen alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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