CN103255302A - Process for producing vanadium-nitrogen alloy by plasma nitrogen gas - Google Patents
Process for producing vanadium-nitrogen alloy by plasma nitrogen gas Download PDFInfo
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- CN103255302A CN103255302A CN201310162277XA CN201310162277A CN103255302A CN 103255302 A CN103255302 A CN 103255302A CN 201310162277X A CN201310162277X A CN 201310162277XA CN 201310162277 A CN201310162277 A CN 201310162277A CN 103255302 A CN103255302 A CN 103255302A
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Abstract
The invention discloses a process for producing vanadium-nitrogen alloy by plasma nitrogen gas. The process comprises the following steps of: (1), mixing and forming a vanadium-oxygen compound with carbon powder by pressing; (2), filling the formed compaction blank to a roasting device; and (3), filling the compaction blank to a medium-frequency vertical furnace, heating the medium-frequency vertical furnace to 1000 DEG C under the vacuum condition of 100pa-300pa, preserving the heat for 1-2 hours, charging active nitrogen gas treated by a plasma generator, and carrying out carbonization reaction and nitridization reaction in sequence, cooling the materials to 50 DEG C-250 DEG C, and discharging to obtain the product which is the vanadium-nitrogen alloy. According to the process for producing vanadium-nitrogen alloy by plasma nitrogen gas disclosed by the invention, the nitrogen gas treated by the plasma generator is utilized for nitriding, so that the speed at a high-temperature nitriding stage is increased, the energy consumption is lowered, and the loss of medium-frequency vertical furnace material is reduced.
Description
Technical field
The present invention relates to a kind of iron and steel microalloying additive---the production technique of VN alloy, relate in particular to the technology of utilizing plasma nitrogen production VN alloy, belong to metallurgical technology field.
Background technology
The micro-alloying technology of China's use at present has vanadium, niobium two big classes.China has a large amount of v-ti magnetite ore resources, and vanadium resource is abundant relatively, and vanadium micro-alloying uses more general.Because the excellent comprehensive strengthening effect of vanadium and nitrogen and can effectively save vanadium resource.As the VN alloy that two kinds of elements of vanadium nitrogen can be provided suitability for industrialized production, and obtain tangible society and economic benefit.
The variation of existing VN alloy production technique, but its production technique all adopts nitrogen to carry out nitriding.Nitrogen is a kind of rare gas element, chemical property is very stable, be difficult under the normal temperature react with other materials, only under high temperature, high-energy condition, just react with some material, it is general that its chemical bond just can rupture more than 3000 degree when temperature reaches, and VN alloy production temperature is below 1600, and the stability of nitrogen causes that high-temperature ammonolysis operation speed is slow in the VN alloy production process, the time is long.This phase temperature high energy consumption height causes the main phase of furnace high-temperature consumptive material loss especially.
Summary of the invention
The objective of the invention is to overcome the shortcoming that high-temperature ammonolysis operation speed is slow in the prior art, the time is long, energy consumption is high, a kind of technology by plasma generator activating nitrogen gas production VN alloy is provided, shorten the time of high-temperature ammonolysis operation, cut down the consumption of energy.
For achieving the above object, the present invention adopts following technical scheme to realize:
A kind of plasma nitrogen production VN alloy technology comprises the steps:
1) compression moulding after oxyvanadium compound and the carbonaceous powder mixes;
2) pressed compact after the moulding is encased in the calciner;
3) in pressed compact was packed the intermediate frequency shaft furnace into, the intermediate frequency shaft furnace was heated to 1000 ℃ under vacuum 100-300pa condition, and was incubated 1-2 hour; Charge into the active nitrogen gas of handling through plasma generator then, guarantee malleation 0.8-1.0Mpa, temperature rises to 1200 ℃-1500 ℃, is incubated 3-5 hour, carries out carburizing reagent, generates vanadium carbide; Then nitrogen guarantees malleation 0.3-0.5MPa, and temperature rises 1200-1400 ℃, is incubated 1 hour, and material and nitrogen carry out nitrogenizing reaction in the stove, generates vanadium nitride; At last material is cooled to 50-200 ℃, delivers from godown, product is VN alloy.
Described vanadium nitrogen compound is Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or their mixture, preferably vanadium tetraoxide.
Described carbonaceous powder is Graphite Powder 99, crystalline flake graphite, preferably Graphite Powder 99.
Described calciner is shaft furnace or tunnel furnace, and the temperature of shaft furnace is 1200-1400 ℃, and the temperature of tunnel furnace is 1300-1500 ℃.
The nitrogen content of described vanadium nitride is 16-18%.
The VN alloy hot stage is consuming time to be 3-6 hour, and this phase temperature is 1250-1350 ℃.
The invention has the advantages that: the nitrogen that uses plasma generator to handle carries out nitriding, make the VN alloy hot stage reduce to 3-6 hour by original 8-12 hour, accelerated the speed in high-temperature ammonolysis stage, temperature also has been reduced to 1250 ℃-1350 ℃ by 1400 ℃-1600 ℃, reduce energy consumption, also reduced the consume of the perpendicular rate material of intermediate frequency.
Embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
A kind of plasma nitrogen production VN alloy technology comprises the steps:
1) compression moulding after oxyvanadium compound and the carbonaceous powder mixes;
2) pressed compact after the moulding is encased in the calciner;
3) pressed compact is packed in the intermediate frequency shaft furnace, the intermediate frequency shaft furnace is heated to 1000 ℃ under vacuum 100-300pa condition, and insulation charged into the active nitrogen gas that plasma generator is handled after 1-2 hour in stove, through carbonation stage, nitrogenize stage and cooling stages, make VN alloy.
Charge into the purpose of nitrogen on the one hand as shielding gas, prevent material in reaction process by secondary oxidation, reduce the dividing potential drop of reaction product greatly, be the reactant gases as nitrogenizing reaction on the other hand.
The purpose of carbonization is the oxygen of deviating from the raw material, and for nitrogenize creates conditions, temperature is crossed the high energy consumption height, increases cost, crosses to hang down and can cause the deoxidation deficiency.The temperature control of carbonization is at 1200-1500 ℃.
The nitrogenize phase temperature is 1250-1350 ℃, and temperature is too high to be unfavorable for the nitriding reaction, and the depth of penetration of crossing low nitrogen is not enough.
Cooling stages is in order to prevent the secondary oxidation of product.Typical temperature is 50-200 ℃.
Furnace pressure is pressure-fired, and charing stage pressure-controlling is 0.8-1.0Mpa, and nitrogenize stage pressure-controlling is 0.3-0.5MPa.
Embodiment 1
Vanadium tetraoxide powder and the 200kg Graphite Powder 99 of quality 1000kg are mixed, carrying out the dry powder pressure ball to rolling ball press, be 2400kg/h to the delivery rate of rolling ball press, the forming pressure of rolling ball press is 80Mpa, makes footpath 30mm, the elliposoidal blank of thickness 10mm, material base after the moulding drops in the intermediate frequency shaft furnace, intermediate frequency furnace is evacuated to 280pa, is being heated to 1000 ℃ simultaneously, be incubated 2 hours; Charge into the active nitrogen gas that plasma generator is handled in stove, guarantee malleation 1.0Mpa, temperature rises to 1300 ℃, is incubated 3 hours, carries out carburizing reagent, generates vanadium carbide; Then nitrogen guarantees malleation 0.5MPa, and temperature rises to 1350 ℃, is incubated 1 hour, and material and nitrogen carry out nitrogenizing reaction in the stove, generates vanadium nitride; At last material is cooled to 150 ℃, delivers from godown, obtain the 260kg VN alloy, the product content of vanadium 78% by analysis, nitrogen content 17.5%.
Embodiment 2
Vanadous oxide powder and the 200kg Graphite Powder 99 of quality 1000kg are mixed, carrying out the dry powder pressure ball to rolling ball press, be 2400kg/h to the delivery rate of rolling ball press, the forming pressure of rolling ball press is 80Mpa, makes footpath 30mm, the elliposoidal blank of thickness 10mm, material base after the moulding drops in the intermediate frequency shaft furnace, intermediate frequency furnace is evacuated to 280pa, is being heated to 1000 ℃ simultaneously, be incubated 2 hours; Charge into the active nitrogen gas that plasma generator is handled in stove, guarantee malleation 0.8Mpa, temperature rises to 1300 ℃, is incubated 3 hours, carries out carburizing reagent, generates vanadium carbide; Then nitrogen guarantees malleation 0.3MPa, and temperature rises to 1250 ℃, is incubated 1 hour, and material and nitrogen carry out nitrogenizing reaction in the stove, generates vanadium nitride; At last material is cooled to 200 ℃, delivers from godown, obtain the 270kg VN alloy, the product content of vanadium 77% by analysis, nitrogen content 16.5%.
Embodiment 3
Vanadium pentoxide powder and the 200kg Graphite Powder 99 of quality 1000kg are mixed, carrying out the dry powder pressure ball to rolling ball press, be 2400kg/h to the delivery rate of rolling ball press, the forming pressure of rolling ball press is 80Mpa, makes footpath 30mm, the elliposoidal blank of thickness 10mm, material base after the moulding drops in the intermediate frequency shaft furnace, intermediate frequency furnace is evacuated to 280pa, is being heated to 1000 ℃ simultaneously, be incubated 2 hours; Charge into the active nitrogen gas that plasma generator is handled in stove, guarantee malleation 1.0Mpa, temperature rises to 1300 ℃, is incubated 3 hours, carries out carburizing reagent, generates vanadium carbide; Then nitrogen guarantees malleation 0.4MPa, and temperature rises to 1300 ℃, is incubated 1 hour, and material and nitrogen carry out nitrogenizing reaction in the stove, generates vanadium nitride; At last material is cooled to 100 ℃, delivers from godown, obtain the 280kg VN alloy, the product content of vanadium 77.5% by analysis, nitrogen content 16.5%.
The present invention can use without prejudice to the specific form of spirit of the present invention or principal character and summarize; above-mentioned embodiment is only in order to technical scheme of the present invention to be described but not design of the present invention and protection domain are limited; those of ordinary skill of the present invention is made amendment to technical scheme of the present invention or is equal to replacement; and not breaking away from aim and the scope of technical scheme, it all should be encompassed in the claim scope of the present invention.
Claims (11)
1. a plasma nitrogen production VN alloy technology is characterized in that: comprise the steps:
1) compression moulding after oxyvanadium compound and the carbonaceous powder mixes;
2) pressed compact after the moulding is encased in the calciner;
3) in pressed compact was packed the intermediate frequency shaft furnace into, the intermediate frequency shaft furnace was heated to 1000 ℃ under vacuum 100-300pa condition, and was incubated 1-2 hour; Charge into the active nitrogen gas of handling through plasma generator then, guarantee malleation 0.8-1.0Mpa, temperature rises to 1200 ℃-1500 ℃, is incubated 3-5 hour, carries out carburizing reagent, generates vanadium carbide; Then nitrogen guarantees malleation 0.3-0.5MPa, and temperature rises to 1200-1400 ℃, is incubated 1 hour, and material and nitrogen carry out nitrogenizing reaction in the stove, generates vanadium nitride; At last material is cooled to 50-200 ℃, delivers from godown, product is VN alloy.
2. a kind of plasma nitrogen production VN alloy technology according to claim 1, it is characterized in that: described vanadium nitrogen compound is Vanadium Pentoxide in FLAKES, vanadium tetraoxide, vanadous oxide or their mixture.
3. a kind of plasma nitrogen production VN alloy technology according to claim 2, it is characterized in that: described vanadium nitrogen compound is vanadium tetraoxide.
4. a kind of plasma nitrogen production VN alloy technology according to claim 1, it is characterized in that: described carbonaceous powder is Graphite Powder 99, crystalline flake graphite.
5. a kind of plasma nitrogen production VN alloy technology according to claim 4, it is characterized in that: described carbonaceous powder is Graphite Powder 99.
6. a kind of plasma nitrogen production VN alloy technology according to claim 1, it is characterized in that: the mass ratio of oxyvanadium compound and carbonaceous powder is 4-5:1.
7. a kind of plasma nitrogen production VN alloy technology according to claim 1, it is characterized in that: described calciner is shaft furnace or tunnel furnace.
8. a kind of plasma nitrogen production VN alloy technology according to claim 7, it is characterized in that: the temperature of described shaft furnace is 1200-1400 ℃.
9. a kind of plasma nitrogen production VN alloy technology according to claim 7, it is characterized in that: the temperature of described tunnel furnace is 1300-1500 ℃.
10. a kind of plasma nitrogen production VN alloy technology according to claim 1, it is characterized in that: the nitrogen content of described vanadium nitride is 16-18%.
11. a kind of plasma nitrogen production VN alloy technology according to claim 1 is characterized in that: the VN alloy hot stage is consuming time to be 3-6 hour, and this phase temperature is 1250-1350 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543611A (en) * | 2015-12-27 | 2016-05-04 | 南通汉瑞新材料科技有限公司 | Re-transformation-utilization method for non-nitrided alloy carbide in vanadium-nitrogen alloy sintering process |
| CN106119588A (en) * | 2016-08-01 | 2016-11-16 | 江苏省冶金设计院有限公司 | Prepare the method and system of nitrogen-vanadium alloy |
| CN106148751A (en) * | 2016-08-01 | 2016-11-23 | 江苏省冶金设计院有限公司 | Prepare the method and system of nitrogen-vanadium alloy |
| CN106435243A (en) * | 2016-08-01 | 2017-02-22 | 江苏省冶金设计院有限公司 | Apparatus for preparing nitrogen-vanadium alloy |
| CN109295338A (en) * | 2018-11-29 | 2019-02-01 | 湖南众鑫新材料科技股份有限公司 | Improve the production method of content of nitrogen in vanadium-nitrogen alloy |
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| CN1562769A (en) * | 2004-03-30 | 2005-01-12 | 上海大学 | Method for preparing vanadium nitride and device |
| CN101082089A (en) * | 2007-07-12 | 2007-12-05 | 四川大学 | Preparation method of nitriding vanadium alloy |
| CN101638733A (en) * | 2009-02-04 | 2010-02-03 | 南通汉瑞实业有限公司 | Vanadium nitrogen alloy preparing method |
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- 2013-05-06 CN CN201310162277XA patent/CN103255302A/en active Pending
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| CN1562769A (en) * | 2004-03-30 | 2005-01-12 | 上海大学 | Method for preparing vanadium nitride and device |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543611A (en) * | 2015-12-27 | 2016-05-04 | 南通汉瑞新材料科技有限公司 | Re-transformation-utilization method for non-nitrided alloy carbide in vanadium-nitrogen alloy sintering process |
| CN106119588A (en) * | 2016-08-01 | 2016-11-16 | 江苏省冶金设计院有限公司 | Prepare the method and system of nitrogen-vanadium alloy |
| CN106148751A (en) * | 2016-08-01 | 2016-11-23 | 江苏省冶金设计院有限公司 | Prepare the method and system of nitrogen-vanadium alloy |
| CN106435243A (en) * | 2016-08-01 | 2017-02-22 | 江苏省冶金设计院有限公司 | Apparatus for preparing nitrogen-vanadium alloy |
| CN109295338A (en) * | 2018-11-29 | 2019-02-01 | 湖南众鑫新材料科技股份有限公司 | Improve the production method of content of nitrogen in vanadium-nitrogen alloy |
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Application publication date: 20130821 |