CN1775661A - Method for preparing vanadium nitride - Google Patents
Method for preparing vanadium nitride Download PDFInfo
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- CN1775661A CN1775661A CN 200510022245 CN200510022245A CN1775661A CN 1775661 A CN1775661 A CN 1775661A CN 200510022245 CN200510022245 CN 200510022245 CN 200510022245 A CN200510022245 A CN 200510022245A CN 1775661 A CN1775661 A CN 1775661A
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Abstract
The invention provides a method for preparing vanadium nitride, raising the temperature of ammonium melavanadate, ammonium polyvanadate, V2O5 whose crystallization water content is smaller than 8wt% or greater than 10wt%, VO2, V2O3, VO, or other low-valence vanadium oxides and V-Fe alloys, or their mixture in the reducing atmosphere containing nitrogen element or nitrogen and carbon elements up to 400-800 deg.C to react for 0.5-48 hours, so as to obtain the vanadium nitride whose oxygen content is less than 3%. The vanadium nitride powder is pressed by equistatic pressure blocking into balls or blocks with apparent density greater than 3.0g/ml so as to be used in the additives for V-containing alloy steels or other V-containing alloys. The advantages of the invention are that its reaction temperature is low, it can save energy sources, it can continuously produce and it is suitable for large scale industrialized production.
Description
Technical field
The invention belongs to the ferrous metallurgy field, relate to the preparation method of vanadium nitride.
Background technology
Vanadium nitride is a kind of good steel-making additive, can improve and improve the comprehensive mechanical performance and the welding property of steel significantly.With use vanadium iron to compare can to save 20%～40% vanadium resource, thereby reduced the STEELMAKING PRODUCTION cost.With the construction industry is example, and the new grade III steel muscle that uses the production of VN alloy technology has not only strengthened security, shock resistance, obdurability, the welding property of buildings because of its intensity improves, and can also use regular reinforcement to save advantages such as steel 10% to 12%.
People such as J.H.Downing disclosed in US3334992 in 1967, with the V of 181Kg
2O
5, the 62Kg carbon dust, behind 4.1Kg gum resin and the 3Kg iron powder mixing, compression moulding under 20.68MPa, sample size is 51 * 51 * 38mm.Carry out carbon reduction under 1385 ℃ and 22.7Pa vacuum, system vacuum tightness drops to 2666Pa and keeps 60h again during reduction, and system vacuum tightness reverts to 22.7Pa again, indicates that promptly reduction process finishes.Stop heating with stove this moment, and sample is come out of the stove when being cooled to room temperature, and that obtain is vanadium carbide (VC
x).When vacuum tightness returns to 22.7Pa, stove does not stop heating and temperature when reducing to 1100 ℃, and delivering to nitrogen in the stove and keeping the dividing potential drop of nitrogen is P N2=700～1000Pa.The elder generation constant temperature ooze helium 2h, then furnace temperature is transferred to 1000 ℃ ooze again helium 6h electric furnace stop the heating, under helium-atmosphere, be chilled to room temperature and come out of the stove, the chemical constitution of its product is:
78.75%V-10.5%C-7.3%N is so claim that again this VN is VCN.
U.S. combinating carbide company disclosed in U.S. Pat 4040814 in 1977, V2O3 and carbon had been prepared nitrogenous 12% vanadium nitride at 1100～1500 ℃ of following reduction nitridations.
The people such as J.B.Goddard of Union Carbide Corporation in 1985 disclose in U.S. Pat 4562057, with the high oxide V of vanadium
2O
5Or ammonium vanadate is a raw material, with mixed gas (nitrogen+ammonia) is reductive agent and nitridizing agent, earlier at 675～700 ℃ of following prereduction 1h, low melting point high price barium oxide is reduced to dystectic low price barium oxide, under 950 ℃, reduce simultaneously afterwards and nitriding 3～4h, can obtain the product of 73.3%V, 12.6%N, 15.3%O, and then about 1400 ℃, remove wherein a large amount of oxygen with carbothermic method and get carbon vanadium nitride product.
People (Thin Solid Films, 349 (1999) 14～18) such as I.Galesic had delivered with quick thermal treatment process 1100 ℃ of methods that prepare the vanadium nitride film in 1999.
2000, Prabhat Kumar Tripathy was at J.Mater.Chem., disclosed at 1500 ℃ with V in 2001,11,691～695
2O
5For reducing, material carbon heat and N2 prepared vanadium nitride.
The thick grade of Wang Gong people in 1988 uses V
2O
5With the activated carbon compound stalk forming, carry out carbothermic reduction under experiment condition, reduction generates VC earlier under 1673K and 1.333Pa vacuum, feeds nitrogen subsequently, nitriding is 1.5 hours under PM=101325Pa, can obtain 86%V, 7%C, 9.069%～9.577%N, 2%O sample.In order to improve vanadium nitride intensity, in raw material, add 3% iron powder.
People such as calendar year 2001 grandson morning sunlight disclose in Chinese patent CN1422800A; with pulverous barium oxide; briquetting behind carbonaceous pulvis and the binding agent mixing; moulding; again the material after the moulding is added the preparation stove continuously; do reaction and shielding gas to preparation stove feeding ammonia or nitrogen simultaneously; the preparation stove is heated to 1000～1800 ℃; carbonization and nitrogenizing reaction have taken place in this material in stove; time length was less than 6 hours; to under protective atmosphere, be cooled to 100～250 ℃ before coming out of the stove, come out of the stove and promptly get the vanadium nitride product.
The vanadium nitride preparation method that people such as Yang Zhi loyalty in 2003 disclose in Chinese patent CN1478915A is that Vanadium Pentoxide in FLAKES is become VO2 or V2O3 400～800 ℃ of prereduction earlier, finally is reduced into vanadium nitride at 1000～1500 ℃ again.
The logical grade of Sui Zhi disclosed in Chinese patent CN1212416A in 2003, in the presence of the density reinforcer, at 1300～1500 ℃ of reduction nitridation 0.5～8h, prepared vanadium nitride.
Servaas Middelhoek in 1973 etc. disclose in U.S. Pat 3745209, are raw material with the Vanadium Pentoxide in FLAKES, have synthesized vanadium nitride with ammonia and Sweet natural gas reduction nitridation down at 800～1250 ℃.
China Changsha Longtai Science Co., Ltd discloses in CN1644510, is that raw material is preparing nitrogenous about 14% vanadium nitride more than 1420 ℃ with the method for microwave heating, with the vanadous oxide.
The common drawback of above method is that temperature of reaction is higher, and energy consumption is big.
Zheng Chen scheme in 2002 waits in Chinese patent CN1380247A with (NH
4)
5[(VO)
6(CO
3)
4(OH)
9] 10H
2O is a raw material, has synthesized vanadium nitride under 750～1100 ℃.
People such as high Lian disclosed in Chinese patent CN1431146A in 2003, with the Vanadium Pentoxide in FLAKES (V that contains a crystal water of special methods preparation
2O
5H
2O, the crystal water mass percent is about 9%) be to prepare vanadium nitride in 3～5 hours 500～800 ℃ of insulations by raw material.
Arai in 1991, Tohru have disclosed under 700 ℃ in the metallic surface vapour deposition vanadium nitride in EP471276.
More than three kinds of methods adopt special synthetic special material, raw material obtains difficulty, price height.
Christopher Allen Bennett reached H.Kwon in its Ph D dissertation in 2002, S.Choi etc. are at Journal of Catalysis 184, disclose in the paper on the 236-246 (1999), at 800～1000 ℃ of following micropreparations as the vanadium nitride of the high-specific surface area of catalyzer.The shortcoming of this method is to prepare on thermal-analysis instrumentation, and its preparation amount is very little, has only gram even milligram level.
In sum, among the existing preparation method, all preparations in enormous quantities, then temperature of reaction is generally more than 1000 ℃.In lower temperature of reaction, then must adopt special presoma, as the preparation method of Zheng Chenmou etc., perhaps adopt monohydrate with the nano level Vanadium Pentoxide in FLAKES of special methods preparation or amorphous state as raw material.Energy consumption is big, the raw materials cost height.
Summary of the invention
The object of the present invention is to provide that a kind of energy consumption is low, efficient is high, raw material is easy to get, low for equipment requirements prepare metallurgical method with vanadium nitride.
The object of the present invention is achieved like this: with metavanadic acid ammonia, ammonium poly-vanadate, arsenic, crystal water content Vanadium Pentoxide in FLAKES, the VO less than 8% (weight percent)
2, V
2O
3, VO or other barium oxide, ferro-vanadium at a low price, or more than contain vanadium raw materials mixture in the reducing atmosphere of nitrogenous or nitrogenous and carbon, be warmed up to 400～800 ℃ of reactions 0.5～48 hour, obtain the vanadium nitride product.By waiting static pressure briquetting, the vanadium nitride powder compression is become apparent density spherical or block greater than 3.0g/ml, for use in the additive of vanadium steel or other vanadium-containing alloy.
Further be that the preparation process of vanadium nitride of the present invention can be carried out in vertical heater, rotary kiln, tunnel furnace or pushed bat kiln.
Further be that the reactant vanadium raw materials enters into total residence time of reactor between 1～30h.
Further be, contain ammonia, nitrogen or organic amine in the reducing atmosphere, perhaps their mixture.
Further be when containing a certain amount of carbon in the needs product vanadium nitride, can in reducing atmosphere, add Sweet natural gas or other volatilizable organic carbon.
Further be when containing a certain amount of carbon in the needs product vanadium nitride, the mixed back of vanadium raw materials and not volatile carbon source can added in the reactor.
Further be that reactor used is tunnel furnace, pushed bat kiln, rotary kiln or vertical kiln reactor.Solid and gas material can continuously feeding and dischargings in rotary kiln, tunnel furnace, pushed bat kiln or vertical reactor.
Further be, even vanadium raw materials adopts ammonium meta-vanadate, partial reduction in advance.
Further be to be prepared into carbon content less than 1% or still less vanadium nitride product.
Further be, the method for static pressure such as usefulness is with Powdered vanadium nitride product briquette forming, and the briquetting apparent density is greater than 3.0g/ml.Isostatic pressing process can be used wet bag technology or dry bag technology.
Utilize the vanadium nitride product of technical scheme of the present invention preparation, content of vanadium is greater than 75%, and oxygen level is less than 2%, carbon content 0～12%, nitrogen content 10～21.5%.
Compared with the prior art, the present invention has following characteristics:
1. temperature of reaction is low, the corresponding reduction of energy consumption;
2. temperature of reaction is low, to the material of kiln reactor require, insulation requires corresponding reduction, the also corresponding reduction of facility investment and maintenance cost.
3. technology does not have particular requirement to vanadium raw materials, such as using the intermediate product arsenic (V that produces in the black vanadium production process
2O
5Dihydrate, trihydrate, the hydrate that contains SO3 group, a small amount of monohydrate, vanadic acid, metavanadic acid, the mixture of poly vanadic acid), do not need special earlier with the reduction of pentavalent vanadium or be prepared into other vanadium compound or synthetic monohydrate (V at a low price
2O
5H
2O).
4. the gas phase carbon dope be can pass through, ball mill mixing and briquette forming exempted.
5. can realize the serialization production that the high labour intensity of level of automation is low by rotary kiln.
Description of drawings.
Curve a, b, c, d, e are respectively the X-ray powder diffraction of the vanadium nitride sample for preparing by embodiment 1,2,3,4 and 5 in the accompanying drawing.
Embodiment
Concrete technical solution of the present invention now is described in conjunction with the embodiments.
Embodiment 1
3.0kg piece of Vanadium (purity 98.6%, down together) is pulverized 65 mesh sieve, put into the hopper of rotary kiln, powder was sent into the kiln system of sealing by feeding screw.Kiln bore 99mm, long 146cm, heating segment length 90cm, 780 ± 10 ℃ of heating zone controlled temperature, boiler tube inclination angle 1.5 degree, rotating speed 1r/min.Material is mean residence time 2h in whole boiler tube.The about 450g of charging per hour, ammonia flow 0.5m3/h is with the solid materials adverse current feeding.The about 300g of hourly output, product are dark red brown, and it is golden yellow that the part crystal face is.Continuous production 7 hours, altogether the about 2.0kg of product (have in the kiln part residual).Product is formed V77.5%, N18.6%, O2.6%, C＜0.01%.
Embodiment 2
Piece of Vanadium is smashed to pieces, cross the sieve of aperture 4mm, that gets aperture 1mm sieve tails over part 2.1kg, put into vertical tubular furnace saturated under the ammonia atmosphere of Trimethylamine in 400 ℃ of reduction 1h, be warmed up to 650 ℃ of reduction 30h then and get vanadium nitride product kg, product consists of V78.1%, N16.6%, O1.2%, C2.8%.
Embodiment 3
Piece of Vanadium is smashed to pieces, cross the sieve of aperture 4mm, that gets aperture 1mm sieve tails over part kg, put into several square stainless steel trays, it under ammonia and Sweet natural gas (the carbon mol ratio is 10: 1 in ammonia and the Sweet natural gas) atmosphere is 800 ℃ pushed bat kiln by highest temperature district temperature, the vanadium material is corresponding to preheating section, highest temperature section, ℃ discharging of temperature descending section postcooling to 150 in pushed bat kiln, in the highest temperature district residence time is 1h, get vanadium nitride product kg, product consists of V77.8%, N18.2%, O2.3%, C0.8%.
Embodiment 4
The 3.0kg piece of Vanadium was pulverized 65 mesh sieve, the ratio and the graphite ball milling that add 33g graphite in every 100g vanadium pentoxide powder are mixed, with this as raw material and by method described in the embodiment 1 handle the vanadium nitride product, it consists of: V78.4%, N14.1%, O1.9%, C8.2%, uncombined carbon wherein～3%.
Embodiment 5
According to embodiment 1, replace the ammonia that is fed and be divided into two-way with nitrogen, one the road is earlier saturated through 25 ℃ toluene solution, another road is saturated through 25 ℃ triethylamine, then the mixed back of this two-way gas is entered rotary kiln with the direction with vanadium material adverse current, the consisting of of the vanadium nitride product that obtains: V79.1%, N13.7%, O0.9%, C4.9%.
Embodiment 6
The mixed ball milling of each 1kg of vanadium nitride product of the foregoing description 1～5 is also crossed 100 mesh sieves, in 70 the soft bags of latexes of packing into then, the about 70g of each latex rubber bag charge amount.With these latex rubber bag sealed after being vacuumized, divide three batches respectively at the inferior static pressure briquetting of the pressure of 100MPa, 250MPa, 450MPa, not very regular globular vanadium nitride, apparent density is respectively 3.05,3.2,3.5g/ml.
Embodiment 7
The mixed ball milling of each 1kg of vanadium nitride product of the foregoing description 1～5 is also crossed 100 mesh sieves, on the dry bag method isopressing device of 100MPa, be pressed into slightly irregular spherical product then, every about 100g, recording its apparent density is 3.1g/ml.
Claims (9)
1. a method for preparing vanadium nitride is characterized in that: will contain vanadium raw materials in the mobile reducing atmosphere, and be warmed up to 400～950 ℃ of 0.5～48 hour synthetic vanadium nitrides of reaction down;
The described vanadium raw materials that contains is: metavanadic acid ammonia, ammonium poly-vanadate, arsenic, crystal water content are less than 8% or greater than the Vanadium Pentoxide in FLAKES of 10% (weight percent), no crystal water Vanadium Pentoxide in FLAKES, VO
2, V
2O
3, VO or other barium oxide, ferro-vanadium at a low price, or more than contain the mixture of vanadium raw materials;
Described reducing atmosphere is: ammonia, N
2, organic amine, hydrogen, CO, Sweet natural gas, benzene or other carbonaceous organic material, or the mixture of above material.
2. the preparation method of vanadium nitride according to claim 1, it is characterized in that: temperature of reaction is 400～800 ℃;
The described vanadium raw materials that contains is: metavanadic acid ammonia, ammonium poly-vanadate, arsenic, crystal water content are less than 8% or greater than the Vanadium Pentoxide in FLAKES of 10% (weight percent), no crystal water Vanadium Pentoxide in FLAKES, VO
2, V
2O
3, VO or other barium oxide, ferro-vanadium at a low price, or more than contain the mixture of vanadium raw materials;
Described reducing atmosphere is: ammonia, N
2, organic amine, hydrogen, CO, Sweet natural gas, benzene or other carbonaceous organic material, or the mixture of above material.
3. the preparation method of vanadium nitride according to claim 2 is characterized in that:
The described vanadium raw materials that contains is: metavanadic acid ammonia, ammonium poly-vanadate, arsenic, crystal water content are less than 4% or greater than the Vanadium Pentoxide in FLAKES of 15% (weight percent), no crystal water Vanadium Pentoxide in FLAKES, VO
2, V
2O
3, VO or other barium oxide, ferro-vanadium at a low price, or more than contain the mixture of vanadium raw materials;
Reactor used is tunnel furnace, pushed bat kiln, rotary kiln or vertical kiln reactor;
The vanadium nitride product oxygen level for preparing is less than 3%.
4. according to the preparation method of claim 2 or 3 described vanadium nitrides, it is characterized in that: the reaction times under 400～800 ℃ of temperature is 1～30 hour.
5. according to the preparation method of claim 2 or 3 described vanadium nitrides, it is characterized in that: with waiting static pressure method that the gained vanadium nitride is pressed into the bulk of apparent density greater than 3.0g/ml.
6. according to the preparation method of claim 2 or 3 described vanadium nitrides, it is characterized in that: the mol ratio of carbon and nitrogen is 0～10 in the reducing atmosphere.
7. according to the preparation method of claim 2 or 3 described vanadium nitrides, it is characterized in that: in vanadium raw materials, sneak into graphite, gac, carbon nanotube, carbon black, pitch, starch or other carbon compound in advance.
8. according to the preparation method of claim 2 or 3 described vanadium nitrides, it is characterized in that: content of vanadium is greater than 65% in the prepared vanadium nitride, and oxygen level is less than 3%, carbon content 0～20%, nitrogen content 5～25%.
9. the preparation method of vanadium nitride according to claim 8 is characterized in that: content of vanadium is greater than 75% in the prepared vanadium nitride, and oxygen level is less than 2%, carbon content 0～12%, nitrogen content 10～22%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457605C (en) * | 2006-07-06 | 2009-02-04 | 四川大学 | Process for preparing nano vanadium nitride and nano vanadium carbonitride powder |
| CN101851749A (en) * | 2010-03-12 | 2010-10-06 | 江苏工业学院 | Method for preparing vanadium nitride coating by using low-temperature flowing layer and device thereof |
| CN101392333B (en) * | 2007-09-20 | 2010-12-22 | 杭州天港生物科技有限公司 | Vanadium-nitrogen alloy preparation method and device |
| CN103754839A (en) * | 2013-11-15 | 2014-04-30 | 上海大学 | Preparation method of nanocrystal vanadium nitride powder |
| CN105087994A (en) * | 2015-09-06 | 2015-11-25 | 湖南众鑫新材料科技股份有限公司 | Method for preparing high-nitrogen high-purity vanadium-nitrogen alloy |
| CN106006736A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution |
| CN106399786A (en) * | 2016-11-25 | 2017-02-15 | 南通汉瑞新材料科技有限公司 | Novel method for preparing vanadium-nitrogen alloy |
| CN106809808A (en) * | 2015-11-27 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of preparation method of uniform hollow ball-shape VN nano particles |
| CN109437126A (en) * | 2018-10-29 | 2019-03-08 | 福州大学 | A kind of method and application of simple synthesis VN hollow sphere |
| CN114318015A (en) * | 2021-12-31 | 2022-04-12 | 马鞍山钢铁股份有限公司 | Treatment and utilization method of waste vanadium catalyst |
| CN114873569A (en) * | 2022-06-15 | 2022-08-09 | 昆明理工大学 | Method for preparing high-quality vanadium nitride by vanadium oxide reduction nitridation under reducing atmosphere |
-
2005
- 2005-12-07 CN CN 200510022245 patent/CN1775661A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100457605C (en) * | 2006-07-06 | 2009-02-04 | 四川大学 | Process for preparing nano vanadium nitride and nano vanadium carbonitride powder |
| CN101392333B (en) * | 2007-09-20 | 2010-12-22 | 杭州天港生物科技有限公司 | Vanadium-nitrogen alloy preparation method and device |
| CN101851749A (en) * | 2010-03-12 | 2010-10-06 | 江苏工业学院 | Method for preparing vanadium nitride coating by using low-temperature flowing layer and device thereof |
| CN101851749B (en) * | 2010-03-12 | 2012-08-29 | 江苏工业学院 | Method for preparing vanadium nitride coating by using low-temperature flowing layer and device thereof |
| CN103754839B (en) * | 2013-11-15 | 2016-01-13 | 上海大学 | A kind of preparation method of nanocrystal vanadium nitride powder |
| CN103754839A (en) * | 2013-11-15 | 2014-04-30 | 上海大学 | Preparation method of nanocrystal vanadium nitride powder |
| CN105087994A (en) * | 2015-09-06 | 2015-11-25 | 湖南众鑫新材料科技股份有限公司 | Method for preparing high-nitrogen high-purity vanadium-nitrogen alloy |
| CN106809808A (en) * | 2015-11-27 | 2017-06-09 | 中国科学院大连化学物理研究所 | A kind of preparation method of uniform hollow ball-shape VN nano particles |
| CN106006736A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution |
| CN106399786A (en) * | 2016-11-25 | 2017-02-15 | 南通汉瑞新材料科技有限公司 | Novel method for preparing vanadium-nitrogen alloy |
| CN109437126A (en) * | 2018-10-29 | 2019-03-08 | 福州大学 | A kind of method and application of simple synthesis VN hollow sphere |
| CN114318015A (en) * | 2021-12-31 | 2022-04-12 | 马鞍山钢铁股份有限公司 | Treatment and utilization method of waste vanadium catalyst |
| CN114318015B (en) * | 2021-12-31 | 2023-08-15 | 马鞍山钢铁股份有限公司 | Treatment and utilization method of waste vanadium catalyst |
| CN114873569A (en) * | 2022-06-15 | 2022-08-09 | 昆明理工大学 | Method for preparing high-quality vanadium nitride by vanadium oxide reduction nitridation under reducing atmosphere |
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