CN106834775A - A kind of carbon thermal reduction and the method for Nitration synthesis ferrovanadium nitride - Google Patents
A kind of carbon thermal reduction and the method for Nitration synthesis ferrovanadium nitride Download PDFInfo
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- CN106834775A CN106834775A CN201611041848.4A CN201611041848A CN106834775A CN 106834775 A CN106834775 A CN 106834775A CN 201611041848 A CN201611041848 A CN 201611041848A CN 106834775 A CN106834775 A CN 106834775A
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- thermal reduction
- ferrovanadium nitride
- iron
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- vanadium
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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
- C22C1/055—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 carbon
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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
-
- 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
Abstract
A kind of use carbon thermal reduction and the method for Nitration synthesis ferrovanadium nitride, FeV45N10, tri- trades mark of FeV55N11, FeV65N13 are divided into according to composition difference, FeV45N10 products are containing vanadium 43 49%, nitrogenous 10 13%, FeV55N11 products are containing vanadium 53 58%, nitrogenous 11 14%, FeV65N13 products are containing vanadium 63 69%, nitrogenous 12 15%, the ferrovanadium nitride of three kinds of trades mark is compact massive thing, and its density reaches 5.0 6.5g/cm3.The present invention is directly with the oxide of vanadium, the oxide of iron or iron simple substance, binding agent and carbonaceous reductant as primary raw material; after raw material mixing, mixing; compound stalk forming; then in putting it into pushed bat kiln; protected with nitrogen atmosphere; prereduction district, middle temperature carbon thermal reduction and nitridation area, high temperature sintering area and the region of cooling zone four are sequentially entered, final ferrovanadium nitride is obtained.The product compactness of present invention synthesis is good, and nitrogen content is uniform.Compared to the technique that tradition prepares ferrovanadium nitride with vanadium iron, this product directly prepares ferrovanadium nitride by raw material of barium oxide, can significantly reduce technological process and cost；The intensity of product is larger, and the wear rate in use is transported is low, loses small.
Description
Technical field
The invention belongs to ferroalloy preparation field, and in particular to a kind of ferrovanadium nitride and its method for preparation.
Background technology
China is vanadium resource big country, possesses abundant vanadium-containing shale resource, and total reserves occupy first place in the world.With China's steel
The fast development of iron industry, the demand for high-quality steel grade is also increasingly improved, and ferrovanadium nitride is used as high strength microalloy steel
A kind of important alloy addition, its demand is also improved therewith.Ferrovanadium nitride can be efficiently used nitrogen to optimize vanadium
Precipitation state, strengthens precipitation strength and the effect of refined crystalline strengthening, therefore, it is possible to optimize the performance of steel.It has now been found that, Xiang Gang
Middle addition ferrovanadium nitride alloy can improve intensity, toughness, wearability, corrosion resistance and the thermal fatigue resistance of steel, and make steel
Material possesses excellent weldability energy.Compared to vanadium iron, vanadium nitride, ferrovanadium nitride can improve the utilization of vanadium, and return
Yield, can reduce by 30% or so vanadium addition, greatly reduce the cost of high strength microalloy steel.
The main method of production ferrovanadium nitride is solid State Nitriding method, liquid nitriding process and combustion synthesis method at present.First two
Method is all that, with vanadium iron as raw material, nitrogen is passed through under uniform temperature and pressure carries out nitriding reaction, but the method is anti-
Overlong time is answered, nitriding amount is relatively low, and energy consumption is excessive, cause production ferrovanadium nitride flow complicated, high cost improves production high
The cost of intensity steel grade.Combustion synthesis method produces ferrovanadium nitride, is placed in closed pressure vessel after vanadium iron is crushed, and is passed through height
Pressure nitrogen, nitrogenizes vanadium iron powder, it is not necessary to be separately supplemented with the energy from the outside using ferrovanadium nitride liberated heat.Product is in nitrogen
Middle cooling, can obtain the compact massive product that nitrogen content is 8-12%, but the technique is again based on vanadium iron for raw material, cost
Naturally it is not low.
The content of the invention
The invention aims to directly prepare ferrovanadium nitride by raw material of barium oxide, significantly reduce technological process and
Cost.
A kind of carbon thermal reduction and the method for Nitration synthesis ferrovanadium nitride iron, it is characterised in that with the oxide of vanadium, the oxygen of iron
Compound or iron, binding agent and carbonaceous reductant are primary raw material, after the above raw material is mixed, are mixed, briquetting into
Type, then to put it into and carry out high temperature carbon thermal reduction and nitridation reaction in the pushed bat kiln full of nitrogen atmosphere, prepares described
Ferrovanadium nitride, 3 trades mark of ferrovanadium nitride point of synthesis；FeV45N10 ferrovanadium nitrides include vanadium 43-49%, nitrogen 11-13%, carbon 0-
1%, oxygen 0-1%, balance of Fe；FeV55N11 ferrovanadium nitrides 53-58% containing vanadium, nitrogenous 11-14%, carbon 0-1%, oxygen 0-1%,
Balance of Fe；FeV65N13 ferrovanadium nitrides 63-69% containing vanadium, nitrogenous 12-15%, carbon 0-1%, oxygen 0-1%, balance of Fe.Should
Product is compact massive, and density reaches 5.0-6.5g/cm3, intensity is high, and other impurities content can be controlled in extremely low level.Separately
Outward, because this method is directly raw material using barium oxide, the production process for preparing vanadium iron has been skipped, nitridation can have been greatly shortened
The production time of vanadium iron, reduce production cost, improve production efficiency.The CO gases that this technique is produced in process of production can be used for
Generate electricity or heat, realize the secondary utilization of the energy.
The present invention is achieved by the following technical solutions：
A kind of carbon thermal reduction and the method for Nitration synthesis ferrovanadium nitride, the present invention is with the oxide of vanadium, iron simple substance or its oxygen
Compound, binding agent and carbonaceous reductant are primary raw material, after the above raw material is mixed, are mixed, compound stalk forming, so
After put it into pushed bat kiln, be passed through nitrogen atmosphere, successively experience prereduction district, middle temperature carbon thermal reduction and the nitridation of pushed bat kiln
Area, high temperature sintering area and the region of cooling zone four, prepare the ferrovanadium nitride.
Further, the raw material for preparing the ferrovanadium nitride only oxide of vanadium, iron simple substance or its oxide, binding agent
And carbonaceous reductant, and no added other influences product quality raw material.Wherein the oxide of vanadium includes V2O3、V2O5With VO,
Ammonium metavanadate and ammonium poly-vanadate；The oxide of iron includes FeO, Fe2O3And Fe3O4；Carbonaceous reductant includes graphite, carbon black, activity
Charcoal, petroleum coke, coke and other carbon containing reducers；Binding agent is including flour, polyvinyl alcohol, starch, cellulose, syrup etc..
Further, the method specific steps for preparing ferrovanadium nitride include：Raw material prepare, mix and compound stalk forming and
Pushed bat kiln pyroreaction step.
Further, it is described prepare ferrovanadium nitride method be specifically：With the oxide of vanadium, the oxide of iron and carbonaceous
Reducing agent is primary raw material, after the above raw material is mixed by a certain percentage, is mixed, and is pushed in the pressure of 10-50MP
Formation of lots, then puts it into pushed bat kiln, is passed through nitrogen atmosphere, experiences the four reaction areas domain of equipment, prepares described
Ferrovanadium nitride.Regional temperature is respectively 500-650 DEG C, 650-1500 DEG C, 1500-1600 DEG C and 50-200 DEG C, right successively
The time answered respectively 1h, 3h, 2h, 1h..
Further, it is described prepare ferrovanadium nitride course of reaction be：First reactant cold stage is carried out at prereduction
Reason, reactant is restored to low price barium oxide, in case V2O5Volatilization loss, then with carbon direct reduction reactor in middle temperature area
Based on, nitridation reaction is carried out simultaneously.Secondly, in hot stage, based on sintering reaction, deepen deoxygenation, increase product
Nitrogen content, further deoxidation, decarburization, improve product quality.
Advantageous Effects of the invention：
(1) carbon thermal reduction and Nitration synthesis vanadium nitride iron-stone are carried out at ambient pressure, low for equipment requirements, small investment, factory
Room floor space is small.
(2) this technique synthesis is directly synthesized ferrovanadium nitride with barium oxide as raw material, saves and is prepared with barium oxide at present
The flow of vanadium iron, and carbon-thermal reduction and nitridation reaction are fast, substantially reduce the production cycle, it is big from the energy, equipment, raw material
Reduce production cost greatly.
(3) the ferrovanadium nitride consistency for being obtained using the synthesis technique is high, than great, up to 5-6.5g/cm3, nitrogen content
It is evenly distributed, FeV45N10 compositions are 43-49% containing vanadium, nitrogen 11-13%, carbon 0-1%, oxygen 0-1%, remaining is Fe,
FeV55N11 products are 53-58% containing vanadium, nitrogenous 11-14%, carbon 0-1%, and oxygen 0-1%, FeV65N13 product is 63- containing vanadium
69%, nitrogenous 12-15%, carbon 0-1%, oxygen 0-1%.In GB for oxygen content it is not strictly necessary that, but oxygen content pair
There is important influence in product quality, too high oxygen level can reduce the recovery rate of vanadium, the vanadium part of addition is entered into slag
In.
(4) this technique is main with barium oxide as raw material, and purity is high, reduces the impurity brought into production process, product
Middle P, S, Si, Al, Mn content is in extremely low level.
(5) product improves molten steel to vanadium, the absorptivity of nitrogen with molten steel proportion close to molten steel is soluble in, and promotes nitrogen
Invigoration effect to alloying element to steel, may be omitted with the addition of vanadium to reduce production cost.
(6) the ferrovanadium nitride intensity for being obtained using the synthesis technique is big, without broken during transport and use.
(7) this synthesis technique uses push pedal kiln plant, makes full use of the equipment advantage, and reaction is divided into four temperature provinces,
Oxygen content in abundant carbon thermal reduction reduction product, so as to improve the nitrogen content of product.
(8) this technique can produce CO gases to can be used to heat or generate electricity in process of production, realize the secondary utilization of the energy.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, the present invention is carried out further below
Describe in detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to limit this hair
It is bright.
Conversely, the present invention covers any replacement done in spirit and scope of the invention being defined by the claims, repaiies
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also completely understand the present invention.
Embodiment 1
The present invention is with V2O5、Fe2O3It is raw material with activated carbon, mixes, briquetting, in putting it into pushed bat kiln, full of nitrogen gas
Atmosphere, pushes to 650 DEG C of prereduction regions by block sample first, is incubated 2h, then pushes to 1400 DEG C of middle temperature carbon thermal reduction regions, is incubated
3h, then 1600 DEG C of high temperature sintering region 2h are pushed to, sample is finally pushed into cooling zone cooling.What the present embodiment was obtained
Nitrogen content is 12.08% in FeV45N10 ferrovanadium nitrides, and carbon content is 0.67%.Table one is this handicraft product and GB and U.S.
Strategic mineral company of state come to China promote VN alloy Nitrovan12 comparison of ingredients.It will be seen that this product from table
Product obtain nitrogen content higher under the basis of lower content of vanadium, and cost is more much lower than u s company, in addition carbon content control
In lower level.Because this product is with high-purity barium oxide as raw material, so the content of the element such as Si, Al, P, S is very
It is low, reach national top grade standard.
Table one
Embodiment 2
The present invention is with V2O3, Fe and graphite be raw material, mix, briquetting, it is first full of nitrogen atmosphere in putting it into pushed bat kiln
Block sample is first pushed into 600 DEG C of prereduction regions, 2h is incubated, then pushes to 1300 DEG C of middle temperature carbon thermal reduction regions, be incubated 3h, then
1500 DEG C of high temperature sintering region 1h are pushed to, sample is finally pushed into cooling zone cooling.The FeV55N11 that the present embodiment is obtained
Nitrogen content is 13.47% in ferrovanadium nitride, and carbon content is 0.23%.
Embodiment 3
The present invention is with NH4VO3、Fe2O3It is raw material with graphite, mixes, briquetting, in putting it into pushed bat kiln, full of nitrogen gas
Atmosphere, pushes to 450 DEG C of prereduction regions by block sample first, is incubated 2h, then pushes to 1200 DEG C of middle temperature carbon thermal reduction regions, is incubated
3h, then 1550 DEG C of high temperature sintering region 2h are pushed to, sample is finally pushed into cooling zone cooling.What the present embodiment was obtained
Nitrogen content is 14.2% in FeV65N13 ferrovanadium nitrides, and carbon content is 0.36.
Claims (7)
1. a kind of method of carbon thermal reduction and Nitration synthesis ferrovanadium nitride iron, it is characterised in that with the oxide of vanadium, the oxidation of iron
Thing or iron, binding agent and carbonaceous reductant are primary raw material, after the above raw material is mixed, are mixed, compound stalk forming,
Then to put it into and carry out high temperature carbon thermal reduction and nitridation reaction in the pushed bat kiln full of nitrogen atmosphere, prepare the nitridation
Vanadium iron, 3 trades mark of ferrovanadium nitride point of synthesis；FeV45N10 ferrovanadium nitrides include vanadium 43-49%, nitrogen 11-13%, carbon 0-1%,
Oxygen 0-1%, balance of Fe；FeV55N11 ferrovanadium nitrides 53-58% containing vanadium, nitrogenous 11-14%, carbon 0-1%, oxygen 0-1%, surplus
It is Fe；FeV65N13 ferrovanadium nitrides 63-69% containing vanadium, nitrogenous 12-15%, carbon 0-1%, oxygen 0-1%, balance of Fe.
2. the method for a kind of carbon thermal reduction according to claim 1 and Nitration synthesis ferrovanadium nitride, it is characterised in that：Product
It is compact massive, density reaches 5.0-6.5g/cm3。
3. the method for a kind of carbon thermal reduction according to claim 1 and Nitration synthesis ferrovanadium nitride, described barium oxide
It is V2O3、V2O5, VO2, VO, ammonium metavanadate and ammonium poly-vanadate.
4. the method for a kind of carbon thermal reduction according to claim 1 and Nitration synthesis ferrovanadium nitride, it is characterised in that：It is described
The compound of iron be Fe, FeO, Fe2O3And Fe3O4；In industrial processes, it is using steel scrap, iron scale, iron filings directly
Raw material.
5. the method for a kind of carbon thermal reduction according to claim 1 and Nitration synthesis ferrovanadium nitride, it is characterised in that：Carbonaceous
Reducing agent includes graphite, carbon black, activated carbon, petroleum coke, coke.
6. the method for a kind of carbon thermal reduction according to claim 1 and Nitration synthesis ferrovanadium nitride, it is characterised in that：Bond
Agent includes flour, polyvinyl alcohol, starch, cellulose, syrup.
7. the method for a kind of carbon thermal reduction according to claim 1 and Nitration synthesis ferrovanadium nitride, it is characterised in that：Specifically
Step includes：Raw material is prepared, mixed and compound stalk forming and pushed bat kiln pyroreaction step；The synthesis device for using is pushed bat kiln,
Inside is full of nitrogen, and raw material continuous conveying to the closed bin after mixing is reacted, and reaction is to carry out at ambient pressure；The push pedal
Firer makees to be divided into 4 regions, i.e. prereduction district, middle temperature carbon thermal reduction and nitridation area, high temperature sintering area and the region of cooling zone four；
Regional temperature is respectively 500-650 DEG C, 650-1500 DEG C, 1500-1600 DEG C and 50-200 DEG C, the time being corresponding in turn to point
Wei not 1h, 3h, 2h, 1h.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287493A (en) * | 2017-07-05 | 2017-10-24 | 河钢股份有限公司承德分公司 | A kind of method that waste resource recovery containing vanadium is utilized |
| CN107587024A (en) * | 2017-09-19 | 2018-01-16 | 芜湖人本合金有限责任公司 | A kind of method that alloy of vanadium nitride is prepared with vanadic anhydride and iron oxide |
| CN107604234A (en) * | 2017-09-05 | 2018-01-19 | 河钢股份有限公司承德分公司 | A kind of method for preparing silicon nitride ferrovanadium |
| CN107699780A (en) * | 2017-09-21 | 2018-02-16 | 河钢股份有限公司承德分公司 | A kind of method for preparing ferrovanadium nitride alloy |
| CN107829018A (en) * | 2017-10-27 | 2018-03-23 | 西安建筑科技大学 | A kind of method for preparing ferrovanadium nitride |
| CN107974608A (en) * | 2017-11-20 | 2018-05-01 | 西安建筑科技大学 | A kind of ferrovanadium nitride and preparation method thereof |
| CN108018474A (en) * | 2017-11-09 | 2018-05-11 | 中国电子科技集团公司第四十八研究所 | A kind of method that vanadium nitride is prepared with ammonium metavanadate serialization |
| CN110467160A (en) * | 2019-09-25 | 2019-11-19 | 攀钢集团钒钛资源股份有限公司 | Carbothermal reduction-nitridation prepares the feedstock composition of titanium nitride and the preparation method of titanium nitride |
| CN110923557A (en) * | 2019-10-30 | 2020-03-27 | 中色（宁夏）东方集团有限公司 | Preparation method of high-density nitrided ferrovanadium |
| CN110938751A (en) * | 2019-12-11 | 2020-03-31 | 湖南众鑫新材料科技股份有限公司 | Method for improving recovery rate of nitrided ferrovanadium |
| CN113736987A (en) * | 2021-08-02 | 2021-12-03 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy |
| CN115821100A (en) * | 2022-11-21 | 2023-03-21 | 攀钢集团研究院有限公司 | Method for preparing nitrided ferrovanadium by using pushed slab kiln |
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| CN105483507A (en) * | 2016-01-05 | 2016-04-13 | 北京科技大学 | Nitrided ferrovanadium alloy and preparing method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287493B (en) * | 2017-07-05 | 2019-03-05 | 河钢股份有限公司承德分公司 | A method of waste resource recovery containing vanadium utilizes |
| CN107287493A (en) * | 2017-07-05 | 2017-10-24 | 河钢股份有限公司承德分公司 | A kind of method that waste resource recovery containing vanadium is utilized |
| CN107604234A (en) * | 2017-09-05 | 2018-01-19 | 河钢股份有限公司承德分公司 | A kind of method for preparing silicon nitride ferrovanadium |
| CN107587024A (en) * | 2017-09-19 | 2018-01-16 | 芜湖人本合金有限责任公司 | A kind of method that alloy of vanadium nitride is prepared with vanadic anhydride and iron oxide |
| CN107699780A (en) * | 2017-09-21 | 2018-02-16 | 河钢股份有限公司承德分公司 | A kind of method for preparing ferrovanadium nitride alloy |
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| CN107829018A (en) * | 2017-10-27 | 2018-03-23 | 西安建筑科技大学 | A kind of method for preparing ferrovanadium nitride |
| CN108018474A (en) * | 2017-11-09 | 2018-05-11 | 中国电子科技集团公司第四十八研究所 | A kind of method that vanadium nitride is prepared with ammonium metavanadate serialization |
| CN107974608A (en) * | 2017-11-20 | 2018-05-01 | 西安建筑科技大学 | A kind of ferrovanadium nitride and preparation method thereof |
| CN110467160A (en) * | 2019-09-25 | 2019-11-19 | 攀钢集团钒钛资源股份有限公司 | Carbothermal reduction-nitridation prepares the feedstock composition of titanium nitride and the preparation method of titanium nitride |
| CN110923557A (en) * | 2019-10-30 | 2020-03-27 | 中色（宁夏）东方集团有限公司 | Preparation method of high-density nitrided ferrovanadium |
| CN110938751A (en) * | 2019-12-11 | 2020-03-31 | 湖南众鑫新材料科技股份有限公司 | Method for improving recovery rate of nitrided ferrovanadium |
| CN113736987A (en) * | 2021-08-02 | 2021-12-03 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy |
| CN113736987B (en) * | 2021-08-02 | 2023-11-28 | 河钢承德钒钛新材料有限公司 | Preparation method of nitrided ferrovanadium alloy |
| CN115821100A (en) * | 2022-11-21 | 2023-03-21 | 攀钢集团研究院有限公司 | Method for preparing nitrided ferrovanadium by using pushed slab kiln |
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