CN107904425A - The preparation method of ferrovanadium nitride - Google Patents
The preparation method of ferrovanadium nitride Download PDFInfo
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- CN107904425A CN107904425A CN201711205996.XA CN201711205996A CN107904425A CN 107904425 A CN107904425 A CN 107904425A CN 201711205996 A CN201711205996 A CN 201711205996A CN 107904425 A CN107904425 A CN 107904425A
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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
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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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- 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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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The invention belongs to metallurgical technology field, and in particular to a kind of preparation method of ferrovanadium nitride.Easily be mixed into fe in the ferrovanadium nitride product prepared for existing method, it is of poor quality the defects of, the present invention provides a kind of preparation method of ferrovanadium nitride, comprises the following steps：A, VFe50 and VFe80 are ground, are uniformly mixed；B, the material prepared is transferred in graphite crucible, fabric thickness is 20~50mm, adds 30~50g titanium valves as igniting agent；C, graphite crucible is transferred to reaction unit, is vacuumized after sealing, be filled with nitrogen to normal pressure, vacuumize again, be filled with nitrogen again to 7~9MPa, light igniting agent using electronic ignition, be cooled to 45~55 DEG C, ferrovanadium nitride is made.The present invention, according to self- propagating principle, utilizes closed container nitrogen pressurization electronic ignition technology using the nitrogen of 50 vanadium iron, 80 vanadium iron and cleaning as raw material, with easy to operate, labor intensity is small, and operating environment is good, the advantages that product quality produced is stablized, and recovery rate is high.
Description
Technical field
The invention belongs to metallurgical technology field, and in particular to a kind of preparation method of ferrovanadium nitride.
Background technology
Ferrovanadium nitride is progressively to expand the steel-smelting alloy additive used in recent years, can change distributing alternately for vanadium, is improved
The creep rupture strength of steel, improves the toughness and plasticity of steel, while also improves heat resistanceheat resistant intensity and anti-short creep ability.Add vanadium nitride
Iron can also reduce expensive rare vanadium metal usage amount.
In industrial production, prepare the method for ferrovanadium nitride mainly have it is following two：(1) it is using vanadium oxide, carbon dust, iron powder
Waste ferrovanadium nitride；The method raw produce quality is unstable, and impurity content changes greatly, it is difficult to produce up-to-standard nitrogen
Change vanadium iron.(2) using vanadium iron as raw material, a certain amount of iron powder is added, combustion reaction is nitrogenized in confined space and produces nitridation
Vanadium iron；Though the product quality that this method is produced is better than first method, the defects of product quality fluctuation is big is still suffered from, in alloy
Still with the presence of fe.
The content of the invention
The technical problem to be solved in the present invention is：Fe is easily mixed into ferrovanadium nitride product prepared by existing method,
The defects of of poor quality.
The present invention solve above-mentioned technical problem technical solution be：A kind of preparation method of ferrovanadium nitride is provided.This method
Comprise the following steps：
A, VFe50 and VFe80 are ground, are uniformly mixed；
B, the material prepared is transferred in graphite crucible, fabric thickness is 20~50mm, adds 30~50g titanium valves as point
Fiery agent；
C, graphite crucible is transferred to reaction unit, is vacuumized after sealing, be filled with nitrogen to normal pressure, vacuumize again, again
Nitrogen is filled with to 7~9MPa, igniting agent is lighted using electronic ignition, after reacting 30~45min, is cooled to 45~55 DEG C, be made
Ferrovanadium nitride.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, ground described in step a and cross 80 mesh sieves to be milled to granularity.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, incorporation time described in step a is 3~8min.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, the weight ratio of VFe50 and VFe80 described in step a for 38~
93 ︰ 18~175.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, the VFe50 components described in step a meet VFe50 countries mark
It is accurate；VFe80 components meet VFe80 national standards.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, vacuumizing described in step c be evacuated to vacuum for≤
0.01Pa。
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, nitrogen gas purity >=99.5%, O described in step c2≤ 0.1%.
Beneficial effects of the present invention are：
The present invention make full use of production vanadium iron caused by fine powder, directly by the use of ferrovanadium fine powder as raw material, avoid use
Vanadium iron and iron powder, V2O3, carbon dust and iron powder as raw material when, have situation existing for fe in product；The present invention with 50 vanadium iron,
80 vanadium iron and clean nitrogen, according to self- propagating principle, utilize closed container nitrogen pressurization electronic ignition technology, tool as raw material
There is the advantages that easy to operate, labor intensity is small, and operating environment is good, and the product quality produced is stablized, and recovery rate is high, be vanadium nitride
The production of ferroalloy provides a kind of green, cleaning, efficient method, has great importance.
Embodiment
The present invention provides a kind of preparation method of ferrovanadium nitride, comprise the following steps：
A, VFe50 and VFe80 are ground, are uniformly mixed；
B, the material prepared is transferred in graphite crucible, fabric thickness is 20~50mm, adds 30~50g titanium valves as point
Fiery agent；
C, graphite crucible is transferred to reaction unit, is vacuumized after sealing, be filled with nitrogen to normal pressure, vacuumize again, again
Nitrogen is filled with to 7~9MPa, igniting agent is lighted using electronic ignition, after reacting 30~45min, is cooled to 45~55 DEG C, be made
Ferrovanadium nitride.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, ground described in step a and cross 80 mesh sieves to be milled to granularity.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, incorporation time described in step a is 3~8min.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, the weight ratio of VFe50 and VFe80 described in step a for 38~
93 ︰ 18~175.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, the VFe50 components described in step a meet VFe50 countries mark
It is accurate；VFe80 components meet VFe80 national standards.
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, vacuumizing described in step c be evacuated to vacuum for≤
0.01Pa。
Wherein, in the preparation method of above-mentioned ferrovanadium nitride, nitrogen gas purity >=99.5%, O described in step c2≤ 0.1%.
Explanation will be further explained to the embodiment of the present invention by embodiment below, but do not indicated that this
The protection domain of invention is limited in described in embodiment in scope.
Embodiment 1 prepares ferrovanadium nitride using the method for the present invention
Exemplified by producing FeV55N11-A, 80 ferrovanadium fine powder 20kg, the 50 ferrovanadium fine powder 24kg for being ground to -80 mesh are taken, are filled
Enter mixing tank, with batch mixer batch mixing 8min, after mixing, on arc graphite crucible, fabric thickness 30mm, adds cloth
Enter 50g titanium valves and make igniting agent, be put into (the nitridation reaction device requirement of nitridation reaction device：It is closed, high temperature resistant, high pressure resistant), vacuumize
Except the air in closed container, nitrogen is then injected into pressure 8MPa and to keep pressure be 7~9MPa, uses ignition point
Fire is reacted, and reaction time 30min, question response terminates, and temperature is cooled to 50 DEG C ± 5 DEG C in container, stops nitrogen charging, is opened
Nitridation reaction device, takes out product.
Embodiment 2 prepares ferrovanadium nitride using the method for the present invention
Exemplified by producing FeV55N11-A, 80 ferrovanadium fine powder 21kg, the 50 ferrovanadium fine powder 23kg for being ground to -80 mesh are taken, are filled
Enter mixing tank, with batch mixer batch mixing 8min, on arc graphite crucible, fabric thickness 40mm, adds cloth after mixing
Enter 50g titanium valves and make igniting agent, be put into nitridation reaction device, vacuumize the air removed in closed container, be then injected into nitrogen to pressure
Power 8MPa, is lighted a fire using ignition and reacted, reaction time 45min, is treated that temperature is cooled to 50 DEG C or so, is opened reaction
Device, takes out.
Embodiment 3 prepares ferrovanadium nitride using the method for the present invention
Exemplified by producing FeV65N13-A, 80 ferrovanadium fine powder 37kg, the 50 ferrovanadium fine powder 5kg for being ground to -80 mesh are taken, are loaded
Mixing tank, with batch mixer batch mixing 8min, cloth is on arc graphite crucible after mixing, fabric thickness 25mm, adds
50g titanium valves make igniting agent, are put into nitridation reaction device, vacuumize the air removed in closed container, are then injected into nitrogen to pressure
8MPa, is lighted a fire using ignition and reacted, reaction time 45min, is treated that temperature is cooled to 50 DEG C or so, is opened reactor,
Take out.
The ferrovanadium nitride alloy component prepared in embodiment 1~3 is as shown in table 1 below.
1 ferrovanadium nitride alloy component statistical form of table
From the result of embodiment, N content ＞ 11% in the ferrovanadium nitride alloy prepared using the method for the present invention, and matter
Amount is stablized, and nitrogenizing effect is good, and alloying quality is good, and impurity content is low, and especially oxygen content is averagely less than 1%.
Claims (7)
1. the preparation method of ferrovanadium nitride, it is characterised in that comprise the following steps：
A, VFe50 and VFe80 are ground, are uniformly mixed；
B, the material prepared is transferred in graphite crucible, fabric thickness is 20~50mm, adds 30~50g titanium valves as igniting
Agent；
C, graphite crucible is transferred to reaction unit, is vacuumized after sealing, be filled with nitrogen to normal pressure, vacuumize, be filled with again again
Nitrogen lights igniting agent using electronic ignition, after reacting 30~45min, is cooled to 45~55 DEG C, nitridation is made to 7~9MPa
Vanadium iron.
2. the preparation method of ferrovanadium nitride according to claim 1, it is characterised in that：Ground described in step a to grind
80 mesh sieves are crossed to granularity.
3. the preparation method of ferrovanadium nitride according to claim 1, it is characterised in that：Incorporation time described in step a is 3
~8min.
4. the preparation method of ferrovanadium nitride according to claim 1, it is characterised in that：VFe50 described in step a and
The weight ratio of VFe80 is 38~93 ︰ 18~175.
5. the preparation method of ferrovanadium nitride according to claim 1, it is characterised in that：VFe50 components described in step a
Meet VFe50 national standards；VFe80 components meet VFe80 national standards.
6. the preparation method of ferrovanadium nitride according to claim 1, it is characterised in that：Vacuumizing described in step c
It is≤0.01Pa to vacuum.
7. the preparation method of ferrovanadium nitride according to claim 1, it is characterised in that：Nitrogen gas purity described in step c >=
99.5%, O2≤ 0.1%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711205996.XA CN107904425B (en) | 2017-11-27 | 2017-11-27 | Preparation method of nitrided ferrovanadium |
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| CN201711205996.XA CN107904425B (en) | 2017-11-27 | 2017-11-27 | Preparation method of nitrided ferrovanadium |
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| CN107904425B CN107904425B (en) | 2020-05-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (5)
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| CN1873036A (en) * | 2005-05-30 | 2006-12-06 | 三河燕郊新宇高新技术陶瓷材料有限公司 | Production method of burning synthesis for preparing 50 iron vanadium nitride |
| CN101824556A (en) * | 2009-03-05 | 2010-09-08 | 承德金科科技开发有限责任公司 | Method for producing ferrovanadium nitride by adopting self-propagating high temperature synthesis process |
| CN102644015A (en) * | 2012-04-11 | 2012-08-22 | 河北钢铁股份有限公司承德分公司 | Production method for vanadium nitride ferroalloy |
| CN103834849A (en) * | 2014-03-07 | 2014-06-04 | 承德金科科技开发有限责任公司 | FeV45N10 ferric vanadium nitrate and combustion synthesis method thereof |
| CN103866175A (en) * | 2014-02-24 | 2014-06-18 | 承德金科科技开发有限责任公司 | Ferrous vanadium nitride (FeV65N13) and synthetic method thereof |
-
2017
- 2017-11-27 CN CN201711205996.XA patent/CN107904425B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1873036A (en) * | 2005-05-30 | 2006-12-06 | 三河燕郊新宇高新技术陶瓷材料有限公司 | Production method of burning synthesis for preparing 50 iron vanadium nitride |
| CN101824556A (en) * | 2009-03-05 | 2010-09-08 | 承德金科科技开发有限责任公司 | Method for producing ferrovanadium nitride by adopting self-propagating high temperature synthesis process |
| CN102644015A (en) * | 2012-04-11 | 2012-08-22 | 河北钢铁股份有限公司承德分公司 | Production method for vanadium nitride ferroalloy |
| CN103866175A (en) * | 2014-02-24 | 2014-06-18 | 承德金科科技开发有限责任公司 | Ferrous vanadium nitride (FeV65N13) and synthetic method thereof |
| CN103834849A (en) * | 2014-03-07 | 2014-06-04 | 承德金科科技开发有限责任公司 | FeV45N10 ferric vanadium nitrate and combustion synthesis method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115821100B (en) * | 2022-11-21 | 2024-05-31 | 攀钢集团研究院有限公司 | Method for preparing vanadium nitride iron by using pushed slab kiln |
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