CN105002386A - Process capable of producing high-purity vanadium-nitrogen alloy on a large scale - Google Patents
Process capable of producing high-purity vanadium-nitrogen alloy on a large scale Download PDFInfo
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- CN105002386A CN105002386A CN201510558364.6A CN201510558364A CN105002386A CN 105002386 A CN105002386 A CN 105002386A CN 201510558364 A CN201510558364 A CN 201510558364A CN 105002386 A CN105002386 A CN 105002386A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title abstract description 10
- 229910001199 N alloy Inorganic materials 0.000 title abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 16
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 239000010439 graphite Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 238000005516 engineering process Methods 0.000 claims description 10
- 229910052720 vanadium Inorganic materials 0.000 claims description 10
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 10
- 241000209456 Plumbago Species 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000005049 combustion synthesis Methods 0.000 claims description 7
- 238000005121 nitriding Methods 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229910003206 NH4VO3 Inorganic materials 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000010959 steel Substances 0.000 description 24
- 229910000831 Steel Inorganic materials 0.000 description 23
- 239000000047 product Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000628 Ferrovanadium Inorganic materials 0.000 description 3
- 238000005275 alloying Methods 0.000 description 3
- -1 ferrovanadium nitride Chemical class 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910001018 Cast iron Inorganic materials 0.000 description 2
- 229910000756 V alloy Inorganic materials 0.000 description 2
- CJELDIUSJNERDX-UHFFFAOYSA-N [C].[S].[Si] Chemical compound [C].[S].[Si] CJELDIUSJNERDX-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910001208 Crucible steel Inorganic materials 0.000 description 1
- 229910000746 Structural steel Inorganic materials 0.000 description 1
- GBZWGKOCDBBAEB-UHFFFAOYSA-N [V].[Fe].[V] Chemical compound [V].[Fe].[V] GBZWGKOCDBBAEB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a process capable of producing high-purity vanadium-nitrogen alloy on a large scale and belongs to the technical field of metallurgy. A self-propagating high temperature synthetic technique is used, coarse ammonium metavanadate is used as a raw material and is directly doped with powdered carbon and ignited, NH4<+> in NH4VO3 is used for promoting nitrogen synthesis, and nitridation is performed at high temperature; after complete reaction, high purity vanadium-nitrogen alloy is cooled by introducing nitrogen gas in a graphite crucible and then taken out and crushed into blocks. The process is short in reaction time and low in energy consumption and cost, and can be produced on a large scale; produced vanadium-nitrogen alloy is high in purity with nitrogen content being larger than or equal to 17%. The nitrogen content is superior to that of American VN alloy.
Description
Technical field
The present invention relates to a kind of can the technique of the high-purity VN alloy of scale production, belong to metallurgical technology field.
Background technology
China is Iron and Steel Production state maximum in the world, is also steel consumption state maximum in the world.But using maximum in steel is low carbon-structural steel, accounts for 70% of steel usage quantity, the intensity therefore improving straight carbon steel promotes China's Iron And Steel Industry technical progress, carries out the important directions of iron structure adjustment.Its method solved strengthens alloying steel-add high-purity VN alloy.Adopt VN alloy, do not need to add other valuable alloying element again, under general hot-rolled condition, just can obtain the high-strength steel that yield strength is 550 ~ 600Mpa level, therefore obtain a wide range of applications in the exploitation of the products such as the isometric material of high strength cast iron and steel plate (band), slab, heavy wall shaped steel, weldless steel tube, CSP.
American strategy mineral company in 1998 carries out applying of VN alloy technological development and patented product VN alloy thereof at the steel industry of China, more domestic steel mills have carried out application test in production HRB400 level reinforcing bar is produced, domestic research unit and some large steel mills have carried out large quantity research on adding VN alloy in steel to the impact of steel mechanics performance and strengthening mechanism, result shows: the nitrogen in VN alloy adds after in steel as the alloying element of cheapness together with vanadium, not only performance can be produced better, more stable HRB400MpaIII level Twisted Steel and V-N steel, the add-on of 30-40% vanadium can also be saved simultaneously, greatly reduce steel product cost.American side declares, the U.S. is uniquely can the country of commercial production VN alloy, but technique not unofficial biography.Domestic enterprise is after tackling key problem test, and can be mass-produced VN alloy at present, but the output of China's vanadium-nitrogen alloy product can not meet needed for the steel such as domestic production high strength cast iron at present.We adopted SHS technology R&D and production ferrovanadium nitride from 2003, and some large steel mills are successfully applied to the production of V-N steel at home, and result of use quite or be better than U.S.'s VN alloy.
SHS technology finds when being USSR (Union of Soviet Socialist Republics) academy of sciences chemical physics place exploration rocket solid fuel in 1967, its composition principle first utilizes the outside minute quantity energy provided, bring out the high heat-producing chemical reaction in powder or powdered compact between foreign peoples's material, with the combustion wave of forming reactions leading edge, after this building-up reactions brings out the continuation chemical reaction self-sustaining burning of contiguous material again under the support of self-heat generation, until whole complete and compound-materials of the required composition and structure of synthesis of material reaction.The advantage of SHS technology is energy-conservation (building-up process does not need external energy), efficient (resultant velocity is exceedingly fast), environmental protection (discharge of building-up process contamination-free), high-quality (stable components, purity are high).SHS technology is the hi-tech in current synthesis field, and at the end of the eighties in last century, many units of China have carried out the research of this respect.
SHS process in building-up process without the need to external heat source, therefore calculation of thermodynamics focus on discuss its reaction possibility, it is the basis that Combination Process of SHS is discussed, and according to this building-up reactions adiabatic combustion temperature (Tad) that Thermodynamics Formulas directly calculates, again characterize the important parameter of conbustion synthesis, for the theoretical investigation of SHS process and application all significant.To realize the most reliable method of possibility be the adiabatic combustion temperature calculating given mixed system to prediction Combination Process of SHS, and it judges that can combustion synthesis reaction the qualitative foundation of self―sustaining.Self-propagating High-temperature Synthesis Process originator Merzhanov etc. propose some general experience judge methods [" conbustion synthesis " 1999:P.56]: when only having Tad > 1800K, and SHS process reaction could continue to carry out certainly.For the nitrogenize of vanadium metal or vanadium alloy raw material, mainly calculate adiabatic combustion temperature by the reaction of vanadium and nitrogen, the adiabatic combustion temperature of vanadium nitrogen compound building-up reactions is 3500K, even its adiabatic combustion temperature of vanadium iron raw material also proposes the requirement of Tad > 1800K empirical value close to Merzhanov etc.Such as on 09 08th, 2010, Chinese invention patent application publication No. CN101824556A, disclose a kind of method adopting Self-propagating High-temperature Synthesis Process to produce ferrovanadium nitride, raw material is vanadium iron and nitrogen, first raw material vanadium iron is broken in abrasive blast equipment, to be bulked in crucible after vanadium iron raw material drying good for fragmentation, crucible to be placed in high-pressure synthesis device and to be filled with the nitrogen of 6-12MPa, the starting ignition device raw material that ignites carries out building-up reactions, combustion synthesis reaction is from continuing to carry out, the ferrovanadium nitride of conbustion synthesis cools rear taking-up in nitrogen, is broken into block.But nitrogen content is only 9.0 ~ 17.0% in sintetics, there is nitrogen content low (≤17%), the problems such as the foreign matter contents such as carbon sulphur silicon are high, have a strong impact on steel nitrogen increased amount and performance.And the performance such as intensity, toughness, ductility, fatigue resistance that nitrogen content (>=17%) VN alloy more effectively can promote to improve steel compared with common low nitrogen VN alloy and the usage quantity that reduces vanadium further save cost.Reduce when the impurity such as the carbon sulphur silicon in VN alloy then can be reduced in steel-making interpolation VN alloy and bring too much external impurity into, affect the performance of steel.
Summary of the invention
Technical problem to be solved by this invention is: propose a kind of can the technique of the high-purity VN alloy of scale production, by thick level ammonium meta-vanadate directly for vanadium-nitrogen alloy raw material and not with the high price such as vanadium iron vanadium product for raw material, utilize self-propagating low-temperature burning to react self-heat generation and carry out nitrogenize, reaction times is short, energy consumption and cost low, can scale operation; The nitrogen-vanadium alloy height nitrogen produced is high-purity, nitrogen content >=17%.Nitrogen content is better than U.S. VN alloy.
According to requirement of the present invention, the technical solution adopted in the present invention is: a kind of can the technique of the high-purity VN alloy of scale production, utilize SHS technology, with thick level ammonium meta-vanadate for raw material, direct blending powdered carbon, igniting, by NH
4vO
3in NH
4 +promote that nitrogen closes, at high temperature nitriding; Concrete steps are: before reaction, by thick level ammonium meta-vanadate and powdered carbon mixing fully, load one by one in plumbago crucible; These plumbago crucibles become laminated arrangement to put into airtight synthesising container; The starting ignition device raw material that ignites carries out building-up reactions, the high-purity VN alloy of conbustion synthesis; The water vapour produced and carbon monoxide are discharged from the top of airtight synthesising container through vent valve; When vanadium nitrogenizing reaction temperature reaches 1500 DEG C-1520 DEG C; Regulable control vent valve makes the gaseous tension in airtight synthesising container be 2-3Mpa, and combustion synthesis reaction is from continuing to carry out; After reacting completely, high-purity VN alloy is taken out after logical nitrogen cooling in plumbago crucible, is broken into block.
During above-mentioned thick level ammonium meta-vanadate and powdered carbon mix, powdered carbon add-on is the 11%-15% of thick level ammonium meta-vanadate gross weight.
Innovative point of the present invention and beneficial effect are:
The present invention is that the production of high-purity VN alloy provides a kind of selection newly, and the present invention directly utilizes thick level ammonium meta-vanadate for raw material blending powdered carbon, by NH
4vO
3in NH
4 +promote that nitrogen closes, at high temperature nitriding; The synthesis pressure that the present invention utilizes vent valve to control in airtight synthesising container is 2-3Mpa, the H in building-up process in VN alloy
2the discharge of O and CO is limited, and becomes slow, and can not gush out from VN alloy surface same position continuously and form air cleft, therefore the surface crack of the finished product VN alloy of the present invention be few, improves its surface quality, thus improves its quality product.
Compared with CN101824556A technique, the inventive method tool has the following advantages:
1, the present invention is by thick level NH
4vO
3it is directly vanadium-nitrogen alloy raw material and not with V
2o
5be raw material Deng high price vanadium product, raw material sources more easily obtain; Both NH can be utilized
4vO
3in NH
4 +promote that nitrogen closes, save great amount of cost again;
2, in building-up process of the present invention except powdered carbon, help the material of reduction or heating to add without other, greatly can reduce the impurity in product, and three-waste free discharge, quality product is high;
3, the present invention utilize self-propagating low-temperature burning to react self-heat generation can to realize vanadium and nitrogen two material reaction abundant, thus realize the high nitrogen content of alloy, and ensure uniform in quality, stablize.And whole Reactive Synthesis process is without electrically heated and insulation, has saved the energy and operation, be easy to control, apparatus processing and easy for installation.Use self-propagating low-temperature burning new technology that synthesis cycle can also be made less than 50 minutes, be far shorter than the prior art reaction times, greatly enhance productivity, can scale operation;
4, the present invention adopts vent valve to control the synthesis pressure in airtight synthesising container and controls the surperficial air cleft of the finished product VN alloy; Product strength prepared by combustion synthesis process is comparatively large, almost without broken in transportation of materials and use, thus reduces the wastage rate of material;
5, employing combustion synthesis process, synthesizes furnace charge at the beginning of being or final product does not need briquetting.Sintetics is fine and close, than great, can reach 6.5g/cm
3, nitrogen content is evenly distributed, and this product high purity vanadium nitrogen alloy composition is: VN alloy V content>=78%, VN alloy leaded wastewater>=17%, VN alloy C content≤5%, VN alloy S content≤0.1%, VN alloy silicone content≤0.1%.
Embodiment
The present invention is a kind of can the technique of the high-purity VN alloy of scale production:
Can the technique of the high-purity VN alloy of scale production, utilize SHS technology, with thick level ammonium meta-vanadate for raw material, direct blending powdered carbon, igniting, by NH
4vO
3in NH
4 +promote that nitrogen closes, at high temperature nitriding;
NH
4VO
3+C=VN+2H
2O +CO；
Powdered carbon add-on of the present invention is the 11%-15% of thick level ammonium meta-vanadate gross weight; Fully mixing before reaction; Load one by one in plumbago crucible, these plumbago crucibles become laminated arrangement to put into airtight synthesising container, and the starting ignition device raw material that ignites carries out building-up reactions, the high-purity VN alloy of conbustion synthesis; H
2o and CO discharges from the top of airtight synthesising container through vent valve; When vanadium nitrogenizing reaction temperature reaches 1500 DEG C-1520 DEG C; Regulable control vent valve makes the gaseous tension in airtight synthesising container be 2-3Mpa, and combustion synthesis reaction is from continuing to carry out; After reacting completely, high-purity VN alloy is taken out after logical nitrogen cooling in plumbago crucible, is broken into block.
As mentioned above, the invention provides a kind of can the technique of the high-purity VN alloy of scale production, the existing application in accordance with the law proposing patent of invention; But above implementation is one of present pre-ferred embodiments, not limit to the present invention with this, therefore approximate with feature of the present invention etc., identical person such as, all should belong within claim of the present invention.
Claims (2)
1. can the technique of the high-purity VN alloy of scale production, utilize SHS technology, it is characterized in that with thick level ammonium meta-vanadate for raw material, direct blending powdered carbon, igniting, by NH
4vO
3in NH
4 +promote that nitrogen closes, at high temperature nitriding; Concrete steps are: before reaction, by thick level ammonium meta-vanadate and powdered carbon mixing fully, load one by one in plumbago crucible; These plumbago crucibles become laminated arrangement to put into airtight synthesising container; The starting ignition device raw material that ignites carries out building-up reactions, the high-purity VN alloy of conbustion synthesis; The water vapour produced and carbon monoxide are discharged from the top of airtight synthesising container through vent valve; When vanadium nitrogenizing reaction temperature reaches 1500 DEG C-1520 DEG C; Regulable control vent valve makes the gaseous tension in airtight synthesising container be 2-3Mpa, and combustion synthesis reaction is from continuing to carry out; After reacting completely, high-purity VN alloy is taken out after logical nitrogen cooling in plumbago crucible, is broken into block.
2. according to claim 1 a kind of can the technique of the high-purity VN alloy of scale production, it is characterized in that: in described thick level ammonium meta-vanadate and powdered carbon mixing, powdered carbon add-on is the 11%-15% of thick level ammonium meta-vanadate gross weight.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510558364.6A CN105002386B (en) | 2015-09-06 | 2015-09-06 | It is a kind of can the high-purity VN alloy of large-scale production technique |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510558364.6A CN105002386B (en) | 2015-09-06 | 2015-09-06 | It is a kind of can the high-purity VN alloy of large-scale production technique |
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| Publication Number | Publication Date |
|---|---|
| CN105002386A true CN105002386A (en) | 2015-10-28 |
| CN105002386B CN105002386B (en) | 2017-06-16 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857695A (en) * | 1973-06-21 | 1974-12-31 | Int Minerals & Chem Corp | Production of vanadium composition |
| US4562057A (en) * | 1984-03-29 | 1985-12-31 | Union Carbide Corporation | Preparation of low-carbon vanadium nitride |
| CN101172585A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing vanadium nitride |
| CN101225495A (en) * | 2008-01-29 | 2008-07-23 | 刘先松 | Method for producing vanadium-nitrogen alloy |
| CN101787456A (en) * | 2010-03-08 | 2010-07-28 | 南通汉瑞实业有限公司 | Production method of vanadium-nitrogen alloy |
| 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 |
-
2015
- 2015-09-06 CN CN201510558364.6A patent/CN105002386B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3857695A (en) * | 1973-06-21 | 1974-12-31 | Int Minerals & Chem Corp | Production of vanadium composition |
| US4562057A (en) * | 1984-03-29 | 1985-12-31 | Union Carbide Corporation | Preparation of low-carbon vanadium nitride |
| CN101172585A (en) * | 2007-09-30 | 2008-05-07 | 冯良荣 | Method for producing vanadium nitride |
| CN101225495A (en) * | 2008-01-29 | 2008-07-23 | 刘先松 | Method for producing vanadium-nitrogen alloy |
| 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 |
| CN101787456A (en) * | 2010-03-08 | 2010-07-28 | 南通汉瑞实业有限公司 | Production method of vanadium-nitrogen alloy |
Non-Patent Citations (1)
| Title |
|---|
| 王雄等: "微波加热制备氮化钒工艺", 《稀有金属材料与工程》 * |
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