CN103388096A - Vanadium-nitrogen alloy production method - Google Patents
Vanadium-nitrogen alloy production method Download PDFInfo
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- CN103388096A CN103388096A CN2012101400110A CN201210140011A CN103388096A CN 103388096 A CN103388096 A CN 103388096A CN 2012101400110 A CN2012101400110 A CN 2012101400110A CN 201210140011 A CN201210140011 A CN 201210140011A CN 103388096 A CN103388096 A CN 103388096A
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- vanadium pentoxide
- vanadium
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- flakes
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 229910001199 N alloy Inorganic materials 0.000 title abstract description 4
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title abstract description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 14
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 14
- 239000004571 lime Substances 0.000 claims abstract description 14
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000010926 purge Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 19
- 239000000956 alloy Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000011230 binding agent Substances 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000005255 carburizing Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 abstract description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000009865 steel metallurgy Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- QCJQWJKKTGJDCM-UHFFFAOYSA-N [P].[S] Chemical compound [P].[S] QCJQWJKKTGJDCM-UHFFFAOYSA-N 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- JNVCSEDACVAATK-UHFFFAOYSA-L [Ca+2].[S-]SSS[S-] Chemical compound [Ca+2].[S-]SSS[S-] JNVCSEDACVAATK-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009851 ferrous metallurgy Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229940051851 sulfurated lime Drugs 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention belongs to a vanadium-nitrogen alloy production method, and belongs to a steel metallurgy technical field. According to the method, lime, ammonium nitrate and an ethylene glycol solution are added into finely grinded vanadium pentoxide powder; carbon dioxide is used for purging and drying the surfaces of spherical substances prepared after the materials are uniformly mixed. The method comprises the specific steps of (1) grinding, (2) mixing, (3) drying, (4) reaction, and (5) cooling. With the method, vanadium-nitrogen alloy production energy consumption is greatly reduced, and sulfur and phosphorous impurities in raw materials can be effectively removed. The method has the characteristics of high vanadium utilization rate and low energy consumption.
Description
Technical field
The invention belongs to technical field of ferrous metallurgy, relate to a kind of production method of VN alloy of steel-making additive.
Background technology
VN alloy is a kind of steel-making additive, VN alloy is added the mechanical propertys such as intensity, toughness, ductility and thermal fatigue resistance that can improve steel in steel to, simultaneously can give steel good solderability, so Iron and Steel Production increase day by day to the demand of high-quality VN alloy.At present, report about vanadium nitrogen alloy preparation method is a lot, such as vacuum method, normal pressure nitriding etc., and produce the higher level that all reached, but all there are the problems such as output is lower, quality is unstable in it,, in order to improve the Quality and yield of VN alloy, be badly in need of a kind of production method of VN alloy of high-quality economy in industry.
Chinese patent CN101289713A discloses a kind of production method of VN alloy, be Vanadium Pentoxide in FLAKES is levigate after, make globe after adding iron powder, carbon dust, binding agent to mix, globe is delivered to horizontal pushed bat kiln, pass into nitrogen in pushed bat kiln, keep pressure-fired in kiln, carry out carbonization and nitrogenizing reaction, carbonation reaction temperature is 1350-1500 ℃, reaction times 2-3.5 hour, nitriding temperature is 1000-1150 ℃, and reaction times 0.5-1.5 hour progressively is cooled to below 100 ℃ and comes out of the stove.Vacuum unit is not used in this invention, simplified flow process, reduced facility investment, but carbonization and nitrogenizing reaction temperature requirement are high, power consumption is large, generally can contain simultaneously the impurity such as sulphur phosphorus in iron powder, well-known, the sulphur phosphorus impurities can increase iron and steel fragility, destroy the performances such as ductility, toughness, affected the VN alloy quality, the utilization ratio of this invention vanadium is lower, and production cost is high.
Summary of the invention
The invention provides a kind of production method of VN alloy, the vanadium utilization ratio that exists with the solution prior art is low, power consumption is large and can't go deimpurity problem.
The technical solution adopted for the present invention to solve the technical problems is to add lime, ammonium nitrate and aqueous glycol solution in levigate vanadium pentoxide powder, use carbon dioxide to purge the spherical surface of making after mixing dry, its concrete steps are as follows:
(1) levigate: as in ball mill, the raw material Vanadium Pentoxide in FLAKES to be finely ground to powder;
(2) batch mixing: add carbon dust, lime, reaction promotor ammonium nitrate in the vanadium pentoxide powder that obtains to step (1), after stirring, add again the binding agent aqueous glycol solution, make globe, wherein the carbon dust add-on is the 19-25% of Vanadium Pentoxide in FLAKES quality, lime adding amount is the 0.5-2% of Vanadium Pentoxide in FLAKES quality, the ammonium nitrate add-on is the 2-5% of Vanadium Pentoxide in FLAKES quality, binding agent is the aqueous glycol solution that contains 3-5%, and the binding agent add-on is the 13-19% of Vanadium Pentoxide in FLAKES quality;
(3) drying: the spherical surface of making to step (2) purges carbon dioxide, and carbon dioxide gas pressure is controlled in 2kgf, and flow control is at 2Nm
3/ h, purge time were controlled in 1 hour;
(4) reaction: globe is delivered in the baking oven that is full of nitrogen and carried out carburizing reagent, the about 600-800 ℃ of carbonation reaction temperature, be incubated about 4 hours; Then globe is gone in rotary kiln and carry out nitrogenizing reaction, the nitrogenizing reaction temperature is controlled at 500-600 ℃, and passes into nitrogen continuously in kiln, keeps pressure-fired, about 6 hours of time in kiln;
(5) cooling discharging: be cooled in 100 ℃, obtain the finished product VN alloy.
The volumetric concentration of the carbon dioxide that passes in above-mentioned drying step is 99.99%.
The preferred 720 ℃ of left and right of carbonation reaction temperature in above-mentioned reactions steps; The preferred 560 ℃ of left and right of nitrogenizing reaction temperature.
By add lime in Vanadium Pentoxide in FLAKES, lime is that sulphur phosphorus removes agent, lime is calcium oxide, calcium oxide can with nickel powder in sulphur and phosphoric reaction, calcium oxide and phosphorus reaction generate calcium phosphate, calcium oxide and reaction of Salmon-Saxl generate sulfurated lime, can effectively the sulphur phosphorus impurities that contains in various raw materials be removed; Ammonium nitrate is reaction promotor, and ammonium nitrate can form complex compound with carbon or vanadium, accelerates carbonization and the nitrogenizing reaction of Vanadium Pentoxide in FLAKES, and carbonization and nitrogenizing reaction are carried out at lower temperature; Aqueous glycol solution can make the meals such as Vanadium Pentoxide in FLAKES, carbon dust effectively bonding.
Compared with prior art, beneficial effect of the present invention is:
By adding desulfurization phosphorus agent lime, reaction promotor ammonium nitrate and tackiness agent aqueous glycol solution, reaction is carried out at lower temperature, the power consumption of VN alloy production process reduces greatly; Sulphur phosphorus in desulfurization phosphorus agent lime white raw material removes, and has improved the final product quality of VN alloy; This processing method has improved the vanadium utilization ratio, can reach more than 70%.
Embodiment
The present invention is further described below in conjunction with specific embodiment.
(1) levigate: as in ball mill, the raw material Vanadium Pentoxide in FLAKES to be finely ground to powder;
(2) batch mixing: add carbon dust, lime, reaction promotor ammonium nitrate in the vanadium pentoxide powder that obtains to step (1), after stirring, add again the binding agent aqueous glycol solution, make globe, the carbon dust add-on is 21% of Vanadium Pentoxide in FLAKES quality, and lime adding amount is 1% of Vanadium Pentoxide in FLAKES quality, and the ammonium nitrate add-on is 3% of Vanadium Pentoxide in FLAKES quality, binding agent is to contain 4% aqueous glycol solution, and the binding agent add-on is 15% of Vanadium Pentoxide in FLAKES quality;
(3) drying: the carbon dioxide of the spherical surface purge volume concentration 99.99% of making to step (2), carbon dioxide gas pressure is controlled at 1kgf, and flow control is at 2Nm
3/ h, purge time are 45 minutes;
(4) reaction: globe is delivered in the baking oven that is full of nitrogen and carried out carburizing reagent, about 720 ℃ of temperature of reaction, be incubated about 4 hours; Then globe is gone in rotary kiln and carry out nitrogenizing reaction, temperature of reaction is controlled at 560 ℃, and passes into nitrogen continuously in kiln, keeps pressure-fired, about 6 hours of time in kiln;
(5) cooling discharging: be cooled in 100 ℃, obtain the finished product VN alloy.
Finished product VN alloy apparent density is 3.2g/cm
3, content of vanadium is 77.4%, and nitrogen content is 16.8%, and the vanadium utilization ratio reaches 72%.
Claims (3)
1. the production method of a VN alloy, is characterized in that adding lime, ammonium nitrate and aqueous glycol solution in levigate vanadium pentoxide powder, uses carbon dioxide to purge the spherical surface of making after mixing dry, and its concrete steps are as follows:
(1) levigate: as in ball mill, the raw material Vanadium Pentoxide in FLAKES to be finely ground to powder;
(2) batch mixing: add carbon dust, lime, reaction promotor ammonium nitrate in the vanadium pentoxide powder that obtains to step (1), after stirring, add again the binding agent aqueous glycol solution, make globe, wherein the carbon dust add-on is the 19-25% of Vanadium Pentoxide in FLAKES quality, lime adding amount is the 0.5-2% of Vanadium Pentoxide in FLAKES quality, the ammonium nitrate add-on is the 2-5% of Vanadium Pentoxide in FLAKES quality, binding agent is the aqueous glycol solution that contains 3-5%, and the binding agent add-on is the 13-19% of Vanadium Pentoxide in FLAKES quality;
(3) drying: the spherical surface of making to step (2) purges carbon dioxide, and carbon dioxide gas pressure is controlled in 2kgf, and flow control is at 2Nm
3/ h, purge time were controlled in 1 hour;
(4) reaction: globe is delivered in the baking oven that is full of nitrogen and carried out carburizing reagent, the about 600-800 ℃ of temperature, be incubated about 4 hours; Then globe is gone in rotary kiln and carry out nitrogenizing reaction, temperature is controlled at 500-600 ℃, and passes into nitrogen continuously in kiln, keeps pressure-fired, about 6 hours of time in kiln;
(5) cooling discharging: be cooled in 100 ℃, obtain the finished product VN alloy.
2. the production method of VN alloy according to claim 1, the volumetric concentration that it is characterized in that the carbon dioxide that passes in drying step is 99.99%.
3. the production method of VN alloy according to claim 1, is characterized in that in reactions steps that carbonation reaction temperature is 720 ℃ of left and right; The nitrogenizing reaction temperature is 560 ℃ of left and right.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101400110A CN103388096A (en) | 2012-05-07 | 2012-05-07 | Vanadium-nitrogen alloy production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101400110A CN103388096A (en) | 2012-05-07 | 2012-05-07 | Vanadium-nitrogen alloy production method |
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| Publication Number | Publication Date |
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| CN103388096A true CN103388096A (en) | 2013-11-13 |
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| CN2012101400110A Pending CN103388096A (en) | 2012-05-07 | 2012-05-07 | Vanadium-nitrogen alloy production method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532034A (en) * | 2015-01-05 | 2015-04-22 | 南通汉瑞新材料科技有限公司 | Preparation method for low-oxygen vanadium-nitrogen alloy |
| CN111101051A (en) * | 2019-11-05 | 2020-05-05 | 河钢股份有限公司承德分公司 | Method for improving nitrogen content in vanadium-nitrogen alloy production process |
| CN113430402A (en) * | 2021-06-07 | 2021-09-24 | 湖南众鑫新材料科技股份有限公司 | Raw material forming method in vanadium-nitrogen alloy production process |
| CN113718120A (en) * | 2021-08-22 | 2021-11-30 | 湖南众鑫新材料科技股份有限公司 | Process for synthesizing vanadium nitride from nitrogen and vanadium |
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| CN101603132A (en) * | 2009-07-16 | 2009-12-16 | 钢铁研究总院 | A kind of method and apparatus of production VN alloy |
| CN101693975A (en) * | 2009-10-28 | 2010-04-14 | 攀钢集团攀枝花钢钒有限公司 | Method for increasing nitrogen content of vanadium-nitrogen alloy |
| CN102168191A (en) * | 2011-04-12 | 2011-08-31 | 浙江欣万飞科技有限公司 | Vanadium-nitrogen alloy preparation method for preventing fired alloy from being adhered and oxidized |
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2012
- 2012-05-07 CN CN2012101400110A patent/CN103388096A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| US5676775A (en) * | 1993-01-18 | 1997-10-14 | Cacace; Antonino Giorgio | Process for manufacturing corrosion resistant metal products |
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| CN101603132A (en) * | 2009-07-16 | 2009-12-16 | 钢铁研究总院 | A kind of method and apparatus of production VN alloy |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104532034A (en) * | 2015-01-05 | 2015-04-22 | 南通汉瑞新材料科技有限公司 | Preparation method for low-oxygen vanadium-nitrogen alloy |
| CN111101051A (en) * | 2019-11-05 | 2020-05-05 | 河钢股份有限公司承德分公司 | Method for improving nitrogen content in vanadium-nitrogen alloy production process |
| CN111101051B (en) * | 2019-11-05 | 2021-09-10 | 河钢股份有限公司承德分公司 | Method for improving nitrogen content in vanadium-nitrogen alloy production process |
| CN113430402A (en) * | 2021-06-07 | 2021-09-24 | 湖南众鑫新材料科技股份有限公司 | Raw material forming method in vanadium-nitrogen alloy production process |
| CN113430402B (en) * | 2021-06-07 | 2022-02-01 | 湖南众鑫新材料科技股份有限公司 | Raw material forming method in vanadium-nitrogen alloy production process |
| CN113718120A (en) * | 2021-08-22 | 2021-11-30 | 湖南众鑫新材料科技股份有限公司 | Process for synthesizing vanadium nitride from nitrogen and vanadium |
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