CN102899510A - Production method of high-purity metal vanadium - Google Patents
Production method of high-purity metal vanadium Download PDFInfo
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- CN102899510A CN102899510A CN2012104266293A CN201210426629A CN102899510A CN 102899510 A CN102899510 A CN 102899510A CN 2012104266293 A CN2012104266293 A CN 2012104266293A CN 201210426629 A CN201210426629 A CN 201210426629A CN 102899510 A CN102899510 A CN 102899510A
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Abstract
The invention relates to a production method of high-purity metal vanadium, which comprises the following steps that: vanadium pentoxide as a raw material and Al powder as a reducing agent are smelted by an external furnace method to obtain a vanadium aluminum alloy ingot; the surface of the vanadium aluminum alloy ingot is cleaned and cut into vanadium aluminum alloy strips with uniform shape, and the vanadium aluminum alloy strips are welded into vanadium aluminum alloy rods matched with the size of an electron beam melting furnace feed by argon arc welding; the vanadium aluminum alloy rods are sent to an electron beam melting furnace, the electron beam melting furnace is vacuumized, and the vanadium aluminum alloy rods are bombarded by electron beams, so that the vanadium aluminum alloy rods are melted to flow into a water-cooled crucible to be melted, and a metal vanadium liquid in the water-cooled crucible is cooled and solidified into a metal vanadium ingot. The method has the advantages that: the production period is short, the production capacity is large, the environmental pollution is little, the energy is saved, the production cost is substantially reduced, other impurities are not introduced in the production process, and the product purity can reach 99.5% to 99.9%. The method is suitable for industrial production.
Description
Technical field
The invention belongs to the Metal smelting field, particularly a kind of production method of high purity vanadium metal.
Background technology
High purity vanadium metal is called as metal " VITAMIN ", has that fusing point is high, plasticity good, good ductility, the characteristics such as corrosion-resistant, and purposes is very extensive.Vanadium metal is a kind of alloy addition of excellence, is added in the steel alloy energy refinement crystalline grain of steel, thereby intensity, toughness and the wear resistance of increase steel.In addition, vanadium metal also has good nuclear physics performance, can be as the lapping of nuclear fuel.
At present, fused salt electrolysis process is the main method of producing high purity vanadium metal, and the method is to utilize to contain the vanadium crude metal as soluble anode, by the electrochemistry refining at negative electrode high purity vanadium metal.But fused salt electrolysis process produces that high purity vanadium metal throughput is little, and manually the amount of expending is large, and take the fused salt electrolysis stove of Φ 200 as example, power is under the 15KW, and the output of vanadium metal only has 0.7kg/ days; Need a large amount of electric energy in the whole electrolytic process, energy consumption is high, and production cost is higher, has restricted the Application Areas of vanadium metal; And produce K, Ca, three kinds of abraum salts of Li in the electrolytic process, can pollute environment, need to process.
Summary of the invention
The technical problem to be solved in the present invention provides that a kind of throughput is large, production cost is low, the production method of the high purity vanadium metal of energy-conserving and environment-protective.
Technical solution of the present invention is:
A kind of production method of high purity vanadium metal, its concrete steps are:
1, the preparation of vananum
Take Vanadium Pentoxide in FLAKES as raw material, take the Al powder as reductive agent, the mass ratio of described Vanadium Pentoxide in FLAKES and Al powder is 100:44～100:50, adopts perrin process to smelt, and gets the vananum ingot;
2, the surface treatment of vananum ingot
The vananum ingot surface is cleaned out, be cut into the vananum bar of shape homogeneous, the vananum bar is welded into the vananum rod that is complementary with electron beam melting furnace charging size with argon arc welding;
3, refining
The vananum rod is sent in the electron beam melting furnace, and electron beam melting furnace is evacuated to 3 * 10
-3Pa～6 * 10
-2Pa, cold-crucible in the electron beam melting furnace is carried out water-cooled, temperature maintains 20 ℃～60 ℃, it is 9kV～10kV that high pressure is set, and adopts the electron beam bombardment vananum rod of 1000mA～1500mA, and its melt flow is entered in the cold-crucible, under 3000 ℃～3400 ℃, melting 20min～30min closes electronic beam current in the cold-crucible melting zone, and the vanadium metal liquid cooling in the cold-crucible but is frozen into the vanadium metal ingot.
The content of vanadium of described vananum ingot is 92%～95%.
Described vananum rod length is 600mm～800mm.
During the cleaning of vananum ingot surface, adopt grinder buffing.
The invention has the beneficial effects as follows: the vananum rod enters in the electron beam melting furnace process, beam bombardment is to the vananum rod, make the fusing of vananum rod, in the melting process, lower-boiling impurity (aluminium, iron, the impurity such as chromium) vapor away, vanadium alloy forms stream of liquid droplets and enters cold-crucible, and electron beam continues vanadium alloy heating in the cold-crucible, make that impurity further volatilizees in the cold-crucible melting zone, thereby improved product purity, do not introduced other impurity in the production process, product purity can reach 99.5%～99.9%, the method is with short production cycle, throughput is large, and environmental pollution is little, and the energy save energy, production cost reduces significantly, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is vananum rod schematic diagram of the present invention.
Embodiment
Embodiment 1
1, the preparation of vananum
Get 20kg Vanadium Pentoxide in FLAKES raw material, the agent of 8.8kg aluminum reduction adds in the thermite reaction stove, cuts as priming mixture take magnesium, under 2200 ℃, carries out perrin process and smelts, and reaction finishes, and gets the 10.1kg content of vanadium and be 95% vananum piece;
2, the surface treatment of vananum piece
Adopt grinder buffing that the removing surface of vananum piece is clean, being cut into specification is the vananum bar of 400mm * 60mm * 30mm, the vananum bar is welded into the vananum rod that specification is 600mm * 60mm * 60mm with argon arc welding, as shown in Figure 1;
3, refining
Be that the vananum rod of 600mm * 60mm * 60mm is sent in the electron beam melting furnace with the 7.2kg specification, electron beam melting furnace is evacuated to 6 * 10
-2Pa, cold-crucible in the electron beam melting furnace is carried out water-cooled, water temp maintains 20 ℃, and it is 10kV that high pressure is set, and adopts the electron beam bombardment vananum rod of 1500mA that its melt flow is entered in the cold-crucible, after the fusing, at 3000 ℃ of lower melting 30min, close electronic beam current, the vanadium metal liquid cooling in the cold water crucible but is frozen into the vanadium metal ingot 6.6kg of Φ 60, after testing, the content of vanadium of vanadium metal ingot is 99.5%.
Embodiment 2
1, the preparation of vananum
Get 20kg Vanadium Pentoxide in FLAKES raw material, the agent of 10kg aluminum reduction adds in the thermite reaction stove, cuts as priming mixture take magnesium, under 2200 ℃, carries out perrin process and smelts, and reaction finishes, and gets the 10.6kg content of vanadium and be 92% vananum piece;
2, the surface treatment of vananum piece
Adopt grinder buffing that the removing surface of vananum piece is clean, being cut into specification is the vananum bar of 400mm * 60mm * 30mm, the vananum bar is welded into the vananum rod that specification is 800mm * 60mm * 60mm with argon arc welding, as shown in Figure 1;
3, refining
Be that the vananum rod of 800mm * 60mm * 60mm is sent in the electron beam melting furnace with the 9.6kg specification, electron beam melting furnace is evacuated to 3 * 10
-3Pa, cold-crucible in the electron beam melting furnace is carried out water-cooled, water temp maintains 60 ℃, and it is 9kV that high pressure is set, and adopts the electron beam bombardment vananum rod of 1200mA that its melt flow is entered in the cold-crucible, after the fusing, at 3400 ℃ of lower melting 20min, close electronic beam current, the vanadium metal liquid cooling in the cold water crucible but is frozen into the vanadium metal ingot 8.7kg of Φ 60, after testing, the content of vanadium of vanadium metal ingot is 99.9%.
Embodiment 3
1, the preparation of vananum
Get 20kg Vanadium Pentoxide in FLAKES raw material, the agent of 9.5kg aluminum reduction adds in the thermite reaction stove, cuts as priming mixture take magnesium, under 2200 ℃, carries out perrin process and smelts, and reaction finishes, and gets the 10.3kg content of vanadium and be 93% vananum piece;
2, the surface treatment of vananum piece
Adopt grinder buffing that the removing surface of vananum piece is clean, being cut into specification is the vananum bar of 400mm * 60mm * 30mm, the vananum bar is welded into the vananum rod that specification is 800mm * 60mm * 60mm with argon arc welding, as shown in Figure 1;
3, refining
Be that the vananum rod of 800mm * 60mm * 60mm is sent in the electron beam melting furnace with the 9.3kg specification, electron beam melting furnace is evacuated to 1 * 10
-2Pa, cold-crucible in the electron beam melting furnace is carried out water-cooled, water temp maintains 40 ℃, and it is 10kV that high pressure is set, and adopts the electron beam bombardment vananum rod of 1000mA that its melt flow is entered in the cold-crucible, after the fusing, at 3200 ℃ of lower melting 25min, close electronic beam current, the vanadium metal liquid cooling in the cold water crucible but is frozen into the vanadium metal ingot 8.3kg of Φ 60, after testing, the content of vanadium of vanadium metal ingot is 99.7%.
Claims (4)
1. the production method of a high purity vanadium metal is characterized in that concrete steps are:
1.1, the preparation of vananum
Take Vanadium Pentoxide in FLAKES as raw material, take the Al powder as reductive agent, the mass ratio of described Vanadium Pentoxide in FLAKES and Al powder is 100:44～100:50, adopts perrin process to smelt, and gets the vananum ingot;
1.2, the surface treatment of vananum ingot
The vananum ingot surface is cleaned out, be cut into the vananum bar of shape homogeneous, the vananum bar is welded into the vananum rod that is complementary with electron beam melting furnace charging size with argon arc welding;
1.3, refining
The vananum rod is sent in the electron beam melting furnace, and electron beam melting furnace is evacuated to 3 * 10
-3Pa～6 * 10
-2Pa, cold-crucible in the electron beam melting furnace is carried out water-cooled, temperature maintains 20 ℃～60 ℃, it is 9kV～10kV that high pressure is set, and adopts the electron beam bombardment vananum rod of 1000mA～1500mA, and its melt flow is entered in the cold-crucible, under 3000 ℃～3400 ℃, melting 20min～30min closes electronic beam current in the cold-crucible melting zone, and the vanadium metal liquid cooling in the cold-crucible but is frozen into the vanadium metal ingot.
2. the production method of high purity vanadium metal according to claim 1, it is characterized in that: the content of vanadium of described vananum ingot is 92%～95%.
3. the production method of high purity vanadium metal according to claim 1 is characterized in that: described vananum rod length is 600mm～800mm.
4. the production method of high purity vanadium metal according to claim 1 is characterized in that: during the cleaning of vananum ingot surface, adopt grinder buffing.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103667746A (en) * | 2013-11-04 | 2014-03-26 | 宝鸡市嘉诚稀有金属材料有限公司 | Preparation method of pure vanadium ingot |
| CN104894388A (en) * | 2014-03-06 | 2015-09-09 | 北京工业大学 | Method for preparing vanadium target material through electron beam melting |
| CN107267831A (en) * | 2017-07-04 | 2017-10-20 | 中国工程物理研究院材料研究所 | A kind of high-purity vanadium-silicon alloy and preparation method thereof |
| CN109277429A (en) * | 2018-09-03 | 2019-01-29 | 重庆材料研究院有限公司 | The preparation method of high purity vanadium silk |
| CN110923476A (en) * | 2019-10-30 | 2020-03-27 | 中色（宁夏）东方集团有限公司 | Method for producing high-purity metal vanadium ingot by three-step method |
| CN111644631A (en) * | 2020-06-10 | 2020-09-11 | 重庆材料研究院有限公司 | Preparation method of spherical vanadium powder |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906546A (en) * | 2010-07-14 | 2010-12-08 | 承德天大钒业有限责任公司 | Method for preparing vanadium-aluminum alloy |
| CN102031402A (en) * | 2011-01-06 | 2011-04-27 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of vanadium-aluminum alloy |
| CN102154569A (en) * | 2011-03-18 | 2011-08-17 | 攀钢集团钢铁钒钛股份有限公司 | Vanalium preparation method |
| CN102181640A (en) * | 2011-04-15 | 2011-09-14 | 攀钢集团钢铁钒钛股份有限公司 | Production method of vanadium-aluminium alloy |
| CN102367568A (en) * | 2011-10-20 | 2012-03-07 | 宁波江丰电子材料有限公司 | Preparation method of high-purity tantalum target material |
| CN102534271A (en) * | 2012-02-21 | 2012-07-04 | 四川省达州钢铁集团有限责任公司 | Production method of vanadium-aluminum alloy |
| CN102586637A (en) * | 2012-03-23 | 2012-07-18 | 宁夏东方钽业股份有限公司 | Method for manufacturing multi-component niobium alloy cast ingot |
| CN102660705A (en) * | 2012-04-06 | 2012-09-12 | 宁夏东方钽业股份有限公司 | High-Zr content Nb alloy and melt casting manufacturing method thereof |
-
2012
- 2012-10-31 CN CN2012104266293A patent/CN102899510A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101906546A (en) * | 2010-07-14 | 2010-12-08 | 承德天大钒业有限责任公司 | Method for preparing vanadium-aluminum alloy |
| CN102031402A (en) * | 2011-01-06 | 2011-04-27 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of vanadium-aluminum alloy |
| CN102154569A (en) * | 2011-03-18 | 2011-08-17 | 攀钢集团钢铁钒钛股份有限公司 | Vanalium preparation method |
| CN102181640A (en) * | 2011-04-15 | 2011-09-14 | 攀钢集团钢铁钒钛股份有限公司 | Production method of vanadium-aluminium alloy |
| CN102367568A (en) * | 2011-10-20 | 2012-03-07 | 宁波江丰电子材料有限公司 | Preparation method of high-purity tantalum target material |
| CN102534271A (en) * | 2012-02-21 | 2012-07-04 | 四川省达州钢铁集团有限责任公司 | Production method of vanadium-aluminum alloy |
| CN102586637A (en) * | 2012-03-23 | 2012-07-18 | 宁夏东方钽业股份有限公司 | Method for manufacturing multi-component niobium alloy cast ingot |
| CN102660705A (en) * | 2012-04-06 | 2012-09-12 | 宁夏东方钽业股份有限公司 | High-Zr content Nb alloy and melt casting manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 彭予民: "电子束冷床炉熔炼制备高纯金属钒铸锭", 《宝钢技术》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103667746A (en) * | 2013-11-04 | 2014-03-26 | 宝鸡市嘉诚稀有金属材料有限公司 | Preparation method of pure vanadium ingot |
| CN103667746B (en) * | 2013-11-04 | 2014-10-22 | 宝鸡市嘉诚稀有金属材料有限公司 | Preparation method of pure vanadium ingot |
| CN104894388A (en) * | 2014-03-06 | 2015-09-09 | 北京工业大学 | Method for preparing vanadium target material through electron beam melting |
| CN107267831A (en) * | 2017-07-04 | 2017-10-20 | 中国工程物理研究院材料研究所 | A kind of high-purity vanadium-silicon alloy and preparation method thereof |
| CN109277429A (en) * | 2018-09-03 | 2019-01-29 | 重庆材料研究院有限公司 | The preparation method of high purity vanadium silk |
| CN109277429B (en) * | 2018-09-03 | 2020-01-10 | 重庆材料研究院有限公司 | Preparation method of high-purity vanadium wire |
| CN110923476A (en) * | 2019-10-30 | 2020-03-27 | 中色（宁夏）东方集团有限公司 | Method for producing high-purity metal vanadium ingot by three-step method |
| CN111644631A (en) * | 2020-06-10 | 2020-09-11 | 重庆材料研究院有限公司 | Preparation method of spherical vanadium powder |
| CN111644631B (en) * | 2020-06-10 | 2023-04-18 | 重庆材料研究院有限公司 | Preparation method of spherical vanadium powder |
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Application publication date: 20130130 |