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Method for producing high-purity metal vanadium by directional solidification

A directional solidification and directional solidification furnace technology, applied in the field of vanadium metal smelting, can solve the problems of high energy consumption, high cost, and expensive calcium cost, and achieve the effects of improving production efficiency, reducing reaction temperature, and reducing energy consumption

Active Publication Date: 2020-12-25
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the standard free enthalpy of formation of lithium and beryllium oxides is very low, the preparation of metal lithium and beryllium is relatively difficult, and the cost of using them as metal reducing agents will be quite high
Silicon is not an ideal reducing agent in most cases because of its strong tendency to form stable metal silicides, and the problem of silicon removal is not easy to solve
Due to the high melting point of magnesium oxide, the heat released by the reaction of magnesium and metal oxides is generally not sufficient to form a solid metal; at the same time, since magnesium boils at a lower temperature than calcium and aluminum, airtight containers must be used to prevent magnesium from boiling. The loss of the magnesia thermal reduction method is even more limited.
Compared with the aluminothermic reduction method, the calcithermal reduction method is no longer dominant. There are two main reasons: first, the reaction needs to be carried out in a closed container, and there are inherent limitations in expanding the scale; second, compared with aluminum , the cost of calcium in its pure state is more expensive
The production of pure metal vanadium by the thermite method generally firstly reduces the vanadium oxide to produce vanadium-aluminum alloy. The reduction reaction can be carried out in an open heat-resistant container, and then the vanadium-aluminum alloy is subjected to high-temperature vacuum removal of aluminum and electron beam smelting. Remove other residual impurities to obtain pure metal vanadium, but the process of vacuum dealumination requires a lot of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Select V 2 o 5 20g is vanadium raw material, Mg 4 al 3 Silk is a reducing agent.

[0029] (2) First set V 2 o 5 Put it into a graphite crucible, and put the crucible into an induction heating furnace.

[0030] (3) Argon gas was introduced as a protective atmosphere, and the temperature was raised to 800°C.

[0031] (4) Wait until V 2 o 5 After the melting is complete, magnesium-aluminum alloy wire is fed at 0.43 cm / min to start directional solidification at a rate of 10 mm / h, and the diameter of the alloy cylindrical billet obtained after the solidification is 24 mm.

[0032] (5) After 3 hours, stop feeding the wire, and then stop heating.

[0033] (6) After the sample is cooled to room temperature, cut it in half along the longitudinal centerline, and observe the height of vanadium at the bottom through the color.

[0034] (7) Cut the sample transversely along the height in (6) to separate the vanadium-containing part.

[0035](8) Crush the separated me...

Embodiment 2

[0038] (1) Select V 2 o 5 20g is vanadium raw material, Mg 4 Al 3 Silk is a reducing agent.

[0039] (2) First set V 2 o 5 Put into the crucible, then put the crucible into the induction heating furnace.

[0040] (3) Argon gas was introduced as a protective atmosphere, and the temperature was raised to 750°C.

[0041] (4) Wait until V 2 o 5 After the melting is complete, magnesium-aluminum alloy wire is fed at 0.43 cm / min to start directional solidification at a rate of 10 mm / h, and the diameter of the alloy cylindrical billet obtained after the solidification is 24 mm.

[0042] (5) After 3 hours, stop feeding the wire, and then stop heating.

[0043] (6) After the sample is cooled to room temperature, cut it in half along the longitudinal centerline, and observe the height of vanadium at the bottom through the color.

[0044] (7) Cut the sample transversely along the height in (6) to separate the vanadium-containing part.

[0045] (8) Break the separated metal int...

Embodiment 3

[0048] (1) Select V 2 o 5 20g is vanadium raw material, Mg 4 Al 3 Silk is a reducing agent.

[0049] (2) First set V 2 o 5 Put into the crucible, then put the crucible into the induction heating furnace.

[0050] (3) Argon gas was introduced as a protective atmosphere, and the temperature was raised to 700°C.

[0051] (4) Wait until V 2 o 5 After the melting is complete, magnesium-aluminum alloy wire is fed at 0.43 cm / min to start directional solidification at a rate of 10 mm / h, and the diameter of the alloy cylindrical billet obtained after the solidification is 24 mm.

[0052] (5) After 3 hours, stop feeding the wire, and then stop heating.

[0053] (6) After the sample is cooled to room temperature, cut it in half along the longitudinal centerline, and observe the height of vanadium at the bottom through the color.

[0054] (7) Cut the sample transversely along the height in (6) to separate the vanadium-containing part.

[0055] (8) Break the separated metal int...

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Abstract

The invention discloses a method for producing high-purity vanadium metal by directional solidification, and belongs to the technical field of vanadium metal smelting. The method comprises the following steps of heating a directional solidification furnace to 700-800 DEG C, and adding vanadium oxide for melting; after vanadium oxide is melted completely, feeding a magnesium aluminum alloy wire, and starting directional solidification; after vanadium oxide reacts completely, stopping wire feeding and heating; after a sample is cooled to room temperature, conducting separation to obtain crude vanadium; and after the crude vanadium is broken, leaching with dilute hydrochloric acid, and obtaining high-purity vanadium metal. The method takes vanadium oxide as a raw material and magnesium aluminum alloy Mg4Al3 as a reducing agent, so the reaction temperature is reduced, and energy consumption is reduced significantly. Moreover, the production and separation processes take place simultaneously, so the working procedure is reduced, and the production efficiency is improved. The purity of the prepared vanadium metal is higher than 98%.

Description

technical field [0001] The invention belongs to the technical field of vanadium metal smelting, and in particular relates to a method for producing high-purity metal vanadium by directional solidification. Background technique [0002] Vanadium is a silver-gray shiny metal with a density of 6.1g / cm 3 , with a melting point of 1890°C and a boiling point of 3000°C. Its total content in the earth’s crust ranks 22nd among metals. It is a rare metal with a high melting point. It mainly coexists with some other metal ores. No independent vanadium ore has been found so far. As a very valuable strategic resource, vanadium is widely used in automobiles, aerospace, railways, bridges, fusion reactor vessels and other fields. [0003] At present, the production methods of metal vanadium mainly include: vacuum carbothermal reduction method, silicon thermal reduction method, thermal decomposition method of vanadium nitride, stepwise reduction method, metal thermal reduction method, etc. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B34/22C22B5/04C22B3/10
CPCC22B3/10C22B5/04C22B34/22Y02P10/20
Inventor 顾武安韩子柯吕学伟王烨潘成钟大鹏
Owner SICHUAN UNIV