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Method for preparing vanadium tetrachloride from ferrovanadium fine powder

A technology of vanadium tetrachloride and crude vanadium tetrachloride, applied in vanadium halide and other directions, can solve the problems of low purity of vanadium tetrachloride, lack of recycling process of vanadium ferroalloy fine powder, etc., and achieves mild conditions, easy operation, The effect of broad application prospects

Pending Publication Date: 2022-04-15
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the problem that the purity of vanadium tetrachloride prepared by the existing method in the prior art is not high and that a large amount of vanadium-iron alloy fine powder produced in the crushing process of the vanadium-iron alloy lacks an effective recycling process, and provides a method for using Method for preparing vanadium tetrachloride from ferrovanadium fine powder

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) 400g petroleum coke is mixed with 100g vanadium iron alloy fine powder, wherein, the vanadium content in the vanadium iron fine powder is 85%, Fe content is 10%, other is impurity Fe, Si, Ti and Al, petroleum coke The purity is 99.5%, the average particle size of ferrovanadium fine powder is 0.5mm, and the average particle size of petroleum coke is 0.1mm;

[0051] (2) Spread vanadium-iron alloy fine powder and petroleum coke mixture uniformly in the corundum crucible of the upper opening cuboid shape, the thickness of the mixture is 1mm, and the distance between the upper surface of the mixture and the upper edge of the crucible wall is 5mm; The corundum crucible containing the mixture is placed in a cylindrical quartz reactor (reactor diameter 80 mm), one end of the quartz reactor is connected to an air inlet, and the other end is an air outlet, and the air outlet is connected to a condenser , and then the quartz reactor is placed in a horizontal tubular heating fu...

Embodiment 2

[0056] (1) 600g petroleum coke is mixed with 100g vanadium iron alloy fine powder, wherein, the vanadium content in the vanadium iron fine powder is 75%, Fe content is 20%, other is impurity Fe, Si, Ti and Al, petroleum coke The purity is 99.5%, the average particle size of ferrovanadium fine powder is 1.2mm, and the average particle size of petroleum coke is 0.5mm;

[0057] (2) Spread vanadium-iron alloy fine powder and petroleum coke mixture uniformly in the corundum crucible of the upper opening cuboid shape, the thickness of the mixture is 1.7mm, and the distance between the upper surface of the mixture and the upper edge of the crucible wall is 4mm; The corundum crucible containing the mixture is placed in a cylindrical quartz reactor (reactor diameter 80 mm), one end of the quartz reactor is connected to an air inlet, and the other end is an air outlet, and the air outlet is connected to a condenser , and then the quartz reactor is placed in a horizontal tubular heating ...

Embodiment 3

[0062] (1) 900g petroleum coke is mixed with 90g vanadium iron alloy fine powder, wherein, the vanadium content in the vanadium iron fine powder is 45%, Fe content is 50%, other is impurity Fe, Si, Ti and Al, petroleum coke The purity is 99.5%, the average particle size of ferrovanadium fine powder is 2.0mm, and the average particle size of petroleum coke is 1.0mm;

[0063](2) Spread vanadium-iron alloy fine powder and petroleum coke mixture uniformly in the corundum crucible of upper opening cuboid shape, the thickness of mixture is 5mm, and the distance between the upper surface of mixture and the upper edge of crucible wall is 1mm; The corundum crucible containing the mixture is placed in a cylindrical quartz reactor (reactor diameter 80 mm), one end of the quartz reactor is connected to an air inlet, and the other end is an air outlet, and the air outlet is connected to a condenser , and then the quartz reactor is placed in a horizontal tubular heating furnace, and a mixed...

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Abstract

The invention relates to the technical field of chemical metallurgy, and discloses a method for preparing vanadium tetrachloride from ferrovanadium fine powder. The method comprises the following steps: (1) paving ferrovanadium fine powder and petroleum coke in a crucible, wherein the mass ratio of the ferrovanadium fine powder to the petroleum coke is 1: (4-10); (2) putting the corundum crucible into a quartz reactor, then putting the quartz reactor into a heating furnace, introducing chlorine and nitrogen to perform chlorination reaction, and condensing and centrifugally separating a gas product to obtain crude vanadium tetrachloride; (3) putting the crude vanadium tetrachloride product into a polytetrafluoroethylene distillation-condensation device, adding distilled water, and stirring for reaction; and (4) primary distillation is carried out at 130-140 DEG C, secondary distillation is carried out at 150-160 DEG C when the mass of a condensation product is 5-10% of the mass of the crude vanadium tetrachloride product, and the condensation product is the vanadium tetrachloride product when the mass of the condensation product is 50-75% of the mass of the crude vanadium tetrachloride product. The method is simple, the impurity removal efficiency is high, and the product purity is high.

Description

technical field [0001] The invention relates to the technical field of chemical metallurgy, in particular to a method for preparing vanadium tetrachloride by using ferrovanadium fine powder. Background technique [0002] Vanadium tetrachloride (VCl 4 ) is an important class of chemical products, widely used in organic synthesis, and is an important catalyst in the rubber industry. In addition, vanadium tetrachloride is also an important raw material for the preparation of metal vanadium and other vanadium compounds. Among them, using vanadium tetrachloride as a raw material, high-purity metal vanadium can be prepared by metallothermic reduction-distillation. Usually, it is necessary to use metal vanadium or vanadium-nitrogen alloy as a raw material to prepare vanadium tetrachloride by chlorination. This type of method is expensive, and in the chlorination process, impurities in the raw material are easily chlorinated and decomposed simultaneously. Entering vanadium tetrach...

Claims

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Application Information

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IPC IPC(8): C01G31/04
Inventor 杜光超汪劲鹏饶玉忠王仕伟范川林朱庆山
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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