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Method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder

A technology for high-purity vanadium oxytrichloride and crude vanadium trichloride, which is applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of affecting the production efficiency and economy of the ferrovanadium smelting system, reducing the process feasibility, Increase the preparation cost and other issues, achieve the effect of improving chlorination efficiency, realizing recycling, and increasing added value

Inactive Publication Date: 2020-07-14
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

The raw material for preparing vanadyl trichloride is usually vanadium oxide or vanadium-containing minerals, but the crude vanadyl trichloride prepared from the above-mentioned materials usually needs to go through a complex rectification and impurity removal process to prepare high-purity vanadium trichloride. Not only increases the preparation cost, but also reduces the process feasibility to a certain extent
[0003] During the ferro-vanadium smelting process, after the prepared ferrosanadium alloy is cooled and dismantled, the alloy cake needs to be crushed. During the crushing process, a large amount of ferrovanadium debris is produced. Because its particle size is usually small, it cannot meet the requirements of the ferrovanadium product particle size. diameter standard, so this part of vanadium-iron alloy debris can only be reused by returning to the furnace and remelting, which not only consumes high energy and increases the cost; at the same time, in the process of returning to the furnace and feeding materials, some ultra-fine ) vanadium-iron alloy fine powder is easy to be sucked into the dust removal system, which caused the loss of vanadium to a certain extent
Therefore, how to fully and effectively utilize this part of ferrovanadium fine powder will affect the production efficiency and economy of the ferrovanadium smelting system
At present, there are few reports on the recycling of vanadium-iron alloy fine powder

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put 500g of ferrovanadium fine powder in a corundum crucible, the particle size of ferrovanadium fine powder is 5μm~200μm, and the vanadium content is 40%, put the crucible in a quartz chlorination reactor, and pass 0.01m / s nitrogen, then place the reactor in a tube furnace to heat up; when the furnace temperature reaches and remains constant at 600°C, readjust the nitrogen flow in the reactor, and feed chlorine and oxygen into the reactor to make the reactor The total gas velocity of nitrogen, chlorine and oxygen in the interior is maintained at 0.02m / s, the molar ratio of chlorine to oxygen is 2:1, and the volume fraction of chlorine in the mixed gas (chlorine, nitrogen and oxygen) is 50%; the chlorination reaction During the process, the volatilized components in the chlorination reactor were condensed and collected to obtain the crude product of vanadyl trichloride, and the tail gas was absorbed and purified by 30% aqueous sodium hydroxide solution; after 120 minute...

Embodiment 2

[0033] Put 200g of vanadium-iron fine powder in a corundum crucible, the particle size of the vanadium-iron alloy fine powder is 5 μm to 200 μm, and the vanadium content is 85%, and the crucible is placed in a quartz chlorination reactor, and 0.03m / s of nitrogen, and then place the reactor in a tube furnace to raise the temperature; when the furnace temperature reaches and remains constant at 300°C, readjust the flow rate of nitrogen in the reactor, and feed chlorine and oxygen into the reactor to make the reactor The total gas velocity of nitrogen, chlorine and oxygen in the interior is maintained at 0.05m / s, the molar ratio of chlorine to oxygen is 3:1, and the volume fraction of chlorine in the mixed gas (chlorine, nitrogen and oxygen) is 30%; the chlorination reaction During the process, the volatilized components in the chlorination reactor are condensed and collected to obtain the crude product of vanadyl trichloride, and the tail gas is absorbed and purified by 30% aque...

Embodiment 3

[0035]Put 300g of vanadium-iron fine powder in a corundum crucible, the particle size of vanadium-iron alloy fine powder is 5μm-200μm, and the vanadium content is 50%, put the crucible in a quartz chlorination reactor, and pass 0.02m / s nitrogen, and then place the reactor in a tube furnace to heat up; when the furnace temperature reaches and remains constant at 500°C, readjust the nitrogen flow in the reactor, and feed chlorine and oxygen into the reactor to make the reactor The total gas velocity of nitrogen, chlorine and oxygen in the interior is maintained at 0.08m / s, the molar ratio of chlorine to oxygen is 2.5:1, and the volume fraction of chlorine in the mixed gas (chlorine, nitrogen and oxygen) is 20%; the chlorination reaction During the process, the volatilized components in the chlorination reactor are condensed and collected to obtain the crude product of vanadyl trichloride, and the tail gas is absorbed and purified by 30% aqueous sodium hydroxide solution; after r...

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Abstract

The invention belongs to the technical field of chemical metallurgy, and particularly relates to a method for preparing high-purity vanadium oxychloride from ferrovanadium fine powder. The technical problem to be solved by the invention is to provide a method for preparing high-purity vanadium oxytrichloride by effectively utilizing ferrovanadium fine powder. The method comprises the following steps: a, putting ferrovanadium fine powder into a chlorination reactor, introducing nitrogen, performing heating to 300-600 DEG C, introducing chlorine and oxygen, adjusting the total flow rate of nitrogen, chlorine and oxygen, carrying out chlorination reaction, and condensing volatile components in the reactor in the reaction process to obtain a vanadium oxytrichloride crude product; b, after thechlorination reaction is finished, stopping introducing the chlorine and the oxygen, adjusting the flow rate of the nitrogen again, and stopping introducing the nitrogen after the reactor is cooled toroom temperature; and c, distilling and condensing the vanadium oxytrichloride crude product to obtain high-purity vanadium oxytrichloride. By means of the method, the high-purity vanadium oxychloride product can be prepared, the purity can reach 99.9% or above, and meanwhile the chlorination efficiency of vanadium in ferrovanadium fine powder can be improved.

Description

technical field [0001] The invention belongs to the technical field of chemical metallurgy, and in particular relates to a method for preparing high-purity vanadium oxytrichloride by using ferrovanadium fine powder. Background technique [0002] Vanadyl trichloride is an important chemical intermediate, and is a catalyst or pre-catalyst for the preparation of ethylene-propylene rubber. Vanadyl trichloride can be used as an organic solvent and is a raw material for the synthesis of organic vanadium compounds. In addition, vanadium oxychloride is also an important raw material for preparing high-purity vanadium pentoxide, and the purity of high-purity vanadium pentoxide prepared from vanadium oxytrichloride usually reaches above 99.99% (4N). With the continuous development of chemical industry, energy storage and other industries, the demand for high-purity vanadium oxychloride is increasing day by day, especially in the field of vanadium battery energy storage, high-purity va...

Claims

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Application Information

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IPC IPC(8): C01G31/00
CPCC01G31/00
Inventor 杜光超张溅波范川林杨海涛朱庆山
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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