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Method for purifying crude vanadium oxytrichloride

A technology of vanadium oxychloride and oxygen, applied in chemical instruments and methods, vanadium halide, vanadium compounds, etc., can solve the problem that impurities cannot be effectively removed, and achieve the effect of high popularization and application value, low cost and mild process conditions

Pending Publication Date: 2022-04-22
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is in order to overcome the VCl in the vanadium oxychloride that prior art exists 4 The problem that impurities cannot be effectively removed provides a method for purifying crude vanadium oxychloride, which can efficiently remove VCl in vanadium oxychloride 4 Impurities, to obtain high-purity vanadium oxychloride

Method used

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  • Method for purifying crude vanadium oxytrichloride

Examples

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Comparison scheme
Effect test

Embodiment 1

[0040] (1) Place 100g of crude vanadyl trichloride in a polytetrafluoro flask with magnetic stirring function. The flask contains an air inlet and a condensation return pipe made of polytetrafluoroethylene. 4 The content is 1.003% by weight, VOCl 3 The content is 98.997% by weight, and the oxygen that feeds 0.5L / min purity into the flask is 99.99%, under the condition of condensation reflux (condensation reflux operation adopts dehydrated alcohol as condensation medium, and the temperature of condensation medium is-5 ℃ ), contact the crude vanadyl trichloride with oxygen and react at 100°C (the reaction is carried out under the condition of magnetic stirring, and the speed of magnetic stirring is 200r / min), after reacting for 5h, stop feeding oxygen and stop magnetic stirring; The tail gas produced by condensation reflux is absorbed and purified by 25% by weight of NaOH aqueous solution;

[0041] (2) the condensing reflux tube is replaced with a condensing tube made of polyte...

Embodiment 2

[0043] (1) Place 150g of crude vanadyl trichloride in a polytetrafluoro flask with magnetic stirring function. The flask contains an air inlet and a condensation return pipe made of polytetrafluoroethylene. 4 The content is 3.304% by weight, VOCl 3 The content is 96.696% by weight, and the oxygen of 99.99% is passed into the purity of 1.5L / min in the flask, under the condition of condensation reflux (condensation reflux operation adopts dehydrated alcohol as condensation medium, and the temperature of condensation medium is-15 ℃ ), contact the crude vanadyl trichloride with oxygen and react at 150°C (reaction is carried out under the condition of magnetic stirring, and the speed of magnetic stirring is 300r / min), after reacting for 3h, stop feeding oxygen and stop magnetic stirring; The tail gas produced by condensation reflux is absorbed and purified by 25% by weight of NaOH aqueous solution;

[0044] (2) Replace the condensing reflux tube with a condensing tube made of poly...

Embodiment 3

[0046] (1) Place 200g of crude vanadyl trichloride in a polytetrafluoro flask with magnetic stirring function. The flask contains an air inlet and a condensation return pipe made of polytetrafluoroethylene. 4 The content is 4.951% by weight, VOCl 3 The content is 95.049% by weight, and the oxygen of 2L / min purity is 99.99% is passed into the flask, under the condition of condensation reflux (condensation reflux operation adopts dehydrated alcohol as condensation medium, and the temperature of condensation medium is-20 ℃) , contact the crude vanadyl trichloride with oxygen to react at 180°C (the reaction is carried out under the condition of magnetic stirring, and the speed of magnetic stirring is 500r / min), after reacting for 2h, stop feeding oxygen, stop magnetic stirring; The tail gas produced by reflux is absorbed and purified by 25% by weight of NaOH aqueous solution;

[0047] (2) Replace the condensing reflux tube with a condensing tube made of polytetrafluoroethylene, t...

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Abstract

The invention relates to the field of chemical metallurgy, and discloses a method for purifying crude vanadium oxytrichloride. The method comprises the following steps: (1) under the condition of reflux condensation, crude vanadium oxytrichloride is contacted with oxygen for reaction, the reaction temperature is 100-180 DEG C, the reaction time is 2-5 hours, and the temperature of a condensing medium for reflux condensation is-5 to-20 DEG C; and (2) distilling the material obtained in the step (1), and collecting a liquid product obtained by condensation. The method has the advantages that the effect of removing VCl4 from the crude vanadium oxytrichloride is good, the effect of purifying the crude vanadium oxytrichloride is good, the operation is simple and convenient, the process conditions are mild, and the purity of the obtained vanadium oxytrichloride product is high.

Description

technical field [0001] The invention relates to the field of chemical metallurgy, in particular to a method for purifying crude vanadyl trichloride. Background technique [0002] Vanadium oxychloride (VOCl 3 ) is a typical chemical intermediate, which is widely used in the preparation of vanadium refined chemicals, catalysis, and the preparation of medical drugs and other industries. VOCl 3 The application performance of vanadium chloride is usually highly related to its purity. To achieve better product application performance, high-purity vanadyl trichloride (usually greater than 99.99%) is often required. Currently, VOCl 3 The preparation process is roughly as follows: industrial vanadium pentoxide (V 2 o 5 ) mixed with carbon evenly, at 300-600 ℃ with chlorine (Cl 2 ) to react to convert the vanadium in the raw material into gaseous VOCl 3 , and finally VOCl is obtained by condensation 3 . During the chlorination process, because the oxygen potential in the raw ...

Claims

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Application Information

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IPC IPC(8): C01G31/00C01G31/04
CPCC01G31/00C01G31/04C01P2006/80
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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