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Method for preparing vanadic fluoride

A kind of technology of vanadium pentafluoride and vanadium tetrafluoride, applied in the field of preparing vanadium pentafluoride, can solve the problems such as no product impurity removal and purification, no disclosure of preparation process and conditions, high impurity content, etc. Less, easy to operate, and the effect of improving the conversion rate

Inactive Publication Date: 2012-06-20
HUAHE NEW TECH DEV COMPANY RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the above two methods for preparing vanadium pentafluoride have been reported, they are only theoretically analyzed and studied, and the detailed preparation process and conditions are not disclosed, and the removal of impurities and purification of the product are not involved.
Because the chemical properties of metal vanadium are very active, there are various valence states such as +5, +4, +3, +2, and intermediate fluorides are easily formed during the reaction process, resulting in high impurity content and low purity in the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put 200g of metal vanadium in the reactor. After the reactor is sealed and tested for leaks, it is preheated to 100°C, the heating is stopped, and the reactor is evacuated to -0.1Mpa. Slowly feed fluorine gas into the reactor, metal vanadium and fluorine gas synthesize and react to produce vanadium tetrafluoride, and the temperature of the reactor is controlled at 150°C. Two hours later, the reactor began to cool down. When the temperature reached 15°C, the reactor was evacuated to a pressure of -0.08Mpa. The temperature of the reactor is raised, and when the temperature reaches 100° C., the disproportionation reaction of vanadium tetrafluoride begins to generate the crude product of vanadium pentafluoride, which is maintained for two hours.

[0039] The crude product of vanadium pentafluoride from the reactor enters the distillation tower, the temperature of the distillation tower is 15°C, and the light component impurities such as oxygen, nitrogen and hydrogen fluorid...

Embodiment 2

[0042] Put 200g of metal vanadium in the reactor. After the reactor is sealed and tested for leaks, it is preheated to 150°C, the heating is stopped, and the reactor is evacuated to -0.09Mpa. Slowly feed fluorine gas into the reactor, metal vanadium and fluorine gas synthesize and react to produce vanadium tetrafluoride, and the temperature of the reactor is controlled at 200°C. Two hours later, the reactor began to cool down, and when the temperature reached 20°C, the reactor was evacuated to a pressure of -0.09Mpa. The temperature of the reactor is raised, and when the temperature reaches 110° C., the disproportionation reaction of vanadium tetrafluoride begins to generate the crude product of vanadium pentafluoride, which is maintained for two hours.

[0043] The vanadium pentafluoride crude product from the reactor enters the distillation tower, the temperature of the distillation tower is 20°C, and the light components impurities such as oxygen, nitrogen and hydrogen fluo...

Embodiment 3

[0046] Put 200g of metal vanadium in the reactor, and after the reactor is sealed and tested for leaks, it is preheated to 200°C, the heating is stopped, and the reactor is evacuated to -0.08Mpa. The fluorine gas is slowly introduced into the reactor, the metal vanadium and the fluorine gas synthesize and react to form vanadium tetrafluoride, and the temperature of the reactor is controlled at 250°C. Two hours later, the reactor began to cool down. When the temperature reached 25° C., the reactor was evacuated to a pressure of -0.1 Mpa. The temperature of the reactor is raised, and when the temperature reaches 120° C., the disproportionation reaction of vanadium tetrafluoride begins to generate the crude product of vanadium pentafluoride, which is maintained for two hours.

[0047] The crude product of vanadium pentafluoride from the reactor enters the distillation tower, the temperature of the distillation tower is 25°C, and the light component impurities such as oxygen, nitr...

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Abstract

The invention discloses a method for preparing vanadic fluoride. The method comprises the following steps: (i) the pretreatment is performed to a reactor, vanadium is put in the reactor, and is preheated to 100 to 200 DEG C, and the reactor is evacuated to 0.1 below zero to 0.08 below zero MPa; (ii), the synthetic reaction is carried out, fluorine gas is fed into the reactor slowly, and fluorine gas and vanadium are in synthetic reaction in the reactor to generate vanadium tetrafluoride; (iii), the dismutation reaction is carried out, and vanadium tetrafluoride is in dismutation reaction in the reactor to obtain crude products of vanadic fluoride; (iv) impurities in the crude products of vanadic fluoride are removed; and (v) vanadic fluoride is purified. The invention has the advantages that equipment is simple, the operation is convenient, the content of impurities is low, the rate of conversion of intermediate by-products can be improved effectively, and the product purity can reach more than 95 percent.

Description

technical field [0001] The invention belongs to a method for preparing vanadium pentafluoride, in particular to a method for preparing vanadium pentafluoride by using vanadium tetrafluoride as a raw material. Background technique [0002] Vanadium pentafluoride (VF 5 ) is a lively compound used as a strong oxidizing agent and a fluorinating agent in organic synthesis. The commonly used methods for preparing vanadium pentafluoride are metal direct fluorination and vanadium tetrafluoride disproportionation. The metal direct fluorination method is to prepare vanadium pentafluoride by heating metal vanadium and reacting with fluorine or bromine trifluoride. The reaction formula of metal vanadium and fluorine is: [0003] 2V+5F 2 →2VF 5 [0004] The vanadium tetrafluoride disproportionation method is a disproportionation reaction of vanadium tetrafluoride under vacuum conditions to generate vanadium pentafluoride. Its reaction formula is: [0005] 2VF 4 →VF 5 + VF 3 ...

Claims

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Application Information

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IPC IPC(8): C01G31/04
Inventor 张春芳李于教陈光华谢文雅侯姝刘玉静种保超
Owner HUAHE NEW TECH DEV COMPANY RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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