Preparation method of vanadium pentafluoride

A technology of vanadium pentafluoride and fluorine gas, applied in the field of preparing vanadium pentafluoride, can solve the problems of not involving product impurity removal and purification, not disclosing the preparation process and conditions, high impurity content and the like, achieving low impurity content, Easy to operate and improve 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

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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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preparation example Construction

[0020] A preparation method of vanadium pentafluoride, comprising the following steps:

[0021] (i) Reactor pretreatment

[0022] Put metal vanadium in the reactor, and after the reactor is sealed and tested for leaks, preheat it to 150-300°C, stop heating, and evacuate the reactor to -0.1-0.08Mpa;

[0023] (ii) Synthesis reaction

[0024] Slowly feed fluorine gas into the reactor, and the fluorine gas and metal vanadium contact in the reactor to generate vanadium pentafluoride. This reaction is an exothermic reaction. At this time, the pressure of the reactor will gradually drop, and the temperature will gradually rise. high. When the pressure and temperature in the reactor no longer change, it is considered that the reaction of fluorine gas is complete, and the temperature of the reactor is controlled at 200-450°C. The reaction formula is:

[0025] 2V+5F 2 →2VF 5

[0026] In general, the amount of fluorine gas introduced each time should match the metal vanadium input...

Embodiment 1

[0032] Put 300g 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 -0.1Mpa. Slowly feed fluorine gas into the reactor, metal vanadium and fluorine gas synthesize and react to produce vanadium pentafluoride, and the temperature of the reactor is controlled at 200°C. After four hours, the reactor pressure did not drop any more and the reaction was terminated.

[0033] The crude product of vanadium pentafluoride from the reactor enters the distillation tower, and the temperature of the distillation tower is 15°C. After the light component impurities such as oxygen, nitrogen and hydrogen fluoride in the vanadium pentafluoride enter the tail gas treatment system, the temperature of the distillation tower is raised to 50°C. The temperature of the receiver is maintained at -10°C, and the product is collected in the receiver to obtain 800g of vanadium pentafluoride produc...

Embodiment 2

[0035] Put 300g of metal vanadium in the reactor. After the reactor is sealed and tested for leaks, it is preheated to 220°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 pentafluoride, and the temperature of the reactor is controlled at 320°C. After four hours, the reactor pressure did not drop any more and the reaction was terminated.

[0036] The vanadium pentafluoride crude product from the reactor enters the distillation tower, and the temperature of the distillation tower is 20°C. After the light component impurities such as oxygen, nitrogen and hydrogen fluoride in the vanadium pentafluoride enter the tail gas treatment system, the temperature of the distillation tower is raised to 75°C. The temperature of the receiver is maintained at -20°C, and the product is collected in the receiver to obtain 820g of vanadium pentafluoride product ...

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PUM

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Abstract

The invention discloses a preparation method of vanadium pentafluoride. The method comprises the following steps of: (i) pretreating a reactor, putting vanadium into the reactor, preheating the reactor, and pumping out; (ii) undergoing a synthetic reaction: contacting fluorine gas with metal vanadium in the reactor for undergoing a synthetic reaction to generate vanadium pentafluoride; (iii) removing impurities from crude vanadium pentafluoride in a distillation tower; and (iv) purifying the vanadium pentafluoride in the distillation tower. The method has the advantages of simple equipment, convenience for operating and low impurity content, the transformation rate of an intermediate byproduct can be increased effectively, and product purity can be over 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 fluorine gas and metal vanadium as raw materials. 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 +...

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张淑娟种保超
Owner HUAHE NEW TECH DEV COMPANY RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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