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
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[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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