Method and device for preparing high-purity tungsten hexachloride

Abstract

The invention discloses a method and a device for preparing high-purity tungsten hexachloride. According to the method, tungsten powder, chlorine gas and active carbon are used as raw materials in a mole ratio of 100:(300-600):(1-20), the tungsten powder is added from a side part of a chlorination furnace, part of the chlorine gas is introduced from the bottom of the chlorination furnace, the chlorination temperature is 600-1000 DEG C, gaseous tungsten hexachloride, a small amount of tungsten oxychloride and low-valent tungsten chloride and excess chlorine gas are introduced into a refining furnace, another part of the chlorine gas is also introduced into the refining furnace, the refining furnace is filled with the active carbon, the refining temperature is controlled to be 600-1000 DEG C, the tungsten oxychloride and low-valent tungsten chloride in steam are converted into tungsten hexachloride, the refined tungsten hexachloride steam is introduced into a receiving tower through the upper side of a receiving tower at the other side of the refining furnace, and tungsten hexachloride is extracted out of the bottom of the receiving tower. The method disclosed by the invention is short in flow and less in equipment, is energy-saving and environment-friendly, realizes efficient utilization of resources, achieves integration of roughing and refining of tungsten hexachloride, and has important significances for improvement of a tungsten hexachloride preparation technology.

Description

technical field [0001] This patent relates to a preparation method and device of high-purity tungsten hexachloride, belonging to the field of rare material manufacturing. Background technique [0002] Tungsten hexachloride is a low boiling point (346°C), highly active crystalline powder. As a new material raw material, tungsten hexachloride is oriented to the application field of new materials and has been widely used in many industries. For example, the catalytic application in the chemical industry, the manufacturing and repair of the machinery industry, and the surface coating treatment in the glass industry have been widely used in new material fields such as automobiles and glass industries. It can also be used for the purification of tungsten and the synthesis of organic compounds. [0003] Tungsten hexachloride is used as a new raw material, and its purity is a key concern in the downstream application field. At the same time, as the application range of tungsten he...

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Problems solved by technology

[0004] At present, there are many preparation methods of tungsten hexachloride. The direct chlorination method of tungsten and the chlorination method of tungsten compounds have existed for a long time. The industrial production of tungsten hexachloride has also reached a considerable scale. Facing the problem of insufficient purity, the reason is that tungsten oxychloride compounds such as tungsten oxychloride in the preparation process of tungsten hexachloride affect the quality of downstream products of tungsten hexachloride. , including tungsten oxychloride, tungsten dichloride dioxide, tungsten oxychloride and other compounds, so it is necessary to refine the crude tungsten hexachloride to remove the tungsten oxychloride impurities. The existing tungsten hexachloride The refining method is to steam low-boiling tungsten oxychloride and low-valent tungsten chloride first at low temperature, and then steam hexachloride at high temperature to separate it from high-boiling tungsten oxychloride. On the one hand, the yield of purified tungsten hexachloride is low, and A large part is oxidized to tungsten oxychloride during operation, and part of tungsten hexachloride is also evaporated during the steaming process of low boiling point tungsten oxychloride and low price tungsten chloride, on the other hand, tungsten hexachloride is steamed out It will also entrain a part of high boiling point tungsten oxychloride to affect the purity of tungsten hexachloride

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