It can be prepared by reducing tungsten hexachloride with red phosphorus at 250-280°C or reducing tungsten hexachloride with hydrogen at 380-400°C. It can be obtained by the disproportionation reaction of tungsten tetrachloride, and it can also be obtained by the decomposition of tungsten trichloride in red heat. The specific method is as follows:
One of the synthesis methods of tungsten pentachloride
2WCl6+H2→2WCl5+2HCl
In a quartz tube, heat tungsten hexachloride at 410-425°C while passing hydrogen gas for reduction. Since WClO and low-priced WCl4, WCl2, etc. are generated at the same time, it needs to be sublimated and refined in a nitrogen flow, and then stored in a closed tube.
There are two synthetic methods for tungsten pentachloride
2WCl6+C2Cl4→2WCl5+C2Cl6
Using the same device as in the tungsten tetrachloride production method, if the reaction conditions are changed, the yield of tungsten pentachloride is higher than that of tungsten tetrachloride. That is, for 4-7g of raw material tungsten hexachloride, 25mL of tetrachlorethylene can be used. Vacuum was drawn and irradiated with a 100W bulb, and the reaction was carried out in an oil bath at 100°C for 24 hours. The initial reddish-brown solution turned blue-green, and at the end of the reaction, a fine dark powder was formed.
The operation steps are exactly the same as the preparation of tungsten tetrachloride, but because the product is highly hygroscopic, it cannot be in contact with air and should be fully dried before storage. When refining, the product can be put into a hard glass tube, so that it is in a vacuum or nitrogen, carbon dioxide gas flow, the glass tube is placed in an electric furnace and a temperature gradient of 180 ° C to 25 ° C is formed, then in the chloride of tungsten , the most sublimable tungsten pentachloride will be precipitated first, and tungsten tetrachloride will turn black and finally remain. Take out the target product under inert gas and keep it isolated from air.
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