Tungsten Dioxydibromide Synthesis Process

Tungsten dioxydibromide (WO2Br2) is a purple-brown solid deliquescent prismatic crystal. Tungsten dioxydibromide can produce by mixed a certain stoichiometric tungsten powder, tungsten oxide and bromine to obtain.
Synthesis tungsten dioxydibromide processes as follows:
1. The mixture which consists of 2.758g (15mmol) tungsten powder, 6.956g (30mmol) tungsten oxide and 7.192g (45mmol) bromine with stoichiometry was placed in a reaction tube, putting 2mg of bromine in the tube to prevent generate low-cost tungsten bromide and tungsten bromide oxide and bromine in the reaction.
2. The reaction tube was melted under vacuum seal, and placed in a temperature gradient of 400/40 ℃ was heated until the bromine totally reacted, after preheating, putting the reaction tube  in the temperature gradient of 450/325 ℃ was heated 15h .
3. To sublimation purification the crude product for a second time.
4. To separate off more volatile impurities WOBr4 and WBr5 then can get pure crystalline tungsten dioxydibromide.
During synthesis tungsten dioxydibromide when use bromine or iodine need to preheat the reactants in order to prevent the tube explosion, because there is a higher pressure of halogen partial. And during the heating period, only put the end which containing a mixture of tungsten powder and tungsten oxide into the oven until the elemental halogen exhausted to generate a high halide and halogen tungsten oxide so far.

 

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