Process for separation of hafnium tetrachloride from...

C - Chemistry – Metallurgy – 01 – G

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204/45, 204/80

C01G 27/04 (2006.01) B01D 57/00 (2006.01) C01G 25/04 (2006.01) C22B 4/04 (2006.01) C25B 1/26 (2006.01)

Patent

CA 1333781

A process for separation of hafnium tetrachloride from zirconium tetrachloride is disclosed. Zirconium tetrachloride containing hafnium tetrachloride in natural ratio dissolved in a molten salt is reduced in the first phase electrolysis to produce zirconium trichloride containing a hafnium content lower than that of the zirconium tetrachloride at a cathode. Next, in the second phase eletrolysis the zirconium tetrachloride under maintenance of an initial concentration thereof is further reduced with another cathode by using as an anode the former cathode on which the zirconium trichloride was produced in order to yield zirconium trichloride of a lower hafnium content at another cathode and at the same time evolve on the anode gaseous zirconium tetrachloride having a high pressure by oxdizing zirconium trichloride produced in the first phase electrolysis. This evolved zirconium tetrachloride is separated and recovered as zirconium tetrachloride with a low hafnium content. Further, the zirconium tetrachloride with a low hafnium content and the zirconium trichloride with a lower hafnium content are produced by changing over polarities of the cathode and the anode when zirconium trichloride on the anode decreases. Subsequently, the production of zirconium tetrachloride is continued by exchanging polarities of the electrodes and the second phase electrolysis is carried out repeatedly. After hafnium tetrachloride is concentrated to an expected value in the molten salt at above mentioned electrolysis, the salt is transferred to a separate vessel. And then it is heated to evaporate and separate highly concentrated hafnium tetrachloride. Thus, zirconium tetrachloride and hafnium tetrachloride are respectively separated with high efficiency. A hafnium content of zirconium tetrachloride separated is able to reduce to less than 100ppm, and a zirconium content of hafnium tetrachloride separated is also reduced to less than 25wt%.

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