Method for separating and purifying hafnium and zirconium

C - Chemistry – Metallurgy – 01 – G

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C01G 25/00 (2006.01) C01G 27/00 (2006.01) C22B 3/00 (2006.01)

Patent

CA 2572612

The invention concerns a method for separating hafnium and zirconium from a mixture containing ZrCl4 and HfCl4, the method comprising the following steps: 1) introducing the ZrCl4 and HfCl4 mixture in vapour form into a continuous extractive distillation column; 2) selectively absorbing ZrCl4 and HfCl4 vapours with an extraction solvent circulating counter-current relative to said vapours in the distillation column; 3) drawing a liquid or gaseous ZrCl4 and HfCl4 mixture enriched in ZrCl4; 4) drawing a liquid or gaseous ZrCl4 and HfCl4 mixture enriched in HfCl4; 5) hydrolyzing the mixture obtained at step 4) in an inorganic acid aqueous solution, so as to form an aqueous solution having 7 to 12 acid moles per liter; 6) passing the solution obtained at step 5) through an anion exchanging resin; 7) eluting and recovering a hafnium-enriched fraction.

Procédé pour la séparation du hafnium et du zirconium, à partir d'un mélange contenant ZrCl4 et HfCl4, le procédé comprenant les étapes suivantes : 1. introduire le mélange de ZrCl4 et HfCl4 sous forme vapeur dans une colonne de distillation extractive en continu ; 2. procéder à l'absorption sélective des vapeurs de ZrCl4 et HfCl4 par un solvant d'extraction circulant à contre- courant desdites vapeurs dans la colonne de distillation; 3. soutirer un mélange liquide ou gazeux de ZrCl4 et HfCl4 enrichi en ZrCl4 ; 4. soutirer un mélange liquide ou gazeux de ZrCl4 et HfCl4 enrichi en HfCl4; 5. hydrolyser le mélange obtenu à l'étape (4) dans une solution aqueuse d'acide inorganique fort, de manière à former une solution aqueuse ayant de 7 à 12 moles d'acide par litre ; 6. faire passer la solution obtenue à l'étape (5) dans une résine échangeuse d'anions ; 7. laisser éluer et récupérer une fraction enrichie en hafnium.

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