Method for separating and preparing zirconia from zirconium oxychloride mother liquor

Abstract

The invention relates to a method for separating and preparing zirconia from zirconium oxychloride mother liquor. The zirconium oxychloride mother liquor is taken as a raw material, an organic multielement extraction agent is adopted and comprises, in percentage by volume, 5-25 percent of neutral extraction agent, 5-25 percent of acid extraction agent and 50-90 percent of diluent, zirconium in the zirconium oxychloride mother liquor is extracted into an organic phase to obtain a zirconium containing extract, hafnium contacting raffinate is obtained from a water phase, thereby realizing separating of the zirconium from hafnium. Then the organic phase is subjected to back extraction to obtain the zirconium containing back extraction liquid in the water phase, and the zirconium containing back extraction liquid is precipitated by ammonia water and is roasted to obtain zirconia. The method adopts the organic multielement extraction agent to achieve a better synergic action for the separating of the zirconium from hafnium, no emulsion exists in the extracting process, extracting and separating are easy, and the problem of easiness in emulsion in an extracting process of the single neutral extraction agent is solved; the extraction separating efficiency of the zirconium is obviously improved, and the recovery rate and purity of the zirconia are improved; the method does not use a high toxicity reagent such as thiocyanic acid and has small toxicity on the human body and the environment.

Description

technical field [0001] The invention relates to the technical field of material separation, in particular to a method for separating and preparing zirconia from zirconium oxychloride mother liquor. Background technique [0002] Zirconium and hafnium materials are important strategic materials. Atomic level zirconium is an ideal cladding material and structural material for atomic energy reactors because of its small thermal neutron absorption cross section and good corrosion resistance. For zirconium used in nuclear reactors, the mass content of hafnium is required to be less than 0.01%. This type of zirconium is called atomic-level zirconium. Since zirconium and hafnium have similar outer electron structures, affected by the contraction of lanthanides, their atomic radius, ionic radius, and structure are very close, and their chemical properties are very similar. In nature, zirconium and hafnium always coexist together, so it is necessary to The separation of zirconium an...

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Problems solved by technology

However, the thiocyanic acid in this system is toxic and irritating to the eyes and skin, and it decomposes rapidly at room temperature to produce toxic gases such as nitrogen and sulfur, which poses certain safety hazards

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