Pyrometallurgical separation method for zirconia/hafnium dioxide mixture

A separation method and mixture technology, which is applied in the field of zirconium and hafnium separation, can solve the problems of poor purification and impurity removal, large investment, and high equipment requirements, and achieve the effect of economical equipment investment, good separation effect, and easy industrialization

Active Publication Date: 2014-04-16
ЧЖУ, СИНФЭН
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that the equipment and transportation system are operated at 350-500 °C, which requires high equipment, poor purification and impurity removal, and large investment. It is suitable for large-scale zirconium and hafnium smelters

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a corrosion-resistant and high-temperature resistant ceramic reactor, add zirconium and hafnium oxides, add corresponding carbon, and enter the vaporized raw material pure bromine into the high-temperature reactor through nitrogen. The reactor is kept at 650 degrees, and the raw material bromine is added. After that, keep it at 650 degrees for one hour, and then obtain a mixture of zirconium tetrabromide and hafnium tetrabromide under cooling.

[0026] Enter the next step of rectification tower separation, add the mixture of zirconium tetrabromide and hafnium tetrabromide in the corrosion-resistant and high-temperature resistant ceramic reactor, add the molten salt mixture, the molten salt is a molten mixture of potassium fluoride and potassium aluminum sulfate The weight ratio is potassium fluoride: potassium aluminum sulfate=1.2~1.6:1, keep it below 357 degrees for two hours, the obtained product is non-target, keep it at 357 degrees for five hours, collect the targ...

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PUM

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Abstract

The invention relates to a pyrometallurgical separation method for a zirconia/hafnium dioxide mixture. The zirconia/hafnium dioxide mixture, carbon and pure bromine react at 650 DEG C for 1 hour to obtain bromides of zirconium and hafnium, the bromides of the zirconium and the hafnium are added into a fused salt mixture to perform rectification separation, the temperature of the tower bottom of a rectifying tower is kept below 357 DEG C for 2 hours, and a non-target is obtained; the non-target is kept at 357 DEG C for 5 hours, and a target, namely high-purity zirconia tetrabromide is collected; residue in a kettle is stored; rectification separation is performed in the same equipment, the temperature is increased to 400 DEG C and kept for over 5 hours, hafnium tetrabromide is obtained, and the zirconia tetrabromide and the hafnium tetrabromide are respectively subjected to metathesis to obtain pure zirconium and pure hafnium. The separation effect is good, and the equipment investment is economical, so that industrialization is facilitated. The pyrometallurgical separation method can fill a blank in China, and greatly contributes the localization of zirconia/hafnium nuclear materials.

Description

[technical field] [0001] The invention relates to a method for separating zirconium and hafnium, in particular to a fire separation method for a mixture of zirconium oxide / hafnium oxide. [Background technique] [0002] Zirconium and hafnium have unique high temperature resistance, radiation resistance, and corrosion resistance. In the atomic energy industry, zirconium alloys are used as reactor cladding and structural materials, and hafnium is used as reactor control materials. Zirconium and hafnium are also widely used in chemical industry, metallurgy, electronics and other fields. [0003] The chemical properties of zirconium and hafnium are very similar, and they usually coexist in the ore in the form of oxides. The mass fraction of hafnium in natural zirconium resources is usually 1.5% to 3% of zirconium. Compared with this, atomic-level sponge zirconium requires w( Hf)<0.01%. Therefore, the separation technology of zirconium and hafnium is the key to producing atom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/14
CPCC22B9/02C22B34/14Y02P10/20Y02W30/50C01G25/02C01G27/02C22B7/002C01G25/04C22B5/00C01G27/04C22B15/008C22B15/0073
Inventor 朱兴峰
Owner ЧЖУ, СИНФЭН
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