IP Library › Granted Patent US 10,094,000
Granted Patent B2
US 10,094,000 · App. 15/102,255 · Granted Oct 9, 2018

Method for separating the mixture of zirconium oxide/hafnium oxide by pyrometallurgy

Inventor: Xingfeng Zhu (Wuxi, CN)
C22B34/14C01G25/04C01G27/04C22B5/00C22B7/002C22B9/02C22B15/008C22B15/0073Y02P10/234
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Quick Facts
Patent No.
US 10,094,000
App. No.
15/102,255
Granted
Oct 9, 2018
Kind
B2
Abstract

A method for separating zirconium oxide/hafnium oxide by pyrometallurgy. The mixture of zirconium oxide/hafnium oxide, carbon and pure bromine react one hour at 650° C., then added to molten salt mixture for rectifying separation, and then maintained two hours at rectifying tower bottom below 357° C., to get the non-target substance; and then maintained five hours at 357° C. to collect the target substance zirconium tetrabromide; the residue in the reactor is retained, then rectification separation is performed in the same device, heated to 400° C. to retain more than five hours, to get hafnium tetrabromide, then the zirconium tetrabromide and hafnium tetrabromide are substituted by magnesium to get the pure zirconium and pure hafnium.

Claims (9)

1. A method for separating zirconium oxide and hafnium oxide from a mixture of zirconium oxide and hafnium oxide comprises the following steps:

mixing the mixture of zirconium oxide and hafnium oxide, carbon and pure bromine, reacting one hour at 650° C. which results in a mixture of zirconium tetrabromide and hafnium tetrabromide;

adding the mixture of zirconium tetrabromide and hafnium tetrabromide into molten salt for rectification separation, and maintaining the rectification for two hours at 200-357° C. which yields a non-target substance at the top of a rectification tower, wherein the molten salt is a molten mixture of potassium fluoride and aluminum potassium sulfate with a weight ratio of 1.2-1.6:1;

maintaining for additional five hours at 357° C.-360° C., collecting a target substance zirconium tetrabromide from the top of the rectification tower;

performing the rectification separation in the rectification tower, heat up to 400-403° C. and maintaining for five hours, and then collecting the hafnium tetrabromide from the top of the rectification tower.

2. The method according to claim 1 , wherein the temperature for collecting the zirconium tetrabromide is 357° C.

3. The method according to claim 1 , wherein the temperature for collecting the hafnium tetrabromide is 400° C.

4. The method according to claim 1 , wherein it further comprises: performing a magnetism replacement for the zirconium tetrabromide which yields a pure zirconium.

5. The method according to claim 1 , wherein it further comprises: performing a magnetism replacement for the hafnium tetrabromide which yields a pure hafnium.

Priority Claims (1)
CN 2013 1 0682029 · Dec 12, 2013 · national
Continuity (1)
Related Publication 20160348212A1 · Dec 1, 2016