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Method for separating zirconium from hafnium by using elution extraction method

A technology of zirconium and hafnium and extraction, which is applied in the field of extraction and separation of zirconium and hafnium, can solve the problems that the extraction process cannot be carried out, equipment and plant corrosion, emulsification problems cannot be solved, etc., and achieve easy operation, high product quality and low consumption small effect

Active Publication Date: 2012-06-20
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantages of this process are: first, serious corrosion to equipment and workshops; second, there is no way to solve the emulsification problem in the extraction process, which eventually leads to the inability to carry out the extraction process (document: Zhang Pingwei. Solvent extraction and separation of zirconium and hafnium [J] . Rare Metals, 1992, 16(4): 286-292)

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  • Method for separating zirconium from hafnium by using elution extraction method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Prepare 2L mixed acid solution: add 0.168L concentrated hydrochloric acid (chemically pure, concentrated hydrochloric acid concentration is 12mol / L) to deionized water, then add 0.152 kg of ammonium thiocyanate, add deionized water to 2L, after each addition of substances Stir evenly, and measure the total free acid acidity of the saturated acid solution to be 1.0mol / L.

[0034] Prepare 4L feed liquid: Weigh 1.66 kg of industrial grade zirconium oxychloride, 0.86 kg of ammonium thiocyanate and 0.248 kg of ammonium sulfate, stir and dissolve in 2L of deionized water, filter after dissolving, and add deionized water To 4L, the total concentration of zirconium ion and hafnium ion is 1.17mol / L, the content of hafnium dioxide accounts for 2.07% of the total weight of hafnium dioxide and zirconium dioxide, and the total free acid acidity of described feed liquid is 1.0mol / L ( The acidity here is because the zirconium oxychloride raw material is crystallized from a 6.0mol / L hy...

Embodiment 2

[0048] Prepare 2L mixed acid solution: add concentrated hydrochloric acid (chemically pure, concentration of concentrated hydrochloric acid is 12mol / L) and ammonium thiocyanate in deionized water, wherein the concentration ratio of hydrochloric acid and ammonium thiocyanate is 1:1, add deionized water to 2L, stir evenly, and measure the total free acid acidity of the saturated acid solution to be 1.0mol / L.

[0049] Prepare 2L feed liquid: Weigh 0.415 kg of industrial grade zirconium oxychloride, 0.294 kg of ammonium thiocyanate and 0.085 kg of ammonium sulfate, stir and dissolve in 1L of deionized water, filter after dissolving, add 12mol / L of Concentrated hydrochloric acid 0.066L, add water to 2L, the total concentration that obtains zirconium ion and hafnium ion in the material liquid is 0.58mol / L, the content of hafnium dioxide accounts for 2.04% of hafnium dioxide and zirconium dioxide gross weight, described material The total free acidity of the liquid is 1.0mol / L, the c...

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Abstract

The invention discloses a method for separating zirconium from hafnium by using an elution extraction method, belonging to the technical field of zirconium and hafnium separation. The method comprises the following steps of: preparing liquid MIBK (Methyl Iso Butyl Ketone) into MIBK elution extraction resin; extracting hafnium with an extraction agent of MIBK; reserving hafnium in a material liquid water phase and precipitating water ammonia water; eluting the elution extraction resin with hydrochloric acid and desorbing the elution extraction resin with sulfuric acid solution to obtain a solution containing hafnium; precipitating with ammonia water; and respectively washing and roasting the precipitation to obtain zirconium oxide and hafnium oxide in atomic energy level. The process method has the advantages of less mass transfer, high extraction capacity, large zirconium and hafnium separation coefficient, simple process flow and less investment and is easy for operation; two qualified products can be obtained by one-time extraction; the equipment has high yield and the consumption of chemical materials is low. According to the invention, the concentration of the used thiocyanic acid is lower than that used by a liquid-liquid solvent extraction method; the equipment is easy to close; and the pollution of H2S, HCN and methyl mercaptan generated by decomposing the volatilized MIMK and HSCN to the environment can be greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of zirconium and hafnium separation methods, in particular to a method for separating zirconium and hafnium by extraction and leaching. Background technique [0002] The zirconium ore isolates of zirconium in the earth's crust are mainly badley zircon (ZrO 2 ) and zircon (ZrSiO 4 ) exists in the form of hafnium, but hafnium does not have a separate mineral. It always coexists with zirconium in nature. There is no separate hafnium ore. The content of hafnium in zirconium in nature is generally 2 to 3%. Due to the huge difference in the nuclear properties of zirconium and hafnium, the content of hafnium in atomic energy grade zirconium is required to be less than 100ppm, and the content of zirconium in atomic energy grade hafnium is required to be less than 2%. Zirconium and hafnium are chemically very similar and it is very difficult to separate them from each other. The wet methods for the separation of z...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B34/14C22B3/42C22B3/26
CPCY02P10/20
Inventor 王力军张力徐志高郎书玲陈松罗远辉吕标起
Owner 有研资源环境技术研究院(北京)有限公司
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