Method for separating zirconium hafnium by tributyl phosphate extraction chromatography method

A technology of tributyl phosphate and chromatographic separation, applied in liquid solution solvent extraction, zirconia and other directions, can solve the problems of large dissolution loss of methyl ethyl butyl ketone, inability to solve the emulsification problem, and inability to carry out the extraction process, etc. Achieve the effect of reducing irritating odor, easy operation and reducing product cost

Active Publication Date: 2008-07-02
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

AI Technical Summary

Problems solved by technology

The disadvantages of this method are: first, the dissolution loss of methyl ethyl butyl ketone is large; second, the decomposition of thiocyanate and thiocyanic acid (HCNS) and the decomposition products are toxic, forming toxic waste water
However, the disadvantages of this process are: first, the equipment and workshop are severely corroded; second, there is no way to solve the emulsification problem during the extraction process, which eventually leads to the failure of the extraction process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Configure 10 liters of acid solution: measure 7 liters of deionized water, add 0.85 liters of concentrated hydrochloric acid (chemically pure, the concentration of concentrated hydrochloric acid is 12 mol / liter), then add 2.15 liters of concentrated nitric acid (chemically pure, the concentration of concentrated nitric acid is 14 mol / liter) liter), stirred evenly, and the total free acid acidity of the saturated acid solution was measured to be 4.15 mol / liter.

[0033]Configure 2 liters of feed solution: Weigh 210 grams of industrial grade zirconium oxychloride and put it into 1.4 liters of deionized water to stir and dissolve. After dissolving, add 0.17 liters of concentrated hydrochloric acid (chemically pure, the concentration of concentrated hydrochloric acid is 12 mol / liter), then add 0.43 liters of concentrated nitric acid (chemically pure, concentration of concentrated nitric acid is 14 mol / liter), stir well, measure the total free acid acidity of feed liquid to b...

Embodiment 2

[0042] A method similar to that of Example 1 was used to configure different concentrations of acid solution, feed solution, washing hafnium solution and inverse zirconium solution. Use 50% TBP extraction resin. Rinse with a saturated acid solution of hydrochloric acid and nitric acid mixed acid with a total free acidity of 6.5 mol / liter, wherein the concentration ratio of hydrochloric acid and nitric acid is 4:1, the total volume of the eluate effluent is 10.5 liters, and the final effluent total The acidity of the free acid is 5.87 mol / liter. Add 1.0 liters of feed liquid, wherein the total concentration of zirconium and hafnium is 0.649 mol / liter [in terms of zirconium dioxide], and the content of hafnium oxide is 10%; the total free acid acidity of feed liquid is 7.5 mol / liter, wherein hydrochloric acid and The concentration ratio of nitric acid is 2:1. Then the TBP extraction resin column that adds feed liquid is carried out the drip washing of washing hafnium solution,...

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Abstract

The invention relates to a separation method of zirconium and hafnium by adopting extraction chromatography, in particular to extraction chromatography of zirconium and hafnium by employing tributylphosphate. The method comprises the following steps that: extractant-containing resin TBP is adopted to load the extraction chromatographic column; mixed solution of chlorhydric acid and nitric acid with total free acid acidity being 3.5-7.5 mol/l is adopted for eluting the extraction chromatographic column; then the obtained material is added with material liquid which is the mixed solution of chlorhydric acid and nitric acid with total free acid acidity being 3.5-7.5 mol/l; the total concentration of zirconium and hafnium is 0.05-1.5 mol/l; next, the mixed solution of chlorhydric acid and nitric acid with total free acid acidity being 4-8 mol/l is used for eluting the obtained material, until the concentration of overflowed hafnium solution is less than 0.01 g/l; then the mixed solution containing 0-1.5mol/l chlorhydric acid and nitric acid or 0-1.5mol/l chlorhydric acid solution is used for eluting, so as to get the zirconium solution containing no hafnium.

Description

technical field [0001] The invention relates to a method for separating zirconium and hafnium by extraction chromatography, more precisely, a method for separating zirconium and hafnium by extraction chromatography using tributyl phosphate (TBP) as an extraction agent to produce atomic-level zirconium oxide. Background technique [0002] Zirconium and hafnium in nature are always symbiotic together, and there is no separate hafnium. The extraction method is used to separate zirconium and hafnium, which is an important method for preparing atomic-level zirconium oxide and atomic-level hafnium oxide. In the past, zirconium tetrachloride was used as raw material to extract and separate zirconium and hafnium with ammonium thiocyanate-methyl ethyl butyl ketone (MIBK) extraction system to produce atomic-level zirconium oxide and atomic-level hafnium oxide. The disadvantages of this method are: first, the dissolution loss of methyl ethyl butyl ketone is large; second, the decomposi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02B01D11/04
Inventor 张力王力军郎书玲陈松罗远辉黄永章
Owner 有研资源环境技术研究院(北京)有限公司
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