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Method using tributyl phosphate resin for fractional extraction to separate zirconium and hafnium

A technology of tributyl phosphate and resin, which is applied in the field of fractional extraction and separation of zirconium and hafnium with tributyl phosphate resin, which can solve the problems of low extraction efficiency and achieve the effects of large extraction phase capacity, reduced equipment corrosion, and stable operation

Inactive Publication Date: 2014-09-17
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

But the disadvantage is that the extraction chromatography is a single-stage extraction process, and the extraction efficiency is low.

Method used

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  • Method using tributyl phosphate resin for fractional extraction to separate zirconium and hafnium
  • Method using tributyl phosphate resin for fractional extraction to separate zirconium and hafnium
  • Method using tributyl phosphate resin for fractional extraction to separate zirconium and hafnium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment -1

[0057] Prepare 60 liters of acidified mixed acid solution: add 15 liters of hydrochloric acid (chemically pure, acidity of concentrated hydrochloric acid is 12 mol / liter), add 11.2 liters of nitric acid (chemically pure, acidity of concentrated nitric acid is 16 mol / liter), add 33.75 liters of deionized water, Stir evenly, and measure the total free acidity of the acidifying acid to be 6.03 mol / liter.

[0058] Prepare 45 liters of feed liquid: take 4.75 kilograms of industrial grade zirconium oxychloride, put it into 31.5 liters of deionized water, stir and dissolve, after dissolving, add 3.8 liters of hydrochloric acid (chemically pure, concentrated hydrochloric acid acidity is 12 mol / liter), Add 9.7 liters of nitric acid (chemically pure, concentrated nitric acid acidity is 16 mol / liter), stir, the total free acidity of measuring feed liquid is 6.15 mol / liter, and the total concentration of zirconium dioxide and hafnium dioxide is 72.97 grams / liter, The content of hafnium di...

Embodiment -2

[0069] A method similar to Example-1 was used to prepare acid solutions of different concentrations, feed liquid, washing liquid, anti-zirconium solution, and impurity removal solution. 45% TBP resin; The total free acidity of acidifying acid is 4.52 mol / liter; The total free acidity of feed liquid is 4.02 mol / liter, and the total concentration of zirconium and hafnium (calculated as oxide) is 50 grams / liter, the percentage of hafnium dioxide It is 5.7%; the total free acidity of the washing liquid is 4.05 mol / liter; the total free acidity of the anti-zirconium solution is 1.25 mol / liter; the total free acidity of the impurity removal solution is 1.65 mol / liter; compared to the extraction phase: acidifying acid: Washing solution: stripping solution: impurity removal solution=4.8:3:1:0.5:1.

[0070] The number of separation stages and operations are the same as in Example-1, and the zirconium dioxide concentration obtained in the inverse zirconium solution is 46 grams per liter...

Embodiment -3

[0072] Adopt similar conditions and operating methods as in Example-1, the only difference is that the content of the extractant in the extraction phase is different, use 35% TBP resin, and use a comparison as the extraction phase: acidifying acid: washing liquid: stripping liquid: removing Miscellaneous liquid=3:2:1:0.5:1 ratio, the separation stages are 3 stages of acidification, 7 stages of extraction, 6 stages of washing, 5 stages of stripping, and 5 stages of impurity removal. The zirconium dioxide concentration of the obtained inverse zirconium solution is 58 g / L, the percentage of hafnium dioxide is less than 0.01%, which meets the requirement of atomic energy level zirconium oxide, and the total recovery rate of zirconium dioxide is 81%.

[0073] In the TBP resin that above-mentioned embodiment uses, resin can also select: styrene-methyl methacrylate, styrene-methyl acrylate, styrene-glyceryl trimethacrylate, styrene-ethanol dimethacrylate, Polychlorotrifluoroethylene,...

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Abstract

The invention relates to a method using tributyl phosphate resin for fractional extraction to separate zirconium and hafnium; the tributyl phosphate resin is used as an extraction agent, and the zirconium and hafnium are extracted and separated by use of a box-countercurrent mode; the method comprises the following sections: 1), acidification section, to be more specific, using the tributyl phosphate resin as the extraction agent, putting an extraction phase and a mixed acid solution into a box-type extraction tank for countercurrent acidification; (2) extraction section, to be more specific, putting the acidified extraction phase and a material liquid containing the zirconium and hafnium into the box-type extraction tank for countercurrent acidification; (3) washing section, to be more specific, performing reverse-phase washing on the extraction phase with the zirconium being extracted; (4) back extraction section, to be more specific, performing reverse-phase back extraction on the washed extraction phase; and (5) impurity removal section, to be more specific, performing reverse-phase impurity removal on the back extracted extraction phase, using an impurity removal liquid for washing, wherein effluent is used as waste for emissions, and an outflow extraction phase is recycled. The method has the advantages of large extraction phase capacity, high production capacity, no emulsification, low product cost, stable operation, and high product quality.

Description

technical field [0001] The invention relates to a method for separating zirconium and hafnium by fractional distillation extraction with tributyl phosphate resin, using tributyl phosphate (TBP) to prepare the resin, adopting a box-countercurrent method, fractional distillation extraction and separation of zirconium hafnium, and producing atomic energy level zirconium oxide and Hafnium oxide. Background technique [0002] There are several methods for extraction and separation of zirconium and hafnium. At present, the United States adopts ammonium thiocyanate-methyl ethyl ketone (MIBK) extraction system to separate zirconium and hafnium to produce atomic-level zirconia. The advantage of this method is that the extraction and separation efficiency is high, and the disadvantage is that the dissolution loss of methyl ethyl ketone is large, thiocyanate and thiocyanic acid (HCNS) are easily decomposed and the decomposition products are toxic, forming toxic waste water and polluti...

Claims

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Application Information

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IPC IPC(8): C22B3/24C22B34/14
CPCY02P10/20
Inventor 郎书玲张力陈松王力军薛红霞
Owner 有研资源环境技术研究院(北京)有限公司
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