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Method for fractionating, extracting and separating zirconium and hafnium

An extraction, zirconium and hafnium technology, applied in the field of atomic level hafnium oxide, can solve the problems that the two phases cannot be effectively separated, the liquid-liquid extraction process cannot be carried out, and the emulsification problem cannot be solved, so as to achieve good phase separation, low toxicity, and easy The effect of the operation

Active Publication Date: 2010-06-30
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 fatal shortcoming is that the emulsification problem cannot be solved during the extraction process. As we all know, emulsification is the enemy in the smooth liquid-liquid extraction process.
Due to the emulsification phenomenon, the two phases to be extracted cannot be effectively separated, which eventually leads to the failure of the liquid-liquid extraction process.
[0003] Therefore, providing a method for separating zirconium and hafnium with a large capacity for extracting zirconium and a large separation coefficient of zirconium and hafnium has become an urgent technical problem in this technical field.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Measure 100 milliliters of P204, 25 milliliters of commercially available mixed alcohols with 7-9 carbon atoms (the same below), and 850 milliliters of sulfonated kerosene, pour them into a reaction tank and stir evenly, and prepare 975 milliliters of 10.3% P204 organic phase. 2925 milliliters of the feed liquid was put into the above-mentioned 975 milliliters of 10.3% organic phase, and the stirring continued for 30 minutes. The feed liquid is obtained by adding sulfuric acid to the raffinate obtained by extracting zirconium and hafnium with N235-sulfuric acid system, wherein ZrO 2 2.27g / L, HfO 2 is 0.36g / L, [H + ] is 3.07mol / L, titanium dioxide is 2.0g / L, and silicon dioxide is 1.0g / L. After 30 minutes, stop stirring, place and separate phases, and obtain HfO in the organic phase by phase separation after 20 minutes. 2 % at 23.7%.

[0038] The organic phase after the above extraction was put into a reaction tank, and 975 ml of washing liquid was added and stirred ...

Embodiment 2

[0042] Measure 150 ml of P204, 100 ml of mixed alcohol, and 700 ml of sulfonated kerosene into a reaction tank and stir evenly to prepare 950 ml of 15.8% P204 organic phase. 4750 milliliters of the feed liquid was put into the above-mentioned 950 milliliters of 15.8% P204 organic phase, and the stirring continued for 60 minutes. The feed liquid is obtained by adding sulfuric acid to the raffinate obtained by extracting zirconium and hafnium with N235-sulfuric acid system, wherein ZrO 2 5.38g / L, HfO 2 is 0.93g / L, [H + ] is 2.07mol / L, titanium dioxide is 0.5g / L, and silicon dioxide is 1.5g / L. After 60 minutes, stop stirring, place the phase separation, and obtain the HfO in the organic phase by phase separation after 10 minutes. 2 % is 41.8%.

[0043] The organic phase after the above extraction was put into a reaction tank cup, and 2850 ml of washing liquid was added and stirred continuously for 30 minutes. Wherein the concentration of oxalic acid in the lotion is 0.31mol / ...

Embodiment 3

[0047] Measure 50 ml of P204, 150 ml of mixed alcohol, and 925 ml of sulfonated kerosene into a reaction tank and stir evenly to prepare 1125 ml of 4.4% P204 organic phase. 2250 milliliters of the feed solution was put into the above-mentioned 1125 milliliters of 4.4% P204 organic phase, and the stirring continued for 40 minutes. The feed liquid is obtained by adding sulfuric acid to the raffinate obtained by extracting zirconium and hafnium with N235-sulfuric acid system, wherein ZrO 2 1.0g / L, HfO 2 is 0.6g / L, [H + ] is 2.0mol / L, titanium dioxide is 2.5g / L, and silicon dioxide is 0.5g / L. After 40 minutes, stop stirring, place the phase separation, and obtain the HfO in the organic phase by phase separation after 30 minutes. 2 % is 61.8%.

[0048] The organic phase after the above extraction was put into a reaction tank, and 2250 ml of washing liquid was added and stirred continuously for 10 minutes. Wherein the concentration of oxalic acid in the lotion is 0.15mol / L, [H ...

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Abstract

The invention relates to a method for fractionating, extracting and separating zirconium and hafnium, in particular to a method for fractionating, extracting and separating zirconium and hafnium by using di(2-ethylhexyl)phosphorous acid as an extracting agent. The method comprises the following steps of: (1) extraction, using 50-300 parts by weight of di(2-ethylhexyl)phosphorous acid, 25-150 parts by weight of mixing alcohol with the carbon number of 7-9, and 550-925 parts by weight of sulfonated kerosene to prepare a di(2-ethylhexyl)phosphorous acid organic phase to extract; (2) washing, adding oxalic acid into a sulphuric acid solution to prepare a washing solution to wash; and (3) stripping, using a mixing solution of ammonia and carbonate as a strip liquor, stripping to obtain a strip liquor containing hafnium, slowly adding concentrated hydrochloric acid to adjust the solution into acidity, adding concentrated ammonia to obtain hafnium hydroxide precipitate, washing, filtering, calcining, and then obtaining hafnium oxide. The used chemical agents are difficult to volatilize, the toxicity is low, the corrosion is weak, the disposition is easy, and the discharged waste water can not cause the environments to be polluted. The technology has the advantages of quick phase separation, convenient operation, and high and stable product quality.

Description

technical field [0001] The invention relates to a method for fractional distillation, extraction and separation of zirconium and hafnium, in particular to a method for fractional distillation, extraction and separation of zirconium and hafnium using bis(2-ethylhexyl) phosphoric acid (P204) as an extractant to obtain atomic level hafnium oxide. Background technique [0002] In nature, zirconium and hafnium always co-exist together. To obtain atomic-level zirconium and hafnium, only the extraction method can be used to separate zirconium and hafnium. The whole hydrometallurgical process of extraction and separation of zirconium and hafnium to produce atomic-level hafnium oxide goes through two stages. First, solvent extraction and separation of zirconium and hafnium, and second, precipitation and burning to atomic-level hafnium oxide. Previously, zirconium and hafnium were extracted and separated by liquid-liquid extraction process of TBP-hydrochloric acid and nitric acid mixe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G27/02
Inventor 张力王力军郎书玲陈松罗远辉
Owner 有研资源环境技术研究院(北京)有限公司
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