Method for separating zirconium and hafnium

A technology of zirconium hydroxide and hafnium hydroxide, which is applied in the field of separating zirconium and hafnium, can solve the problems of high water solubility of MIBK, easy pollution of the environment, and easy occurrence of fires, and solve the problems of large solvent loss, low mass transfer, boiling flash and The effect of high flash point

Active Publication Date: 2013-08-14
有研资源环境技术研究院(北京)有限公司
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  • Abstract
  • Description
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Problems solved by technology

[0010] The purpose of the present invention is to provide a solvent extraction method for separating zirconium and hafnium from an acidic aqueous solution containing zirconium and hafnium. , high toxicity, resulting in large loss of solvent, easy to fire, poor working conditions, easy to pollute the environment and other problems

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  • Method for separating zirconium and hafnium
  • Method for separating zirconium and hafnium

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Embodiment 1

[0039] A method for separating zirconium and hafnium, the specific steps are as follows:

[0040] (1) Preparation of acidic feed liquid: the composition of the water phase is the initial total concentration of zirconium and hafnium ions of 1.3 mol / L, of which the concentration of hafnium ions is about 0.016 mol / L, and the acidity of the water phase is 1.0 mol / L, [NH 4 SCN]=3.0mol / L, without adding (NH 4 ) 2 SO 4 .

[0041] (2) Using DIBK as the extractant, first pre-extract the extractant with an equal volume of 3.0 mol / L thiocyanic acid once, then use the extractant as the organic phase and the feed liquid as the water phase to control the comparison (organic phase: water Phase) is 2:1, the feed solution is subjected to single-stage extraction at room temperature, and the two-phase mixing time is 15 minutes. The zirconium remains in the water phase to obtain a hafnium-free zirconium solution, which is then precipitated with ammonia to obtain zirconium hydroxide precipitation , And...

Embodiment 2

[0046] The organic phase is composed of 10% (v / v) TBP and 90% (v / v) DIBK and pre-extracted once with an equal volume of 1.0 mol / L HSCN. The aqueous phase is composed of an initial total concentration of zirconium and hafnium ions of 1.5 mol / L, the concentration of hafnium ion is 0.018mol / L, the acidity of the water phase is 1.0mol / L, [NH 4 SCN]=3.0mol / L, (NH 4 ) 2 SO 4 The addition amount is 0.8mol / L, the control ratio is 2:1, single-stage extraction is performed at room temperature, the two-phase mixing time is 5 minutes, and then precipitation with ammonia water is used to obtain zirconium hydroxide precipitation and a load organic phase containing hafnium; The loaded organic phase was washed with 2.0 mol / L hydrochloric acid and 12 mol / L sulfuric acid for back extraction. The ratio of washing and back extraction was 1:2, and the mixing time of the two phases was 5 minutes to obtain 96% (Hf / (Hf +Zr)) hafnium-rich solution, using ammonia water for precipitation to obtain hafniu...

Embodiment 3

[0049] The organic phase is composed of 10% (v / v) TRPO and 90% (v / v) DIBK and pre-extracted once with an equal volume of 2.0 mol / L HSCN. The aqueous phase is composed of an initial total concentration of zirconium and hafnium ions of 2 mol / L , The concentration of hafnium ion is 0.02mol / L, the acidity of the water phase is 0.5mol / L, [NH 4 SCN]=3.0mol / L, without adding (NH 4 ) 2 SO 4 , The control ratio is 2:1, single-stage extraction is carried out at room temperature, the two-phase mixing time is 10 minutes, and then precipitation with ammonia water to obtain zirconium hydroxide precipitate and hafnium-containing supported organic phase; use 0.5mol of the supported organic phase / L hydrochloric acid for washing and 6.0mol / L sulfuric acid for back extraction, the ratio of washing and back extraction is 1:2, the two-phase mixing time is 10 minutes, and 90% (Hf / (Hf+Zr)) enrichment is obtained. The hafnium solution is precipitated with ammonia water to obtain hafnium hydroxide prec...

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Abstract

The invention relates to a method for separating zirconium and hafnium, which specifically comprises the following steps of: using the acidic water solution of a zirconium compound as a raw material, extracting hafnium in the material liquid into an organic phase by using diisobutyl ketone (DIBK) or the synergism of DIBK with a neutral phosphorous extracting agent or the synergism of DIBK with anacidic phosphorus-containing extracting agent, and washing and stripping the oganic phase to produce a hafnium-rich liquid such that the separation of zirconium and hafnium is realized; respectively precipitating the hafnium-rich liquid and the remaining organic phase by using ammonia water, and washing and roasting the precipitates to obtain atomic energy level zirconium oxide and hafnium oxide.In the technical method provided by the invention, low content of hafnium in zirconium hafnium is preferably extracted, and the method has simple process and high extraction efficiency. The extraction system used in the method reaches the same zirconium and hafnium separation performance to MIBK (Methyl Isobutyl Ketone) but has smaller water solubility, high boiling point and flashing point and smaller toxicity compared with MIBK, and the problems of great solvent loss, easy outbreak of fire, environmental pollution and the like in the MIBK extraction separation method are solved.

Description

Technical field [0001] The invention relates to a method for separating zirconium and hafnium, in particular to a method for separating zirconium and hafnium from an acidic aqueous solution containing zirconium and hafnium by using a solvent extraction method. The present invention uses the acidic aqueous solution of zirconium compound as raw material, adopts diisobutyl ketone (DIBK) or DIBK and neutral phosphorus-containing extractant or DIBK and acidic phosphorus-containing extractant to synergistically extract the hafnium in the feed liquid into the organic phase , The organic phase is washed and stripped to produce hafnium-rich material, so as to realize the separation of zirconium and hafnium. Background technique [0002] Zirconium in the earth's crust is mainly composed of oblique zircon (ZrO 2 ) And zircon (ZrSiO 4 ) Exists in the form of hafnium, and hafnium does not have a separate mineral, and it is always symbiotic with zirconium in nature, and there is no separate ha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/26C22B3/40C22B34/14
CPCY02P10/20
Inventor 王力军徐志高张力陈松郎书玲罗远辉车小奎黄永章蔡振平陈伟东
Owner 有研资源环境技术研究院(北京)有限公司
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