Method for separating zirconium and hafnium

A technology of zirconium hydroxide and hafnium hydroxide, applied in the field of separation of zirconium and hafnium, can solve the problems of high water solubility of MIBK, poor working conditions, easy environmental pollution, etc. The effect of less mass transfer

Active Publication Date: 2012-05-16
有研资源环境技术研究院(北京)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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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

Examples

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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 an initial total concentration of zirconium and hafnium ions of 1.3 mol / L, wherein 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) extractant adopts DIBK, earlier the thiocyanic acid of extractant and equal volume 3.0mol / L is carried out pre-extraction once, then extractant is used as organic phase, feed liquid is used as water phase, control compares (organic phase: water Phase) is 2:1, the material liquid is subjected to single-stage extraction at room temperature, the mixing time of the two phases is 15 minutes, the zirconium is left in the water phase, and a hafnium-free zirconium solution is obtained, and then precipitated with ammonia water to obtain a zirconium hydroxide pre...

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 1.0mol / L HSCN, and the aqueous phase is composed of an initial total concentration of zirconium and hafnium ions of 1.5mol / L L, where the concentration of hafnium ions is 0.018mol / L, the acidity of the aqueous 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 carried out at room temperature, the two-phase mixing time is 5 minutes, and ammonia water is used for precipitation to obtain a zirconium hydroxide precipitate and a loaded organic phase containing hafnium; The loaded organic phase was washed with 2.0mol / L hydrochloric acid and back-extracted with 12mol / L sulfuric acid, 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)) rich hafnium solution, using ammonia for precipitation to obtain...

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 2.0mol / L HSCN, and the aqueous phase is composed of an initial total concentration of zirconium and hafnium ions of 2mol / L , where the concentration of hafnium ions is 0.02mol / L, the acidity of the aqueous 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 precipitated with ammonia water to obtain a zirconium hydroxide precipitate and a loaded organic phase containing hafnium; the loaded organic phase is used 0.5mol / 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, to obtain 90% (Hf / (Hf+Zr)) rich The hafnium solution is precipitated by using ammonia water to obtain hafnium hydroxide...

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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 the raw material, and uses diisobutyl ketone (DIBK) or DIBK and a neutral phosphorus-containing extractant or DIBK and an acidic phosphorus-containing extractant to fully extract the hafnium in the feed solution into the organic phase , the organic phase is washed and back-extracted to produce hafnium-rich material, so as to realize the separation of zirconium and hafnium. 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 there is no separate mineral for hafnium, and it always coexists with zirconium in natur...

Claims

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Application Information

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Patent Type & Authority Applications(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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