Method for extracting zirconium and hafnium from hydrochloric acid medium

An extraction and hydrochloric acid technology, applied in the field of purification, can solve the problems of large solvent loss, environmental pollution, poor operating workshop environment, etc., and achieve the effects of clean separation process, simple process flow and large extraction capacity.

Active Publication Date: 2018-06-05
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are some disadvantages in the MIBK method: (1) the solubility of MIBK in water is as high as 1.7wt% (it is one of the extraction agents with the highest solubility in water), and the solvent loss is large; (2) it is necessary to use unstable thiocyanic acid (and thiocyanic acid Salt), easily decomposed into toxic decomposition products under acidic conditions, such as hydrogen sulfide, methyl mercaptan and CN - etc., pollute the environment; (3) MIBK has a certain smell, which makes the operating workshop environment poor; ④ MIBK has a low flash point, which is easy to cause fire
It is precisely because of these shortcomings of the MIBK method that its industrial application is limited.
[0006] At present, when diisobutyl ketone (DIBK) is used as the extraction agent to separate zirconium and hafnium, thiocyanic acid or its salts are required. Due to the high toxicity of thiocyanic acid or its salts, it is not environmentally friendly during the separation process.

Method used

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  • Method for extracting zirconium and hafnium from hydrochloric acid medium
  • Method for extracting zirconium and hafnium from hydrochloric acid medium
  • Method for extracting zirconium and hafnium from hydrochloric acid medium

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Embodiment 1

[0053] A method for separating zirconium and hafnium, the specific steps are as follows:

[0054] (1) Preparation of acidic feed solution: the water phase is composed of an initial total concentration of zirconium and hafnium ions of 1.5mol / L, wherein the concentration of hafnium ions is about 0.018mol / L, and the acidity of the water phase is 1.7mol / L, (NH 4 ) 2 SO 4 The concentration is 0.8mol / L.

[0055] (2) extractant adopts the mixed organic phase that the DIBK of 90% (v / v) and the Cyanex923 of 10% (v / v) form, earlier the hydrochloric acid of extractant and equal volume 3.5mol / L is carried out pre-extraction once, then The extraction agent after the pre-extraction is used as the organic phase, the acid feed liquid is used as the water phase, and the control ratio (organic phase: water phase) is 2: 1, and the feed liquid is carried out to single-stage extraction at room temperature, and the mixing time of the two phases is 10 Minutes, after phase separation, the zirconiu...

Embodiment 2

[0078] The organic phase is composed of 90% (v / v) of DIBK, 2% (v / v) of Cyanex921 and 8% (v / v) of sulfonated kerosene (as a diluent), and pre-mixed with an equal volume of 3.4mol / L Hydrochloric acid pre-extracted once, the aqueous phase composition is the initial total concentration of zirconium and hafnium ions 1.5mol / L, wherein the concentration of hafnium ions is 0.018mol / L, and the acidity of the aqueous phase is 1.7mol / L, (NH4 ) 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 the raffinate and the loaded organic phase containing hafnium are obtained after phase separation. Re-precipitate with ammonia water to obtain zirconium hydroxide precipitate; carry out back-extraction with 1.0mol / L potassium carbonate on the loaded organic phase, the ratio of washing and back-extraction is 1:2, and the mixing time of the two phases is 5 minutes to obtain zirconium...

Embodiment 3

[0081] The organic phase is composed of 90% (v / v) of DIBK, 8% (v / v) of Cyanex923 and 2% (v / v) of isooctane (as a diluent), and pre-filled with an equal volume of 4.0mol / L Hydrochloric acid pre-extracted once, the aqueous phase composition is the initial total concentration of zirconium and hafnium ions 1.0mol / L, wherein the concentration of hafnium ions is 0.012mol / L, and the acidity of the aqueous phase is 2.0mol / 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 the raffinate and the loaded organic phase containing hafnium are obtained after phase separation. Re-precipitation with ammonia water to obtain precipitation of zirconium hydroxide with less hafnium; back-extract the loaded organic phase with 1.0mol / L sodium carbonate, the ratio of washing and back-extraction is 1:2, and the mixing time of the two phases is 5 minutes. A zirconium-contai...

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Abstract

The invention provides a method for extracting zirconium and hafnium from a hydrochloric acid medium and belongs to the technical field of fine separation of substances. The method is mainly characterized in that acid material liquid of a zirconium compound is extracted by a synergic extraction system consisting of DIBK and a phosphonic acid extracting agent, zirconium is enabled to enter an aqueous phase, and hafnium is enabled to enter an organic phase for realizing separation; toxic substances are not needed in the whole process and the aim of clean production is achieved.

Description

technical field [0001] The invention relates to the technical field of purification, in particular to a method for extracting and separating zirconium and hafnium in a hydrochloric acid medium. Background technique [0002] Zirconium and hafnium are always symbiotic in nature. The content of hafnium in general commercially available zirconium chemicals (m Hf / m (Zr+Hf) ) is less (generally 1% to 3%), and it will have a greater advantage if an extractant that preferentially extracts hafnium is used for its separation. Due to the "lanthanide contraction", the atomic and ionic radii of zirconium and hafnium are basically the same, and their physical and chemical properties are very similar. It is very difficult to separate each other. It is considered to be one of the most difficult elements in the periodic table to separate. However, due to the different nuclear properties of zirconium and hafnium, zirconium has a small thermal neutron absorption cross section, and is widel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/40C22B34/14C22B3/10
CPCC22B3/10C22B34/14C22B3/409C01G25/003C01G25/02C01G27/003C01G27/02
Inventor 徐志高张文杰吴明何正艳何宏杨张蓉
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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