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Use and method of amino-containing neutral phosphine extractant for extracting and separating zirconium and/or hafnium

A neutral phosphine and amino-containing technology, applied in the field of amino-neutral phosphine extractant, extraction and separation of zirconium and/or hafnium, and can solve the problems of tributyl phosphate emulsification, high acidity, HSCN pollution, etc.

Active Publication Date: 2018-06-26
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN101643847A discloses a tributyl phosphate extraction resin for the separation of zirconium and hafnium and its preparation method. Although the method solves the problems of high acidity of the system, severe equipment corrosion and serious emulsification of tributyl phosphate during liquid-liquid extraction and separation of zirconium and hafnium , but it also faces the problems that the separation by resin method cannot be carried out continuously, and the amount of separation treatment is small.
CN1927725A discloses a process for preparing atomic-level zirconium oxide and hafnium oxide by methyl isobutyl ketone dual-solvent extraction method, but this method has serious problems such as MIBK and HSCN pollution

Method used

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  • Use and method of amino-containing neutral phosphine extractant for extracting and separating zirconium and/or hafnium
  • Use and method of amino-containing neutral phosphine extractant for extracting and separating zirconium and/or hafnium
  • Use and method of amino-containing neutral phosphine extractant for extracting and separating zirconium and/or hafnium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0131] Preparation of the organic phase: Mix 3L of 1-(2-ethylhexylamino)methyl bis(2-ethylhexyl)phosphonate with 7L of aviation kerosene to prepare the organic phase.

[0132] Feed liquid is the mixed solution of zirconium sulfate, wherein the concentration of zirconium is 0.2mol / L; Acidity is 1.5mol / L,

[0133] The washing solution is 0.5mol / L sulfuric acid solution.

[0134] The stripping agent is 1.0mol / L ammonia solution.

[0135] A 250ml mixed-clarified extraction tank was used for extraction and separation experiments. First, 20 stages of countercurrent extraction are carried out, and the flow ratio of the organic phase to the feed liquid is 10mL / min: 15mL / min to obtain a zirconium-containing extract. Then carry out 5 stages of countercurrent washing, the flow ratio of the zirconium-containing extract solution to the washing solution is 10mL / min: 5mL / min. Then carry out 5-stage countercurrent back extraction, the flow ratio of zirconium-containing extract solution and...

Embodiment 2

[0137] Preparation of the organic phase: 3 L of 1-(2-ethylhexylamino)ethylphosphonic acid bis(2-ethylhexyl) ester, 1 L of 2-methylheptanol and 6 L of aviation kerosene were mixed to prepare an organic phase.

[0138] The feed liquid is a mixed solution of zirconium and hafnium sulfate, wherein the concentration of zirconium is 0.2mol / L; the concentration of hafnium is 0.004mol / L; the acidity is 1.5mol / L,

[0139] The washing solution is 1.0mol / L hydrochloric acid solution.

[0140] The stripping agent is 1.0mol / L sodium hydroxide solution.

[0141] A 250ml mixed-clarified extraction tank was used for extraction and separation experiments. Firstly, 20 stages of countercurrent extraction are carried out, and the flow ratio of the organic phase to the feed liquid is 10mL / min: 15mL / min to obtain a zirconium-containing extract and a hafnium-containing tail liquid. Then carry out 7 stages of countercurrent washing, the flow ratio of the zirconium-containing extract solution to the...

Embodiment 3

[0143] Preparation of the organic phase: 3 L of 1-(2-ethylhexylamino) 1-methylethylphosphonic acid bis(2-ethylhexyl) ester was mixed with 7 L of aviation kerosene to prepare the organic phase.

[0144] The feed liquid is a mixed solution of zirconium and hafnium nitrate, wherein the concentration of zirconium is 0.5mol / L; the concentration of hafnium is 0.04mol / L; the acidity is 1.5mol / L,

[0145] The washing solution is 1.0mol / L nitric acid solution.

[0146] The stripping agent is 4.0mol / L nitric acid solution.

[0147] A 250ml mixed-clarified extraction tank was used for extraction and separation experiments. Firstly, 20 stages of countercurrent extraction are carried out, and the flow ratio of the organic phase to the feed liquid is 20mL / min: 10mL / min to obtain a zirconium-containing extract and a hafnium-containing tail liquid. Then carry out 7 stages of countercurrent washing, the flow ratio of the zirconium-containing extract solution to the washing solution is 20mL / m...

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Abstract

The present invention relates to the use and method of an amino-containing neutral phosphine extractant of the following general formula I for extracting and separating zirconium and / or hafnium, wherein R1 and R2 are each independently selected from C1-12 alkyl groups; R3 and R4 are each independently is selected from C1-3 alkyl and hydrogen; R5 and R6 are each independently selected from C1-16 alkyl and hydrogen, and at most one of R5 and R6 is hydrogen. After the neutral phosphine extraction system formed by using the amino-containing neutral phosphine extractant of the above general formula I as the main extractant is mixed with the material-liquid phase containing zirconium (IV) and / or hafnium (IV), after extraction, reaction After extraction and other steps, a solution or precipitate containing zirconium or hafnium is obtained, respectively. The results show that the purity of the final zirconium is greater than 99.99%, and the content of hafnium in zirconium is less than 80ppm, especially less than 10ppm. And purification, to reach the use standard of atomic level zirconium and hafnium.

Description

technical field [0001] The invention belongs to the technical field of hydrometallurgy of zirconium and hafnium, and specifically relates to the use and method of extracting and separating zirconium and / or hafnium with an amino neutral phosphine extractant. Background technique [0002] As a clean energy with mature technology, nuclear power has attracted extensive attention from researchers from various countries, and zirconium and hafnium are key materials for building nuclear reactors, and have been included in the key research objects of national strategic development. Zirconium and hafnium have very different nuclear properties and are therefore used in different aspects of nuclear reactors. The thermal neutron absorption cross section of zirconium is small (0.18±0.02b, 1b=10 -28 m 2 / atom), is widely used in reactor cladding and structural materials, while hafnium has a large thermal neutron capture cross section and is an important material for controlling thermonu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B34/14C22B3/38
CPCC22B34/14C22B3/3844C22B3/408Y02P10/20
Inventor 廖伍平陈社张志峰李艳玲
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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