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Purpose and method of amido-contained neutral phosphine extracting agent for extracting and separating zirconium and/or hafnium

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

Active Publication Date: 2017-03-22
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Purpose and method of amido-contained neutral phosphine extracting agent for extracting and separating zirconium and/or hafnium
  • Purpose and method of amido-contained neutral phosphine extracting agent for extracting and separating zirconium and/or hafnium
  • Purpose and method of amido-contained neutral phosphine extracting agent 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 an 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 / mi...

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Abstract

The invention relates to a purpose and a method of an amido-contained neutral phosphine extracting agent for extracting and separating zirconium and / or hafnium. The amido-contained neutral phosphine extracting agent is expressed as the following formula I: FORMULA, wherein R1 and R2 are respectively and independently selected from C1-12 alkyl; R3 and R4 are respectively and independently selected from C1-3 alkyl and hydrogen; R5 and R6 are respectively and independently selected from C1-16 alkyl and hydrogen; and at most one of R5 and R6 is hydrogen. The amido-contained neutral phosphine extracting agent expressed as the formula I serves as a neutral phosphine extracting system for forming a main extracting agent to mix and extract with zirconium (IV) and / or hafnium (IV)-contained liquid; and then, such steps as extraction and reverse extraction are performed to respectively obtain zirconium or hafnium-contained solution or precipitates. The result shows that the purity of the finally obtained zirconium is higher than 99.99%, the content of hafnium in zirconium is lower than 80 ppm, in particular lower than 10 ppm; the purity of the obtained hafnium is higher than 99.0%, the content of zirconium in hafnium is lower than 0.1%; and the separation and the purification of zirconium and hafnium are effectively realized to achieve the use standards of atomic energy 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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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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