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Diphosphoric acid extractant for extracting and separating zirconium and hafnium, and preparation method thereof

An extraction agent, bisphosphoric acid technology, applied in the field of new bisphosphoric acid extraction agent and its preparation, can solve the problem of low extraction rate of zirconium and hafnium

Active Publication Date: 2020-02-04
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, under this acidity, the common acidic organophosphorus extractant has a low extraction rate for zirconium and hafnium, so it is necessary to develop a new type of extractant to improve the extraction capacity for zirconium and hafnium

Method used

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  • Diphosphoric acid extractant for extracting and separating zirconium and hafnium, and preparation method thereof
  • Diphosphoric acid extractant for extracting and separating zirconium and hafnium, and preparation method thereof
  • Diphosphoric acid extractant for extracting and separating zirconium and hafnium, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 100ml three-necked round-bottom flask equipped with a spherical condenser and a mechanical stirring device, add 0.02 mol n-octylamine, 0.02 mol phenyl hypophosphorous acid, 35 ml water and 5 ml concentrated hydrochloric acid, stir the mixture and heat it to 60°C, gradually changing to It is a colorless transparent solution. Add 6 ml of 37% formaldehyde solution dropwise at reflux temperature, keep the temperature constant, and react for one hour. After cooling, the organic phase was washed several times with dilute hydrochloric acid, and then further purified by column chromatography to finally obtain N,N-n-octylamine di(methylene phenylphosphinic acid). The extractant yield and purity are shown in Table 1.

Embodiment 2

[0022] In a 100ml three-necked round-bottom flask equipped with a spherical condenser and a mechanical stirring device, add 0.02 mol n-octylamine, 0.04 mol phenyl hypophosphorous acid, 25 ml water and 15 ml concentrated hydrochloric acid, stir the mixture and heat it to 60°C, gradually changing to It is a colorless transparent solution. Add 6 ml of 37% formaldehyde solution dropwise at reflux temperature, keep the temperature constant, and react for two hours. After cooling, the organic phase was washed several times with dilute hydrochloric acid, and then further purified by column chromatography to finally obtain N,N-n-octylamine di(methylene phenylphosphinic acid). The extractant yield and purity are shown in Table 1.

Embodiment 3

[0024] In a 100ml three-necked round-bottomed flask equipped with a spherical condenser and a mechanical stirring device, add 0.02 mol of n-octylamine, 0.06 mol of phenyl hypophosphorous acid, 10 ml of water and 30 ml of concentrated hydrochloric acid, stir and heat the mixture to 60°C, gradually becoming It is a colorless transparent solution. Add 6 ml of 37% formaldehyde solution dropwise at reflux temperature, keep the temperature constant, and react for four hours. After cooling, the organic phase was washed several times with dilute hydrochloric acid, and then further purified by column chromatography to finally obtain N,N-n-octylamine di(methylene phenylphosphinic acid). The extractant yield and purity are shown in Table 1.

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Abstract

The invention discloses a novel diphosphoric acid extractant N,N-n-octylamine di(methylene phenyl hypophosphorous acid) for extracting and separating zirconium and hafnium, and a preparation method thereof. The extractant has the advantages of convenience in synthesis, good oil solubility and excellent stability. The N,N-n-octylamine di(methylene phenyl hypophosphorous acid) has very strong extraction capacity on zirconium and hafnium, and has a far higher extraction rate than a common acidic organic phosphorus extractant under the same conditions. The diphosphoric acid extractant preferentially extracts zirconium while ensuring the extraction rate, so the problems of low zirconium-hafnium extraction rate and poor separation effect are solved.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of zirconium and hafnium, and in particular relates to a novel bisphosphoric acid extractant for extraction and separation of zirconium and hafnium and a preparation method thereof. Background technique [0002] With the excessive consumption of traditional fossil energy such as coal, oil, and natural gas, and the negative impact of burning fossil fuels on the human living environment, nuclear energy has become an indispensable new energy due to its advantages in environmental protection, economy, and safety. Alternative energy has developed rapidly and matured in recent decades. Zirconium and hafnium are two extremely important metallic materials in the nuclear industry. Zirconium has a small thermal neutron absorption cross section (0.18b) and good corrosion resistance. It is used as cladding and structural materials of reactors, and is the first safety barrier to prevent the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C22B34/14C22B3/38
CPCC07F9/301C07F9/304C22B34/14C22B3/386Y02P10/20
Inventor 崔玉赵嘉琳赵奕铭
Owner UNIV OF JINAN
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