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Process for preparing nuclear-grade hafnium oxide and zirconium oxide through solvent extractive separation of zirconium and hafnium

A technology of hafnium oxide and zirconium oxide, which is applied in the chemical field, can solve problems such as complex processes, and achieve the effects of simplifying process flow, improving extraction efficiency, and reducing work intensity

Inactive Publication Date: 2018-02-23
NANJING YOUTIAN METAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a process for solvent extraction and separation of zirconium and hafnium to prepare nuclear-grade hafnium oxide and zirconium oxide, so as to solve the problems of complex process, waste liquid and environmental protection in the prior art, and improve production efficiency

Method used

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  • Process for preparing nuclear-grade hafnium oxide and zirconium oxide through solvent extractive separation of zirconium and hafnium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Prepare 3molL -1 Acidification of nitric acid solution: Take 5L of concentrated nitric acid solution and add it to 20L of deionized water, stir and mix evenly. Prepare an organic phase containing 40% TBP and 10% ionic liquid by volume: take 10L TBP, 2.5L ionic liquid and 12.5L kerosene and mix them evenly. Prepare 1molL -1 Feed liquid: Take 6.45Kg of zirconium oxychloride, add deionized water to dissolve, add hydrochloric acid and nitric acid, make the solution acidity 4molL -1 , and finally set the volume to 20L. Preparation of 10% P204 organic phase: take 0.8L P204 and 7.2L kerosene and mix evenly. Preparation of 1.6L stripping solution: Dissolve 320g of ammonium bicarbonate in deionized water and dilute to 1.6L.

[0043] (2) First, the organic phase and the acidified nitric acid solution are compared in a ratio of 1:1, and the countercurrent acidification is carried out in a centrifugal extractor, and the organic phase is pretreated in three stages.

[0044]...

Embodiment 2

[0050] A method similar to that of Example 1 was used to prepare acid solutions, feed solutions and organic phases with different concentrations. The concentration of acidified nitric acid is 4molL -1 , in the organic phase, the volume fraction of TBP is 60%, the volume fraction of ionic liquid is 0%, and the acidity of feed liquid is 5molL -1 , the concentration of zirconium and hafnium is 1.5molL -1 . The specific operation method is similar to that of Example 1, the only difference is that the acidified organic phase is 2:1 compared with the feed liquid, and the number of extraction stages is 15 to obtain nuclear-grade zirconium dioxide and hafnium oxide, and the recovery rate of zirconium is greater than 90% %.

Embodiment 3

[0052] A method similar to that of Example 1 was used to prepare acid solutions, feed solutions and organic phases with different concentrations. The concentration of acidified nitric acid is 3molL -1 , in the organic phase, the volume fraction of TBP is 50%, the volume fraction of ionic liquid is 5%, and the acidity of feed liquid is 4molL -1 , the concentration of zirconium and hafnium is 0.5molL -1 . The specific operation method is similar to that of Example 1, the only difference is that the acidified organic phase is 1:1 compared with the feed liquid, and the number of extraction stages is 6 to obtain nuclear-grade zirconium dioxide and hafnium oxide, and the recovery rate of zirconium is greater than 90% %.

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Abstract

The invention discloses a process for preparing nuclear-grade hafnium oxide and zirconium oxide through solvent extractive separation of zirconium and hafnium. The process comprises the following steps: (1) mixing tributyl phosphate or tributyl phosphate and ionic liquid, which serve as extractants, and kerosene, which serves as a diluent, so as to prepare an organic phase; and then, mixing the organic phase with nitric acid, and carrying out countercurrent acidification in a centrifugal extractor; (2) adding zirconium oxychloride, which serves as a raw material, into deionized water, carryingout dissolving, and then, adding hydrochloric acid and nitric acid into the solution, so as to prepare a feed solution containing zirconium and hafnium; (3) carrying out countercurrent extraction onthe acidified organic phase and the feed solution containing zirconium and hafnium, prepared in the step (2), in a centrifugal extractor; (4) carrying out back-extraction on a zirconium-containing organic phase with water, then, carrying out hydrolysis, and carrying out calcination, so as to obtain nuclear-grade zirconium oxide; and (5) enriching hafnium-containing raffinate with P204, then, carrying out back-extraction, carrying out hydrolysis, and carrying out calcination, so as to obtain nuclear-grade hafnium oxide. According to the process, the problems, i.e., complicated process, much waste liquid and environmental pollution in the prior art are solved, and the production efficiency is increased.

Description

technical field [0001] The invention belongs to the technical field of chemistry, in particular to a process for preparing nuclear-grade hafnium oxide and zirconium oxide by solvent extraction and separation of zirconium and hafnium. Background technique [0002] Zirconium and hafnium are widely used in aerospace, semiconductor, optical coating, hard alloy, chemical industry and other fields, and are the core materials of nuclear industry. With the rapid development of my country's nuclear power and nuclear military industry, the amount of zirconium and hafnium materials is increasing, and the amount of zirconium, hafnium and alloy products for civil use is also increasing, and the varieties are increasing. Therefore, it is very important to solve the supply problem of zirconium and hafnium raw materials. [0003] The separation technology of zirconium and hafnium is the key to the preparation of nuclear grade zirconium and hafnium. The technologies that have been industria...

Claims

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Application Information

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IPC IPC(8): C01G27/02C01G25/02B01D11/02
CPCB01D11/0288C01G25/02C01G27/02
Inventor 顾群群陈怀浩
Owner NANJING YOUTIAN METAL TECH
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