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 ox

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
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Example Embodiment

[0041] Example 1

[0042] (1) Prepare 3molL -1 Acidified nitric acid solution: Take 5L concentrated nitric acid solution into 20L deionized water, stir and mix well. To prepare an organic phase containing 40% TBP and 10% ionic liquid: take 10L TBP, 2.5L ionic liquid and 12.5L kerosene and mix them evenly. Prepare 1molL -1 Material liquid: take 6.45Kg of zirconium oxychloride, add deionized water to dissolve, add hydrochloric acid and nitric acid to make the solution acidity 4molL -1 , The final volume is 20L. Prepare 10% P204 organic phase: take 0.8L P204 and 7.2L kerosene and mix well. Prepare 1.6L stripping solution: take 320g of ammonium bicarbonate and dissolve 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 countercurrent acidification is performed in a centrifugal extractor. The organic phase pretreatment has 3 stages.

[0044] (3) The acidified organic phase and the feed...

Example Embodiment

[0049] Example 2

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

Example Embodiment

[0051] Example 3

[0052] A method similar to Example 1 was used to prepare acid solutions of different concentrations, feed liquids and organic phases. The acidified nitric acid concentration 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 the feed solution is 4molL -1 , The concentration of zirconium and hafnium is 0.5molL -1 . The specific operation method is similar to Example 1, the only difference is that the acidified organic phase is 1:1 compared with the feed liquid, and the extraction level is 6 stages to obtain nuclear grade zirconium dioxide and hafnium oxide. 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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