Preparation method for atomic energy level hafnium dioxide

A hafnium dioxide, atomic energy level technology, applied in the field of wet zirconium hafnium metallurgy, can solve the problems of high cost of atomic energy level hafnium dioxide, unstable product quality, large amount of waste water, etc., and achieve obvious social and economic benefits, waste water The effect of reducing the amount of caustic soda and reducing the consumption of caustic soda

Inactive Publication Date: 2020-04-17
中核二七二铀业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a preparation method of atomic level hafnium dioxide, which mainly solves the shortcomings of high cost, la

Method used

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Examples

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preparation example Construction

[0047] A method for preparing atomic-level hafnium dioxide, the process comprising the following steps:

[0048] Step 1, preparation of hafnium extraction stock solution:

[0049] Using industrial zirconium oxychloride as raw material, add water to dissolve according to the set liquid-solid ratio;

[0050] After complete dissolution, precipitate with industrial liquid alkali to prepare a mixture slurry of zirconium hydroxide and hafnium hydroxide;

[0051] The mixture slurry is filtered, and the filter cake is pulped and washed with water;

[0052] The aqueous slurry is filtered, and the filter cake is again washed with water for pulping. After 5 to 6 times of pulping and washing, the chloride ion in the washing water is less than 1g / L;

[0053] The filter cake obtained by filtering the last washing slurry is dissolved with 98wt.% concentrated nitric acid to make a zirconyl nitrate solution;

[0054] After the dissolution is complete, add a set amount of 98wt.% concentrated...

Embodiment 1

[0084] Dissolve 500kg of zirconium oxychloride industrial product in water, add 20% liquid caustic soda to precipitate, wash the slurry with water to remove chloride ions, then dissolve the slurry with concentrated nitric acid, adjust the acidity of the solution to prepare the original solution for the separation of zirconium and hafnium. The extracted stock solution and the organic phase containing 60% (volume concentration) tributyl phosphate are subjected to multistage countercurrent extraction in a mixing clarifier. After the separation of zirconium and hafnium, 1550 L of raffinate was obtained. The concentration of hafnium in the raffinate was 1.21 g / L, the concentration of zirconium was 0.021 g / L, and the concentration of nitric acid was 4.0 mol / L. The raffinate is the original solution enriched in hafnium.

[0085] Prepare 200L P204, 2-octanol and sulfonated kerosene in a stirring tank with a volume ratio of 10%:5%:85% organic phase.

[0086] The organic phase and dilu...

Embodiment 2

[0093] Dissolve 400kg of zirconium oxychloride industrial product in water, add 20% liquid caustic soda to precipitate, wash the slurry with water to remove chloride ions, then dissolve the slurry with concentrated nitric acid, adjust the acidity of the solution to prepare the original solution for the separation of zirconium and hafnium. The extracted stock solution and the organic phase containing 60% (volume concentration) tributyl phosphate are subjected to multistage countercurrent extraction in a mixing clarifier. After the separation of zirconium and hafnium, 1200 L of raffinate was obtained. The concentration of hafnium in the raffinate was 1.50 g / L, the concentration of zirconium was 0.032 g / L, and the concentration of nitric acid was 3.8 mol / L. The raffinate is the original solution enriched in hafnium.

[0094] Prepare 150L of P204, secondary octanol and sulfonated kerosene in a stirring tank with a volume ratio of 10%:5%:85% organic phase.

[0095] The organic pha...

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Abstract

The invention belongs to the technical field of wet-process zirconium and hafnium metallurgy, and particularly relates to a preparation method for atomic energy level hafnium dioxide. According to themethod, P204 is adopted as an extraction agent to extract and enrich hafnium in raffinate, the concentration of the hafnium in the enriched hafnium solution can be improved by 20-30 times, the consumption of caustic soda for precipitation is obviously reduced, and a precipitation mother solution can return to prepare a stripping agent; hafnium-extracted raffinate water can return to a zirconium and hafnium separation system for recycling or for producing a sodium nitrate product; the color of the produced hafnium dioxide is white, and the total impurity content conforms to the atomic energy level hafnium dioxide quality standard; and compared with direct precipitation of the raffinate, the preparation method has the advantages that the waste water amount is reduced by 60% or above, the raffinate can be recycled, the consumption of the caustic soda is reduced by 85% or above, the production cost is low, the product quality of the hafnium dioxide is stable, and obvious social benefits and obvious economic benefits are achieved.

Description

technical field [0001] The invention belongs to the technical field of wet zirconium and hafnium metallurgy, and in particular relates to a method for preparing atomic-level hafnium dioxide. Background technique [0002] The separation of zirconium and hafnium is a key step in the production process of nuclear grade sponge zirconium and atomic energy grade sponge hafnium. Under the mononitric acid system, tributyl phosphate (TBP) is used as the extractant and sulfonated kerosene is used as the diluent to form an organic phase for extraction and separation of zirconium and hafnium. Zirconium oxychloride is used as raw material to prepare zirconium (hafnium) hydroxide slurry by adding water for dissolution and adding liquid alkali for precipitation. The slurry is washed with water to remove the middle chloride ions, and then concentrated nitric acid is used to dissolve the slurry to adjust the acidity of the solution. It is prepared as an extraction stock solution for the sep...

Claims

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Application Information

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IPC IPC(8): C22B34/14C22B3/38C22B3/44
CPCC22B3/44C22B34/14C22B3/3846Y02P10/20
Inventor 孔冬成周密黄召龚道坤尹亮钟华围胡强辉王育学祝和彪肖维
Owner 中核二七二铀业有限责任公司
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