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Method for preparing high-purity hafnium dioxide

The technology of hafnium dioxide and hafnium oxide is applied in the field of zirconium and hafnium hydrometallurgy, which can solve the problems of increasing treatment costs, and achieve the effect of reducing the amount of waste water, obvious social and economic benefits, and reducing the amount of waste water.

Pending Publication Date: 2021-04-23
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

[0003] The conventional treatment method is to add this part of hydrated hafnium oxide with high zirconium content in batches to tributyl phosphate to extract and separate zirconium and hafnium. Although the materials are recovered, the processing cost is increased.

Method used

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  • Method for preparing high-purity hafnium dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Step 1, preparation of extraction stock solution:

[0062] Dissolve the unqualified hydrated hafnium oxide slurry in the production process of zirconium and hafnium separation with 98% concentrated nitric acid. After the dissolution is complete, add 98% nitric acid, industrial grade sodium nitrate and industrial water to prepare an extraction stock solution with a hafnium concentration of 20 ~45g / L, the concentration of zirconium is 0.6g / L~10g / L, m(ZrO 2 ) / m(ZrO 2 +HfO 2 )>3%, the concentration of nitric acid is 2.5-4.0 mol / L, and the concentration of sodium nitrate is 2.5-3.5 mol / L.

[0063] Step 2, organic phase preparation:

[0064] Tributyl phosphate and sulfonated kerosene are mixed to prepare an organic phase with a volume concentration of 55%-61% of tributyl phosphate.

[0065] Step 3, organic phase acidification:

[0066] In step 2, the organic phase and 5.8-6.2 mol / L dilute nitric acid solution are subjected to two-stage countercurrent acidification at roo...

Embodiment 2

[0078] Dissolve 15kg of unqualified hydrated hafnium oxide slurry with 98% concentrated nitric acid. After the dissolution is complete, add 98% nitric acid, industrial grade sodium nitrate and industrial water to prepare a hafnium concentration of 25g / L and a zirconium concentration of 1.1g / L. 60L of extraction stock solution with a concentration of nitric acid of 2.7mol / L and a concentration of sodium nitrate of 3.5mol / L.

[0079] TBP and sulfonated kerosene were used to prepare 60 L of an organic phase with a volume concentration of TBP of 55%.

[0080] The organic phase and 6.0mol / L dilute nitric acid solution are subjected to two-stage countercurrent acidification in a controlled mixing clarifier at room temperature according to the volume ratio V(O) / V(A)=1:1.

[0081] The acidified organic phase and the extraction stock solution are subjected to 6-stage countercurrent extraction at room temperature in a controlled mixing clarifier according to the volume ratio V(O) / V(A)=1...

Embodiment 3

[0087] Dissolve 30kg of unqualified hydrated hafnium oxide slurry with 98% concentrated nitric acid. After the dissolution is complete, add 98% nitric acid, industrial grade sodium nitrate and industrial water to prepare a hafnium concentration of 44g / L and a zirconium concentration of 9.6g / L. , 68L of extraction stock solution with nitric acid concentration of 3.0mol / L and sodium nitrate concentration of 3.0mol / L.

[0088] TBP and sulfonated kerosene were used to prepare 70 L of an organic phase with a volume concentration of TBP of 61%.

[0089] The organic phase and 5.8mol / L dilute nitric acid solution are subjected to two-stage countercurrent acidification in a controlled mixing clarifier at room temperature according to the volume ratio V(O) / V(A)=1:1.

[0090] The acidified organic phase and the extraction stock solution are subjected to 7-stage countercurrent extraction at room temperature in a controlled mixing clarifier according to the volume ratio V(O) / V(A)=1.5:1, an...

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Abstract

The invention provides a method for preparing high-purity hafnium dioxide, which comprises the following steps of: dissolving hydrated hafnium oxide serving as a raw material in nitric acid to prepare an extraction stock solution; carrying out multi-stage counter-current extraction on the extraction stock solution by taking tributyl phosphate as an extracting agent, extracting zirconium in the extraction stock solution into an organic phase, and leaving hafnium in a water phase to obtain a high-purity hafnium nitrate acyl solution with low zirconium content; and enabling the solution to be subjected to alkalifying precipitation, washing, microwave drying and calcining to obtain high-purity hafnium dioxide which can be used as a laser coating material. Compared with a conventional process, the method has the advantages that the concentration of hafnium in the hafnium nitrate acyl solution can be increased by 15-30 times, hafnium enrichment is not needed, and consumption of organic solvents such as P204, sec-octyl alcohol and kerosene and nitric acid is reduced; alkali is directly added into the hafnium nitrate acyl solution for precipitation, and the wastewater amount is reduced by 90% or above; and the zirconium content in the prepared hafnium dioxide is lower than 0.3%, which is superior to the quality standard of nuclear-grade hafnium oxide, the added value of the product is higher, and the method has obvious social and economic benefits.

Description

technical field [0001] The invention belongs to the technical field of zirconium and hafnium hydrometallurgy, and in particular relates to a method for preparing high-purity 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. In the actual production process of tributyl phosphate (TBP) extraction and separation of zirconium and hafnium, if the process control is abnormal or the production line is stopped for a long time after starting the separation and extraction equipment for zirconium and hafnium, some hydrated hafnium oxide with zirconium content higher than 3% in hafnium will be produced, reaching Less than nuclear level requirements. [0003] The conventional treatment method is to add this part of hydrated hafnium oxide with high zirconium content in batches to tributyl phosphate to extract and separate zirconium and haf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G27/02C22B34/14C22B3/38C22B3/44
CPCY02P10/20
Inventor 孔冬成黄召尹亮祝和彪王育学肖维乔深钟华围成冬林呼强辉罗文辉
Owner 中核二七二铀业有限责任公司
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