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Method for enriching hafnium tetrachloride by taking crude zirconium tetrachloride as raw material

A technology for enriching hafnium tetrachloride and crude zirconium tetrachloride is applied in the direction of zirconium halide, process efficiency improvement, etc., and can solve the problems of no development of extraction and enrichment of hafnium, low production capacity, large construction investment, etc. Meet the various needs of the market, improve the quality and grades, and improve the effect of economic benefits

Active Publication Date: 2021-01-12
锦州中特电炉有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the main problems in these two production technologies for the separation of zirconium and hafnium are: (1) the symbiosis of zirconium and hafnium resources, the content of hafnium in zirconium is usually between 0.75-2.0%, due to the low content of hafnium, it is necessary to use symbiotic zirconium and hafnium To extract hafnium from hafnium, a large amount of zirconium and hafnium must be separated, and the processing capacity is large
(2) The extraction equipment is huge, the production capacity is low, and the cost is high
(3) The above two kinds of zirconium and hafnium separation processes have long process flow, huge equipment and large construction investment
(4) The loading capacity of the organic solvent for extraction and separation is low, the concentration of the prepared material liquid is low, and the amount of organic extractant is large, and the waste liquid generated by the regeneration treatment of the organic extractant is difficult to treat
(5) The concentration of the solution obtained after the separation of zirconium and hafnium is low, and the multi-processing energy consumption of the mother liquor produced by precipitation separation is high
(6) Existing enterprises producing industrial zirconium have not developed the technology for extracting and enriching hafnium

Method used

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  • Method for enriching hafnium tetrachloride by taking crude zirconium tetrachloride as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Extract primary hafnium-rich zirconium tetrachloride raw material

[0025] a. Ingredients: first, KCl and NaCl are mixed according to the molar ratio of 1:1 to prepare alkali metal chloride; then thick zirconium tetrachloride and alkali metal chloride are mixed according to the mass ratio of 85:15;

[0026] b. Molten salt chlorination: Add the mixed salt of crude zirconium tetrachloride and alkali metal chloride salt into the molten salt crucible with stirring, start the power supply of the molten salt heating furnace, heat and stir to melt the mixed salt; Atmospheric pressure control 220°C-250°C;

[0027] c. Extract primary hafnium-rich zirconium tetrachloride: control the appropriate temperature to volatilize zirconium tetrachloride and hafnium tetrachloride in the molten mixed salt in the molten salt crucible, and drive away hydrochloric acid gas and silicon tetrachloride in the gas phase, and enter together A condenser with a water-cooled jacket condenses; ther...

Embodiment 2

[0036] (1) Extract primary hafnium-rich zirconium tetrachloride raw material

[0037]a. Ingredients: first, KCl and NaCl are mixed according to the molar ratio of 1:2 to prepare alkali metal chloride; then thick zirconium tetrachloride and alkali metal chloride are mixed according to the mass ratio of 65:35;

[0038] b. Molten salt chlorination: Add the mixed salt of crude zirconium tetrachloride and alkali metal chloride salt into the molten salt crucible with agitation one after another, start the power supply of the molten salt heating furnace, and heat the mixed salt to melt; Control 320°C-350°C;

[0039] c. Extract primary hafnium-rich zirconium tetrachloride: control the appropriate temperature to volatilize zirconium tetrachloride and hafnium tetrachloride in the molten mixed salt in the molten salt crucible, and drive away hydrochloric acid gas and silicon tetrachloride in the gas phase, and enter together The condenser condenses; therefore when P HfCL4> P ZrCL4 And...

Embodiment 3

[0048] (1) Extract primary hafnium-rich zirconium tetrachloride raw material

[0049] a. Ingredients: first, KCl and NaCl are mixed according to the molar ratio of 1:1 to prepare alkali metal chloride; then thick zirconium tetrachloride and alkali metal chloride are mixed according to the mass ratio of 85:15;

[0050] b. Molten salt chlorination: Add the mixed salt of crude zirconium tetrachloride and alkali metal chloride salt into the molten salt crucible with agitation one after another, start the power supply of the molten salt heating furnace, and heat the mixed salt to melt; Control 270°C-290°C;

[0051] c. Extract primary hafnium-rich zirconium tetrachloride: control the appropriate temperature to volatilize zirconium tetrachloride and hafnium tetrachloride in the molten mixed salt in the molten salt crucible, and drive away hydrochloric acid gas and silicon tetrachloride in the gas phase, and enter together The condenser condenses; therefore when P HfCL4 >P ZrCL4 An...

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Abstract

The invention relates to a method for enriching hafnium tetrachloride by taking crude zirconium tetrachloride as a raw material. The method comprises the following steps: sequentially adding mixed salt of crude zirconium tetrachloride and alkali metal chlorate into a molten salt crucible with a stirring function, and preparing primary hafnium-rich zirconium tetrachloride; taking the primary hafnium-rich zirconium tetrachloride as a raw material, and enriching hafnium tetrachloride through single-stage molten salt separation equipment for multiple times to obtain hafnium-rich zirconium tetrachloride containing not less than 30% of hafnium tetrachloride. The method has the advantages of mature process, simple equipment, high treatment capacity, high hafnium extraction rate, high yield, low investment and low cost. On the premise of not changing the main process flow for producing industrial zirconium, only the molten salt purification procedure is properly changed to extract zirconium tetrachloride containing 30% or more of hafnium tetrachloride from crude zirconium tetrachloride, thereby creating conditions for further carrying out zirconium-hafnium separation to produce sponge hafnium; and the hafnium resource in the crude zirconium tetrachloride is recycled. Compared with the existing process for extracting and separating zirconium and hafnium, the method has the characteristics of energy conservation and emission reduction, and meets the development requirements of circular economy.

Description

technical field [0001] The invention relates to a method for enriching hafnium tetrachloride by using crude zirconium tetrachloride as raw material. Background technique [0002] Hafnium is an important rare metal with a high melting point. It has broad application space in emerging electronic materials, graphite purification, ceramic materials, national defense and military industries. Due to its scarcity and low production in China, it cannot meet market demand. Zirconium and hafnium co-growth, the zircon sand that can be separated from zirconium and hafnium in the application only accounts for 0.7% of the total consumption, and the rest of the products that consume zircon sand cannot extract hafnium due to the production process. my country consumes zircon sand (in ZrO 2 65% total) 650,000 tons, accounting for the first place in the world, a large amount of symbiotic hafnium is wasted in vain. [0003] At present, only factories specializing in the production of nuclear-...

Claims

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Application Information

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IPC IPC(8): C01G27/04C01G25/04
CPCC01G27/04C01G25/04C01P2006/80Y02P10/20
Inventor 刘长河薛庆山
Owner 锦州中特电炉有限公司
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