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Method for treating molten salt electrolysis cathode deposits through pyrogenic process

A molten salt electrolysis and pyroprocessing technology, applied in the field of electrochemical metallurgy, can solve the problems of waste of resources and energy, unsuitable for continuous production, increase of procedures and production costs, etc., to reduce processing costs, improve theoretical significance and application Value, the effect of avoiding waste of resources and energy

Active Publication Date: 2017-05-24
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of wet process to treat cathode deposits causes a waste of resources and energy in the separation of hafnium powder and recovery of hafnium elements, increases the process and production costs, and is not suitable for continuous production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Cathodic deposits (including metal hafnium and hafnium low-valent compounds and bonded molten salt electrolytes) obtained by electrolysis and electrorefining of hafnium by pyrolysis, using the following steps:

[0025] (1) The cathode deposit obtained by electrolysis and electrolytic refining of hafnium is broken into particles with a particle size of 2 to 5 mm and mixed with NaCl-KCl-NaF electrolyte in an equimolar ratio, and the content of the cathode deposit is 20% to 30% (mass ratio), and then loaded into a ceramic crucible with a porosity of 70-90%.

[0026] (2) Put the ceramic crucible into the vacuum melting filter tank. After the canning is completed, vacuumize and heat slowly at a heating rate of 5-8°C / min until the pressure reaches -3 Pa, stop vacuuming, and continue to heat up to 700-750°C to keep warm.

[0027] (3) After 30 to 50 minutes of heat preservation, fill the upper part of the equipment with argon to maintain a slight positive pressure of 200 to 40...

Embodiment 2

[0030] The cathodic deposit obtained by pyrolysis and electrolytic refining of zirconium (including metal zirconium and low-valent compounds of zirconium and bonded molten salt electrolyte) adopts the following steps:

[0031](1) The cathode deposit obtained by electrolysis and electrolytic refining of zirconium is broken into particles with a particle size of 2 to 5 mm and mixed with NaCl-KCl-NaF electrolyte in an equimolar ratio, and the content of the cathode deposit is 20% to 30% (mass ratio), and then loaded into a ceramic crucible with a porosity of 70-90%.

[0032] (2) Put the ceramic crucible into the vacuum melting filter tank. After the canning is completed, vacuumize and heat slowly at a heating rate of 5-8°C / min until the pressure reaches -3 Pa, stop vacuuming, and continue to heat up to 700-750°C to keep warm.

[0033] (3) After 30 to 50 minutes of heat preservation, fill the upper part of the equipment with argon to maintain a slight positive pressure of 200 to ...

Embodiment 3

[0036] The cathodic deposit obtained by pyrolysis and electrolytic refining of titanium (including metal titanium and titanium low-valent compounds and bonded molten salt electrolyte) adopts the following steps:

[0037] (1) The cathode deposit obtained by electrolysis and electrolytic refining titanium is broken into particles with a particle size of 2 to 5 mm and mixed with NaCl-KCl-NaF electrolyte in an equimolar ratio, and the content of the cathode deposit is 20% to 30% (mass ratio), and then loaded into a ceramic crucible with a porosity of 70-90%.

[0038] (2) Put the ceramic crucible into the vacuum melting filter tank. After the canning is completed, vacuumize and heat slowly at a heating rate of 5-8°C / min until the pressure reaches -3 Pa, stop vacuuming, and continue to heat up to 700-750°C to keep warm.

[0039] (3) After 30 to 50 minutes of heat preservation, fill the upper part of the equipment with argon to maintain a slight positive pressure of 200 to 400 Pa hi...

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Abstract

The invention relates to a method for treating molten salt electrolysis cathode deposits through a pyrogenic process, and belongs to the technical field of electrochemical metallurgy. The method comprises the following steps of: firstly, crushing cathode deposits obtained by molten salt electrolysis, mixing the cathode deposits with a mixture of alkali metal chloride and alkali metal fluoride, and putting the mixture into a ceramic crucible, wherein a molar ratio of the cathode deposits is equal to that of the mixture; putting the ceramic crucible into a vacuum melting filtering tank, starting vacuum-pumping, heating, stopping vacuum-pumping when pressure is lower than 1-10<-3>Pa, stopping vacuum-pumping, continuously heating to 700-750 DEG C, and preserving heat; after preserving heat, charging argon gas, keeping micro positive pressure, melting molten salt electrolyte mixed up with the deposits, and dripping the molten salt electrolyte under a gravity condition; and collecting dripped molten salt electrolyte into a lower crucible, keeping metal in the ceramic crucible, taking out metal after cooling, and returning the collected molten salt electrolyte to an electrolysis process for use. The method is simple and safe to operate, guarantees continuous production processes through recycled electrolyte, reduces production cost, and has a relatively high application value and relatively good theoretical significance.

Description

technical field [0001] The invention relates to a method for treating cathode deposits of molten salt electrolysis by fire method, the method is mainly used for treating cathode deposits of molten salt electrolytic reduction and refining refractory metals, removing molten salt electrolyte mixed in cathode deposits, and obtaining The method of depositing metal on the cathode and returning the separated electrolyte to the electrolysis process for recycling belongs to the technical field of electrochemical metallurgy. Background technique [0002] Molten salt electrolysis and molten salt electrolytic refining are important methods for the preparation and purification of rare high-melting point metals, especially for the preparation of titanium, zirconium, and hafnium. High-purity titanium is mainly used in high-tech fields such as large-scale integrated circuits, aerospace, and medical alloys. Metal zirconium and hafnium are respectively used as the most ideal structural mater...

Claims

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Application Information

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IPC IPC(8): C25C7/06
Inventor 吴延科陈松王力军蔡振平陈洋
Owner 有研资源环境技术研究院(北京)有限公司
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