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A preparation method of chloride composite electrolyte for molten salt electrolysis

A technology of composite electrolyte and molten salt electrolysis, which is applied in the field of preparation of chloride composite electrolyte for molten salt electrolysis, can solve the problems of non-continuous electrolysis, high cost, difficult control, etc., and achieve the solution of continuous addition of volatile and chloride raw materials , stable chemical composition, low vapor pressure effect

Active Publication Date: 2017-03-15
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

During the electrolysis process, metal chlorides are easy to volatilize, resulting in too low concentration of valuable metal ions in the electrolyte. At the same time, it is difficult to add metal chlorides to the electrolytic cell. The volatilization causes blockage of the evacuation tube and argon inlet of the equipment, resulting in the failure of electrolysis. Continuously
[0006] At present, the preparation of chloride compound salt in the laboratory mainly adopts the method of installing metal chloride and alkali metal chloride at both ends of the quartz glass tube respectively, melting and sealing the quartz glass tube, and heating the two ends respectively to volatilize the metal chloride and the alkali at the other end. Metal chloride reaction, the reaction cannot be produced continuously and is not easy to control, each experiment needs to destroy the quartz tube, the cost is high

Method used

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preparation example Construction

[0029] The preparation method of the chloride composite electrolyte for molten salt electrolysis or refining of the present invention comprises the following steps:

[0030] (1) One or several alkali metal chlorides ACl (A=Li, Na, K, Rb, Cs, etc.) and / or alkaline earth metal chlorides BCl in a certain molar ratio 2 (B=Be, Mg, Ca, Sr, Ba) is heated and melted, and after cooling, it is broken into fine particles with a particle size of 5-10mm and stored in a dry dish for later use.

[0031] (2) Put the lower crucible at the bottom of the reaction tank, put the broken alkali metal or alkaline earth metal chloride prepared in step (1) into the middle crucible with fine holes at the bottom, and put the refractory metal chloride into Inside the upper crucible. The reaction tank is placed in a two-stage temperature-controlled resistance furnace. There are upper, middle and lower crucibles in the reaction tank, and the bottom of the middle crucible is densely covered with pores.

[...

Embodiment 1

[0037] The analytically pure NaCl-KCl with an equimolar ratio is heated and melted in a reaction tank, cooled and broken into solid particles with a particle size of 5-10mm, and put into a drying dish for later use. Put the lower crucible, middle crucible and upper crucible in the reaction tank in turn, the lower crucible is used to hold the final composite electrolyte, and the middle crucible is filled with the prepared NaCl-KCl molten salt electrolyte with an equimolar ratio of 5-10mm in particle size , put the purified TiCl into the upper crucible 4 .

[0038] After the canning is completed, vacuumize, then fill with argon to a slight positive pressure, heat to 120°C in an argon atmosphere, and conduct heat preservation and dehydration for 2 hours in an argon flowing atmosphere, then vacuumize and fill with argon Maintain slight positive pressure.

[0039] Increase the temperature of the upper crucible and the middle crucible by segmented temperature control to keep the t...

Embodiment 2

[0042] The analytically pure NaCl-KCl with an equimolar ratio is heated and melted in a reaction tank, cooled and broken into solid particles with a particle size of 5-10mm, and put into a drying dish for later use. Put the lower crucible, middle crucible and upper crucible in the reaction tank in turn, the lower crucible is used to hold the final composite electrolyte, and the middle crucible is filled with the prepared NaCl-KCl molten salt electrolyte with an equimolar ratio of 5-10mm in particle size , put dry ZrCl in the upper crucible 4 powder.

[0043] After the canning is completed, vacuumize, then fill with argon to a slight positive pressure, heat to 250°C in an argon atmosphere, and conduct heat preservation and dehydration for 2 hours in an argon flowing atmosphere, then vacuumize and fill with argon Maintain slight positive pressure.

[0044] Increase the temperature of the upper crucible and the middle crucible by segmented temperature control to keep the temper...

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Abstract

The invention relates to a preparation method of a chloride composite electrolyte used for molten salt electrolysis. The preparation method comprises following steps: a refractory metal chloride is subjected to heating sublimation so as to obtain a gas material; the gas material is reacted with a granular solid alkali metal and / or a alkaline earth chloride so as to obtain a A2MCl6 type compound and / or a BMC16 type compound, wherein A is used for representing the alkali metal, B is used for representing the alkaline earth metal, and M is used for representing the refractory metal; the A2MCl6 type compound and / or the BMC16 type compound is reacted with the solid alkali metal and / or the alkaline earth chloride particles further so as to obtain a composite electrolyte with a low eutectic point, wherein reaction temperature is controlled, and the obtained composite electrolyte is in liquid states; and the composite electrolyte is separated from the solid alkali metal or the alkaline earth chloride particles, and is dropwise collected under the effect of gravity. Operation of the preparation method is simple and safe; chemical composition of the obtained product is stable; automatic separation of the product from the raw materials can be realized; continuous operation can be realized; and problems of volatilization of chloride electrolytes used for chloride system molten salt electrolysis or refractory metal refining, and raw material continuous adding are solved.

Description

technical field [0001] The invention relates to a preparation method of a chloride composite electrolyte for molten salt electrolysis. The electrolyte is mainly used for molten salt electrolytic reduction and refining refractory metals, and belongs to the technical field of electrochemical metallurgy. Background technique [0002] Molten salt electrolysis is an important method for purifying refractory metals, especially for the preparation of high-purity 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 materials and control materials for nuclear reactors due to their own nuclear properties. With the pollution of the environment by traditional energy sources, the demand for nuclear power as a clean energy source increases, and the demand for zirconium and hafnium materials is also incr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C3/26
CPCC25C3/26
Inventor 吴延科王力军陈松柳旭罗远辉李国勋陈洋张建东
Owner 有研资源环境技术研究院(北京)有限公司
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