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Method for protecting melt containing anhydrous magnesium chloride and/or anhydrous rare earth chloride

A technology of anhydrous magnesium chloride and rare earth chloride, which is applied in the field of protection of melts containing anhydrous magnesium chloride and/or anhydrous rare earth chloride, can solve problems such as high corrosion, melt hydrolysis, and good sealing performance, and achieve Low sealing requirements, inhibition of hydrolysis, and cost reduction effects

Active Publication Date: 2021-07-09
河北大有镁业有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current protection method of anhydrous magnesium chloride and / or anhydrous rare earth chloride melt has the following problems: ①. The container for holding high-temperature melt needs good airtightness
However, the high-temperature chloride melt is highly corrosive, and once a gas leak occurs in the container, the anhydrous magnesium chloride and / or anhydrous rare earth chloride in the protected high-temperature melt will be hydrolyzed quickly
②. Dynamic real-time protection when melt flow cannot be realized
③. Does not have immediate self-healing properties
When the container is corroded by the highly corrosive high-temperature chloride melt and gas leaks or the surface is covered with cracks in the flux, the protective atmosphere does not have immediate self-healing properties, and the high-temperature melt is directly in contact with air, resulting in serious hydrolysis of the melt

Method used

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  • Method for protecting melt containing anhydrous magnesium chloride and/or anhydrous rare earth chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The protected melt containing anhydrous magnesium chloride and anhydrous lanthanum chloride is placed in a container, and the melt composition is KCl (45wt.%)-NaCl (25wt.%)-CaCl 2 (15wt.%)-BaCl 2 (14.7wt.%)-MgCl 2 (0.1wt.%)-LaCl 3 (0.2wt.%). The total content of anhydrous magnesium chloride and anhydrous rare earth chloride in the melt is 0.3wt.%. The container is sealed and the sealed container has a steam inlet and a steam outlet. is 0.05m, and the volume ratio of the melt and its upper space is 105. Heat the melt at 500°C and keep it warm for 5 hours at this temperature, and control the steam escape rate of the sealed container to 3L / min, so that the total vapor partial pressure of anhydrous magnesium chloride and anhydrous rare earth chloride in the protective atmosphere accounts for The vapor partial pressure is 0.2%, and the total chloride vapor partial pressure accounts for 20% of the total pressure of the protective atmosphere. The escaped chlorinated mixtu...

Embodiment 2

[0051] The protected melt containing anhydrous magnesium chloride and anhydrous cerium chloride is placed in a container, and the melt composition is KCl (45wt.%)-NaCl (25wt.%)-CaCl 2 (15wt.%)-BaCl 2 (14.5wt.%)-MgCl 2 (0.4wt.%)-CeCl 3 (0.1wt.%). The total content of anhydrous magnesium chloride and anhydrous rare earth chloride in the melt is 0.5wt.%, the container is sealed and the sealed container has a steam outlet, the gas pressure in the sealed container is equal to 1.0atm, and the height of the upper space of the melt is 0.1m , the volume ratio of the melt to its upper space is 95. Heat the melt at 700°C and keep it warm at this temperature for 5 hours, control the steam escape rate of the sealed container to 5L / min and the gas volume and composition of the steam inlet, so that the anhydrous magnesium chloride and anhydrous rare earth chloride vapor in the protective atmosphere The sum of the partial pressures accounts for 1.0% of the partial pressure of the total ch...

Embodiment 3

[0055] The protected melt containing anhydrous magnesium chloride and anhydrous praseodymium chloride is placed in a container, and the melt composition is KCl (45wt.%)-NaCl (25wt.%)-CaCl 2 (15wt.%)-BaCl 2 (10.0wt.%)-MgCl 2 (4.0wt.%)-PrCl 3(1.0wt.%). The total content of anhydrous magnesium chloride and anhydrous rare earth chloride in the melt is 5.0wt.%. The container is sealed and the sealed container has a steam outlet and a steam inlet. The gas pressure in the sealed container is equal to 2.0 atm, and the height of the upper space of the melt is is 3m, and the volume ratio of the melt and its upper space is 0.5. Heat the melt at 1100°C and keep it warm at this temperature for 10 hours, control the steam escape rate of the sealed container to 10L / min and the gas volume and composition of the steam inlet, so that the anhydrous magnesium chloride and anhydrous rare earth chloride vapor in the protective atmosphere The sum of the partial pressures accounts for 10% of the ...

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Abstract

The invention discloses a method for protecting a melt containing anhydrous magnesium chloride and / or anhydrous rare earth chloride, comprising the following steps: S1, placing the protected melt containing anhydrous magnesium chloride and / or anhydrous rare earth chloride in a container, and sealing the container to keep the height of the upper space of the melt and the volume ratio of the melt to the upper space of the melt; S2, heating the protected melt containing anhydrous magnesium chloride and / or anhydrous rare earth chloride, and forming a protective atmosphere in the upper space of the melt; and S3, controlling the speed of the protective atmosphere escaping from the container to realize protection of the melt containing anhydrous magnesium chloride and / or anhydrous rare earth chloride. By means of the method, the high-temperature melt can be continuously protected under a relatively simple technological condition to restrain hydrolysis, so that the requirement for the sealing performance of equipment is low, dynamic real-time protection can be achieved when the melt flows, and high purity of the high-temperature melt is guaranteed through self-generation and self-repairing of the protective atmosphere.

Description

technical field [0001] The invention relates to a method for protecting a melt, in particular to a method for protecting a melt containing anhydrous magnesium chloride and / or anhydrous rare earth chloride. Background technique [0002] The melt containing anhydrous magnesium chloride and / or anhydrous rare earth chloride can be used as raw material for electrolytic preparation of metal magnesium or rare earth magnesium alloy, and can also be used as raw material for preparation of rare earth magnesium alloy by molten salt reduction method. Important chemical raw materials. However, the high temperature anhydrous magnesium chloride and / or anhydrous rare earth chloride in the melt easily reacts with water vapor and oxygen in the air to generate hydrolysis products that seriously affect the electrolysis or reduction process. When the electrolytic method is used to prepare metal magnesium or magnesium alloy, when the mass ratio of the hydrolyzate to the corresponding anhydrous c...

Claims

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Application Information

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IPC IPC(8): C25C3/04C22B26/22C22B5/02C22B9/00
CPCC25C3/04C22B26/22C22B5/02C22B9/00
Inventor 卢旭晨张志敏闫岩王天华薛立强李金沙
Owner 河北大有镁业有限责任公司
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