Method for preparing high-purity rubidium by one-step thermal reduction of metallic calcium

A metal calcium, high-purity technology is applied in the field of one-step heating reduction to prepare high-purity rubidium, which can solve the problems of inability to complete continuous operation, continuous production, and difficult cleaning of pipelines, and achieve a simple and easy purification process, low cost, and convenient cleaning. Effect

Active Publication Date: 2018-11-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN107164641A introduces a method for preparing high-purity rubidium and cesium metal. This patent uses an environment of pressurized inert gas (the pressure of the inert gas is 0.4-0.5MPa) to prepare high-purity rubidium. This method requires the preparation equipment to be able to withstand high temperatures High pressure, so this method has potential safety hazards, it is not suitable for industrial promotion, and the investment is huge
In addition, the patent is characterized by the use of a box-type resistance furnace, and the tube wall is S-shaped, which makes the method involved in the patent complicated to operate in the actual production process, difficult to clean the pipeline, and cannot be continuously produced
Patent CN105063375A introduces a method for preparing high-purity rubidium and cesium metal by vacuum thermal reduction. This method adopts a metal thermal reduction method in a vacuum environment. The operation process is cumbersome, impractical, and inconvenient
Another disadvantage of the above patents involving the preparation method is that the above methods are all single-furnace and cannot complete continuous operations.

Method used

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  • Method for preparing high-purity rubidium by one-step thermal reduction of metallic calcium
  • Method for preparing high-purity rubidium by one-step thermal reduction of metallic calcium
  • Method for preparing high-purity rubidium by one-step thermal reduction of metallic calcium

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Take 50 grams of rubidium chloride powder (99.5%, white) and 50 grams of metal calcium particles (99.9%, average particle size ~5mm, silver white), mix them evenly, put them in a stainless steel pan, put them in a horizontal vacuum electric furnace, and heat Control the vacuum degree in the furnace to 0.01Pa before, pour in inert gas such as argon to normal pressure, then vacuum, and then purge the inert gas, and repeat the vacuum + inert gas to replace the oxygen in the horizontal vacuum electric furnace 3 times Above, the material was then heated to 750°C for 60 minutes under normal pressure in an inert atmosphere. The pressure did not change significantly during the entire reaction. The liquid metal rubidium was collected in a jar filled with liquid paraffin, and no liquid metal flowed out. After the heat preservation is over, turn off the heating device and open the furnace cover when the furnace temperature is cooled to room temperature. White powder is covering the ...

Embodiment 2

[0054] Take 50 grams of rubidium chloride powder (99.5%, white) and 50 grams of metal calcium particles (99.9%, average particle size ~5mm, silver white), mix them evenly, put them in a stainless steel pan, put them in a horizontal vacuum electric furnace, and heat Control the vacuum degree in the furnace to 0.01Pa before, pour in inert gas such as argon to normal pressure, then vacuum, and then purge the inert gas, and repeat the vacuum + inert gas to replace the oxygen in the horizontal vacuum electric furnace 3 times Above, the material is then heated to 850℃ for 120min under normal pressure in an inert atmosphere. The air pressure changes significantly during the whole reaction. Liquid metal rubidium can be collected with a jar filled with liquid paraffin. It is estimated that the metal rubidium is about 25 grams , The straight recovery rate of metal rubidium is 71.43%.

Embodiment 3

[0060] Take 50 grams of rubidium chloride powder (99.5%, white) and 25 grams of metal calcium particles (99.9%, average particle size ~5mm, silver white), mix them evenly, put them in a stainless steel pan, put them in a horizontal vacuum electric furnace, and heat Control the vacuum degree in the furnace to 0.01Pa before, pour in inert gas such as argon to normal pressure, then vacuum, and then purge the inert gas, and repeat the vacuum + inert gas to replace the oxygen in the horizontal vacuum electric furnace 3 times Above, the material is then heated to 850℃ for 60 minutes under normal pressure in an inert atmosphere. The pressure changes significantly during the reaction. A jar filled with liquid paraffin can be used to collect liquid metal rubidium. It is estimated that the metal rubidium is about 12 grams , The straight yield of rubidium metal is 34.29%.

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Abstract

The invention discloses a method for preparing high-purity rubidium by one-step thermal reduction of metallic calcium. According to the method, metallic calcium particles with the purity being greaterthan 95% and rubidium chloride powder with the purity being 98.0-99.9 are adopted as raw materials, and the method comprises the steps of mixing the metallic calcium particles and the rubidium chloride powder, and putting the obtained mixture in a horizontal vacuum electric furnace, heating to 842-1390 DEG C under the inert atmosphere for carrying out a thermal reduction replacement reaction, guiding metallic rubidium steam to a condensing part by a heated straight-through type pipe under the vacuum suction force, enabling liquid drops formed by condensing of the metallic rubidium steam to flow into a collector, thus obtaining the liquid-state metallic rubidium with the purity being 99.50-99.99%, wherein a container used is made of stainless steel. The invention provides a process for preparing high-purity rubidium by adopting a reducing metal one-step heating method, which does not require complex processes such as multiple heating reduction, electrolysis, distillation and the like,has the advantages of simple and easy purification process, low cost, green, pollution-free, safe and reliable, and is suitable for continuous industrialization. Compared with the prior art, the method has the advantages of better practicability and industrialization.

Description

Technical field [0001] The invention belongs to the field of metal purification, and specifically is a method for preparing high-purity rubidium by using calcium metal particles and rubidium chloride powder as raw materials and adopting one-step heating and reduction. Background technique [0002] Because of its unique properties, rubidium has a wide range of uses and an important position in the national economy. It plays an important role in both traditional and new application fields, especially in the high-tech field. Invention was obvious. In traditional fields, such as catalysts, special glass, electronic devices, biological materials, etc., there has been a great development in recent years. In new fields, such as rubidium atomic clock, magnetic fluid power generation, energy and other fields, it has shown strong vitality. At present, in developed countries, the proportion of rubidium used in high-tech fields reaches 80%, and the proportion of rubidium used in traditiona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B26/10C22B5/04
CPCC22B5/04C22B26/10
Inventor 袁铁锤梅方胜李瑞迪周立波
Owner CENT SOUTH UNIV
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