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Preparation method of high-purity metallic rubidium and cesium

A technology of metal rubidium and metal cesium, applied in the field of metal rubidium and cesium preparation, can solve the problems of poor separation and recovery, complicated extraction process, high cost, etc., and achieve the effect of increasing the value of by-products, simple process, and easy operation control

Active Publication Date: 2018-05-11
湖南中大技术创业孵化器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The basic raw materials for industrial production of rubidium and cesium are mainly solid ores such as cesium garnet and lepidolite, whose extraction process is complicated, costly and energy-consuming
In addition, there is no good method for separating and recovering rubidium and cesium for the mixed rubidium and cesium compounds that are mixed with rubidium and cesium

Method used

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  • Preparation method of high-purity metallic rubidium and cesium
  • Preparation method of high-purity metallic rubidium and cesium

Examples

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Effect test

Embodiment 1

[0041] A preparation method of high-purity metal rubidium, comprising the following steps:

[0042] (1) Place the sample A01 in a vacuum reactor, and dehydrate it through low-temperature preheating treatment. The dehydration temperature is controlled at 200°C for 120 minutes to obtain the pretreated compound;

[0043] (2) Material mixing: mix the pretreatment compound A01 with the reducing agent metal magnesium, calcium, and lithium according to the stoichiometric ratio of 0.75:0.95:0.04:0.01, and then mix evenly in a vacuum glove box with an argon atmosphere, press the cake and load the sample ;

[0044] (3) High-temperature reduction: Place the loading sample obtained in step (2) in a stainless copper reactor, then seal the reactor, evacuate to -0.025-0.03MPa, and then feed inert gas into the reactor. 0.45-0.50MPa, repeat this operation three times to ensure that the gas atmosphere is inert, then raise the temperature to 600°C at 5°C / min, keep the temperature for 30 minutes a...

Embodiment 2

[0048] A preparation method of high-purity metallic cesium, comprising the following steps:

[0049] (1) Place the sample A02 in a vacuum reactor and dehydrate it through low-temperature preheating treatment. The dehydration temperature is controlled at 200°C for 120 minutes to obtain the pretreated compound;

[0050] (2) Material mixing: mix the pretreatment compound A02 with the reducing agent metal magnesium, calcium, and lithium according to the stoichiometric ratio of 1.35:0.90:0.06:0.04, and then mix evenly in a vacuum glove box with an argon atmosphere, press the cake and load the sample ;

[0051] (3) High-temperature reduction: Place the loading sample obtained in step (2) in a stainless copper reactor, then seal the reactor, evacuate to -0.02-0.025MPa, and then feed inert gas into the reactor. 0.45-0.50MPa, repeat this operation three times to ensure that the gas atmosphere is inert, then raise the temperature to 300°C at 5°C / min, keep the temperature for 30 minutes...

Embodiment 3

[0055] Such as figure 1 Shown, a kind of preparation method of high-purity metallic rubidium and cesium comprises the following steps:

[0056] (1) Place the sample A03 in a vacuum reactor and dehydrate it through low-temperature preheating treatment. The dehydration temperature is controlled at 200°C for 120 minutes to obtain the pretreated compound;

[0057] (2) Material mixing: the pretreatment compound A03 and the primary reducing agent metal magnesium are proportioned according to the stoichiometric ratio of 1.55:1, and then mixed evenly in a vacuum glove box with argon atmosphere, cake pressing and sample loading;

[0058] (3) One-time high-temperature reduction: put the loaded sample obtained in step (2) in a stainless copper reactor, then seal the reactor, vacuumize to -0.025 ~ 0.03MPa, and then pass inert gas into the reactor 0.35~0.45MPa, repeat this operation three times to ensure that the gas atmosphere is inert, then raise the temperature to 300°C at 5°C / min, kee...

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Abstract

The invention discloses a preparation method of high-purity metallic rubidium and cesium. The preparation method comprises the steps of (1) preheating and dehydrating rubidium and cesium compounds; (2) carrying out primary reduction to obtain metallic cesium and primary reduction residues; (3) carrying out primary rectification on metallic cesium in the inert atmosphere, so as to obtain a primaryrectification product and primary rectification residues, and carrying out secondary rectification on the primary rectification product in the inert atmosphere, so as to obtain high-purity metallic cesium and secondary rectification residues; (4) mixing the primary reduction residues, the primary rectification residues and the secondary rectification residues with a secondary reducing agent, and carrying out secondary reduction to obtain metallic cesium, metallic rubidium and secondary reduction residues; (5) carrying out vacuum distillation separation on metallic cesium and metallic rubidium,so as to obtain a vacuum distillation product and a distillation residual liquid; and (6) carrying out distillation on the vacuum distillation product in the inert atmosphere for two times, so as toobtain two-time distillation products and high-purity metallic rubidium. The method is particularly suitable for separating the mixed rubidium and cesium compounds in which rubidium and cesium are mixed together to recycle and obtain high-purity metallic rubidium and high-purity metallic cesium.

Description

technical field [0001] The invention belongs to the field of nonferrous metal preparation, in particular to a method for preparing metal rubidium and cesium. Background technique [0002] Yichun, Jiangxi has the largest lepidolite mine in Asia, which is rich in lithium, rubidium, cesium, potassium, sodium, etc., not only Li 2 The content of O is as high as more than 4.5%, and the content of rubidium and cesium is also as high as about 1.5%. Its comprehensive development and utilization has very important economic and strategic value. [0003] People first discovered the important properties of cesium and rubidium because they are "long-eyed" metals-with excellent photoelectric properties. Because there are highly active free electrons in the crystals of alkali metals, they have good electrical conductivity and thermal conductivity. Under the action of light of a certain wavelength, the free electrons of cesium and rubidium can obtain energy and escape from the metal surface...

Claims

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Application Information

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IPC IPC(8): C22B26/10
CPCC22B26/10Y02P10/20
Inventor 姚胜兰
Owner 湖南中大技术创业孵化器有限公司
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