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Method for preparing high-purity rubidium carbonate

A high-purity technology of rubidium carbonate, applied in chemical instruments and methods, rubidium/cesium/francium compounds, alkali metal compounds, etc., can solve the problems of difficult separation of two phases, waste of extraction agent, low extraction efficiency, etc., and achieve extraction Thorough, high recovery and high extraction efficiency

Active Publication Date: 2015-08-19
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Existing methods for preparing high-purity rubidium carbonate, to obtain high-purity products, first use traditional extraction methods to undergo dozens or even hundreds of stages of extraction, the extraction efficiency is low, the extraction agent is seriously wasted, time-consuming and laborious, and the organic solvent In the case of stripping liquid, since the two phases are difficult to separate cleanly, it is impossible to obtain high-purity rubidium carbonate from the wet material after the stripping liquid is concentrated and crystallized only through simple high-temperature burning.
This application intends to use a combination of bipolar membrane and cation exchange membrane for extraction and back extraction. The extraction phase and the back extraction phase are not in direct contact. Rubidium carbonate, there is no related report in the prior art

Method used

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  • Method for preparing high-purity rubidium carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A method for preparing high-purity rubidium carbonate, the raw material is rubidium-containing waste liquid after extracting cesium with the acid leaching solution after leaching cesium garnet with sulfuric acid, and the steps are as follows:

[0046] (1) Get 13t of rubidium-containing waste liquid, after testing, the metal ion content is as follows: Cs + 0.02%, Rb + 1.89%, K + 0.54%, Na + 0.12%, Li + 0.15%, Al 3+ 0.003%, Fe 3+ 0.008%, Mg 2+ 0.06%, Ca 2+ 0.25%, Ba 2+ <0.0001%, concentrated to 1t by heating in a reactor.

[0047] (2) Add lime slurry to the concentrated solution, adjust the pH to 11.5, stir for five minutes, leave to react for 1 hour, and filter;

[0048] (3) Add 5% sulfuric acid solution to the filtrate obtained in step (2), adjust the pH to 6.0-6.5, stir for five minutes, leave to react for 1 hour, and filter;

[0049] (4) Add 10% sodium carbonate solution to the filtrate obtained by filtering in step (3), adjust the pH to 7.5-8.0, stir for fi...

Embodiment 2

[0058] A method for preparing high-purity rubidium carbonate, the raw material is rubidium sulfate and rubidium chloride mixed mother liquor, the steps are as follows:

[0059] (1) Get 6.41t rubidium sulfate and rubidium chloride mixed mother liquor, after testing, metal ion content is as follows: Cs + 0.01%, Rb + 2.37%, K + 1.23%, Na + 0.85%, Li + 0.31%, Al 3+ 0.04%, Fe 3+ 0.009%, Mg 2+ 0.001%, Ca 2+ 0.08%, Ba 2+ <0.0001%, concentrated to 1t by heating in a reactor.

[0060] (2) Add lime slurry to the concentrated solution, adjust the pH to 11.5, stir for ten minutes, leave to react for half an hour, and filter;

[0061] (3) Add 10% sulfuric acid solution to the filtrate obtained in step (2), adjust the pH to 6.0-6.5, stir for ten minutes, leave to react for half an hour, and filter;

[0062] (4) Add 8% sodium carbonate solution to the filtrate obtained by filtering in step (3), adjust the pH to 7.5-8.0, stir for ten minutes, and filter after standing for half an ho...

Embodiment 3

[0071] A method for preparing high-purity rubidium carbonate, the selected raw material is rubidium chloride and rubidium carbonate mixed mother liquor, the steps are as follows:

[0072] (1) Get 20t rubidium chloride and rubidium carbonate mixed mother liquor, after testing, metal ion content is as follows: Cs + 0.018%, Rb + 0.85%, K + 1.34%, Na + 0.03%, Li + 0.08%, Al 3+ 3+ 2+ 0.02%, Ca 2+ 2+ <0.0001%, concentrated to 1t by heating in a reactor.

[0073] (2) Add lime slurry to the concentrated solution, adjust the pH to 11.5, stir for five minutes, leave to react for half an hour, and filter;

[0074] (3) Add 15% sulfuric acid solution to the filtrate obtained in step (2), adjust the pH to 6.0-6.5, stir for five minutes, leave to react for half an hour, and filter;

[0075] (4) Add 5% sodium carbonate solution to the filtrate obtained by filtering in step (3), adjust the pH to 7.5-8.0, stir for five minutes, and filter after standing for half an hour to obtain the ext...

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Abstract

The invention belongs to the technical field of methods for extracting metal ions by the aid of bipolar membrane electric osmosis technology and further generating a high-purity inorganic metal compound, and particularly relates to a method for preparing high-purity rubidium carbonate by the aid of the bipolar membrane electric osmosis technology by taking rubidium-containing waste liquor as a raw material. The method includes the steps: firstly, concentrating the rubidium-containing waste liquor, removing magnesium, iron, aluminum, calcium and barium; secondly, further removing calcium to obtain liquor to be extracted; thirdly, extracting rubidium from the liquor to be extracted by the aid of an electric extraction device to prepare rubidium acetate strip liquor; finally, concentrating, crystallizing and decomposing the rubidium acetate strip liquor at high temperature to obtain the rubidium carbonate. The method is efficient and environmentally friendly, and the obtained rubidium carbonate is excellent in quality and suitable for industrial popularization and application.

Description

technical field [0001] The present invention relates to the technical field of using bipolar membrane electroosmosis technology to extract metal ions and then generate high-purity inorganic metal compounds, in particular to a method of using rubidium-containing waste liquid as raw material to prepare high-purity rubidium carbonate by using bipolar membrane electroosmosis technology Methods. Background technique [0002] The existing method for preparing high-purity rubidium carbonate, in order to obtain high-purity products, firstly use the traditional extraction method to go through dozens or even hundreds of stages of extraction, the extraction efficiency is low, the extraction agent is seriously wasted, time-consuming and labor-intensive, and the separation of organic solvents In the case of stripping liquid, since the two phases are difficult to separate cleanly, it is impossible to obtain high-purity rubidium carbonate from the wet material after the stripping liquid is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D17/00
Inventor 赵正红李兴陈格徐涛黄磊
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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