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Preparation method for anhydrous rare-earth chloride

A rare earth chloride and rare earth oxide technology, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as insufficient technology for synthesizing anhydrous rare earth chloride, avoid adverse effects, reduce costs, eliminate The effect of air disturbance

Inactive Publication Date: 2019-07-23
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing anhydrous rare earth chloride in view of the insufficient technology of synthesizing anhydrous rare earth chloride at present. The method has the advantages of simple operation, high product purity and high yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Put 10g of scandium oxide into the crucible, add 60mL of water, slowly add hydrochloric acid into the crucible under stirring conditions, until completely dissolved, and obtain an aqueous solution of scandium chloride;

[0032] (2) add 70g ammonium chloride in the scandium chloride solution after dissolving, obtain the mixed solution of rare earth chloride and ammonium chloride;

[0033] (3) Evaporate and fry dry under heating conditions to obtain a solid mixture of rare earth chloride and ammonium chloride containing crystal water, transfer the solid to a mortar and grind it into powder, and then transfer it to a crucible again for heating and frying dry, so Repeat until the solid has no agglomeration after heating in the crucible;

[0034] (4) Transfer the above-mentioned solid powder to the sublimation device, heat it by gradient temperature rise and continue the decompression operation, the temperature rise rate is 5°C / min, and the temperature control method is:...

Embodiment 2

[0036] (1) Put 10g of yttrium oxide into the crucible, add 60mL of water, slowly add hydrochloric acid in the crucible under stirring conditions, until completely dissolved, and obtain an aqueous solution of yttrium chloride;

[0037] (2) add 70g ammonium chloride in the yttrium chloride solution after dissolving, obtain the mixed solution of rare earth chloride and ammonium chloride;

[0038] (3) Evaporate and fry dry under heating conditions to obtain a solid mixture of rare earth chloride and ammonium chloride containing crystal water, transfer the solid to a mortar and grind it into powder, and then transfer it to a crucible again for heating and frying dry, so Repeat until the solid has no agglomeration after heating in the crucible;

[0039] (4) Transfer the above-mentioned solid powder to a sublimation device, heat it in a gradient temperature-raising manner and continue the depressurization operation.

Embodiment 3

[0041] (1) Put 10g of lanthanum oxide into the crucible, add 60mL of water, slowly add hydrochloric acid in the crucible under agitation until completely dissolved, and obtain an aqueous solution of lanthanum chloride;

[0042] (2) add 70g ammonium chloride in the lanthanum chloride solution after dissolving, obtain the mixed solution of rare earth chloride and ammonium chloride;

[0043] (3) Evaporate and fry dry under heating conditions to obtain a solid mixture of rare earth chloride and ammonium chloride containing crystal water, transfer the solid to a mortar and grind it into powder, and then transfer it to a crucible again for heating and frying dry, so Repeat until the solid has no agglomeration after heating in the crucible;

[0044] (4) Transfer the above-mentioned solid powder to a sublimation device, heat it in a gradient temperature-raising manner and continue the depressurization operation.

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Abstract

The invention provides a preparation method for an anhydrous rare-earth chloride (REC13). The preparation method comprises the following steps: S1) utilizing hydrochloric acid to dissolve a rare earthoxide, thereby forming a rare-earth chloride solution; S2) adding ammonium chloride into the dissolved rare-earth chloride solution; S3) stir-frying under a heating condition, thereby acquiring a solid mixture of rare-earth chloride containing crystal water and ammonium chloride; S4) transferring the stir-fried solid mixture into a sublimation device, rising temperature to 390 DEG C from 80 DEG Cin the manner of gradient temperature rise, and meanwhile, vacuumizing and heating, and removing ammonium chloride and crystal water of the rare-earth chloride in turn in the vacuumizing and heatingprocess, thereby acquiring the high-purity anhydrous rare-earth chloride. The method provided by the invention has the characteristics of simple and safe production process, no side reaction, high purity of prepared anhydrous rare-earth chloride and being beneficial to large-scale production.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth materials, in particular to a method for preparing anhydrous rare earth chlorides by using rare earth oxides as raw materials. [0002] technical background [0003] Rare earth elements account for about one-seventh of the elements in the periodic table, including scandium, yttrium and 15 lanthanides. In-depth research on rare earth elements will not only help to discover new properties and explore new materials, but also promote the development of inorganic chemistry. The excellent optical, electrical, and magnetic properties of rare earth elements are known as the treasure house of new materials, and have become important strategic elements and the commanding heights of world scientific and technological competition. Anhydrous rare earth chlorides have also received more and more attention as precursors for the preparation of rare earth metal-organic complexes. [0004] The pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01P2006/82C01P2006/80C01F17/271
Inventor 潘付兴苗娟
Owner LANZHOU UNIVERSITY
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