Preparation method of anhydrous rare earth chloride

A technology of rare earth chlorides and rare earth oxides, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of insufficient technology for synthesizing anhydrous rare earth chlorides, avoid adverse effects and eliminate air interference , the effect of improving safety

Inactive Publication Date: 2019-07-30
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 technolo

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, and slowly add hydrochloric acid into the crucible under stirring conditions until it is completely dissolved to obtain an aqueous solution of scandium chloride;

[0032] (2) Add 70g of ammonium chloride to the dissolved scandium chloride solution to obtain a 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 for heating and frying. Repeat until the solid does not agglomerate after being heated in the crucible;

[0034] (4) Transfer the above solid powder to the sublimation device, use a gradient heating method to heat and continue the decompression operation, the heating rate is 5°C / min, and the temperature control method is: 80°C to 130°C, hold for 20 mi...

Embodiment 2

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

[0037] (2) Add 70g of ammonium chloride to the dissolved yttrium chloride solution to obtain a mixed solution of rare earth chloride and ammonium chloride;

[0038] (3) Evaporate and fry dry under heating 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 for heating and frying. Repeat until the solid does not agglomerate after being heated in the crucible;

[0039] (4) Transfer the above-mentioned solid powder to a sublimation device, and use a gradient heating method to heat and continue the decompression operation.

Embodiment 3

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

[0042] (2) Add 70g of ammonium chloride to the dissolved lanthanum chloride solution to obtain a 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 for heating and frying. Repeat until the solid does not agglomerate after being heated in the crucible;

[0044] (4) Transfer the above-mentioned solid powder to a sublimation device, and use a gradient heating method to heat and continue the decompression operation.

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Abstract

The invention provides a preparation method of anhydrous rare earth chloride (REC13). The method comprises the steps of S1, dissolving a rare earth oxide with hydrochloric acid to form a rare earth chloride solution; S2, adding ammonium chloride into the dissolved rare earth chloride solution; S3, parching the mixture until the mixture is thoroughly dried under a heating condition to obtain a solid mixture of the rare earth chloride containing crystal water and the ammonium chloride; S4, transferring the parched solid mixture into a sublimation device, raising the temperature from 80 DEG C to390 DEG C in a gradient heating mode, and simultaneously carrying out vacuuming heating operation, wherein in the vacuuming heating process, the crystal water of the ammonium chloride and the rare earth chloride are sequentially removed, so that the high-purity anhydrous rare earth chloride is obtained. The method has the advantages that the production process is simple and safe, no side reactionhappens, the purity of the prepared anhydrous rare earth chloride is high, and large-scale production is facilitated.

Description

Technical field [0001] The invention belongs to the technical field of rare earth material preparation, and particularly relates to a method for preparing anhydrous rare earth chloride 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. The in-depth study of rare earth elements will not only help 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 an important strategic element and the commanding height of the world's 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...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01P2006/80C01F17/271
Inventor 潘付兴刘伟生潘滢浩苗娟
Owner LANZHOU UNIVERSITY
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