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
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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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