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Preparation method of anhydrous scandium chloride molten salt

A technology of hydrous scandium chloride and scandium chloride, which is applied in the preparation/treatment of rare earth metal compounds, rare earth metal chlorides, rare earth metal halides, etc., can solve the problems of difficult industrial production and safe production of the preparation process, and achieve industrial applicability Strong, low hydrolysis rate, high-purity hydrolysis rate effect

Active Publication Date: 2021-07-06
CHINA ENFI ENGINEERING CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to provide a preparation method of anhydrous scandium chloride molten salt, to solve the problem that the preparation process of anhydrous scandium chloride in the prior art is difficult for industrial safety production

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  • Preparation method of anhydrous scandium chloride molten salt
  • Preparation method of anhydrous scandium chloride molten salt

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preparation example Construction

[0021] As analyzed in the background technology of this application, the preparation process of anhydrous scandium chloride in the prior art is difficult for industrial safe production due to complicated equipment or high risk of poisonous gas leakage. In order to solve this problem, the application provides a method for preparing anhydrous scandium chloride molten salt, the preparation method comprising: step S1, using concentrated hydrochloric acid to dissolve scandium oxide to obtain scandium chloride solution; step S2, dissolving NaCl, KCl and NH 4 The mixed solution of Cl is mixed with the scandium chloride solution to obtain a scandium chloride molten salt solution; step S3, the scandium chloride molten salt solution is first heated to evaporate HCl and more than 90% of free water to obtain aqueous scandium chloride molten salt solution Salt, aqueous scandium chloride molten salt containing NH 4 Cl, free water and crystallization water; step S4, carry out second heating...

Embodiment 1

[0036] Using 50 mL of 30% hydrochloric acid to dissolve 10 g of scandium oxide with a purity of 99.0% at a heating temperature of 90° C., to prepare a scandium chloride solution. Configure NaCl, KCl and NH 4 Cl mixed solution, and then mixed the scandium chloride solution with the chloride mixed solution, where Sc 2 o 3 , (KCl+NaCl) and NH 4 The mass ratio of Cl is 1:1:3, and the residue is filtered off after stirring to obtain a mixed molten salt solution of scandium chloride, and KCl and NaCl are added in equimolar amounts. Heat the mixed scandium chloride molten salt solution prepared above to 120°C, evaporate excess HCl and about 90% of free water, and obtain aqueous scandium chloride molten salt, which contains NH 4 Cl, free water, and water of crystallization. Put the hydrated scandium chloride molten salt into an oven, raise the temperature to 110° C., keep it warm for 4 hours, and dry to completely remove the remaining free water and crystal water in the molten sal...

Embodiment 2

[0038] 105 mL of hydrochloric acid with a concentration of 35% was used to dissolve 15 g of scandium oxide with a purity of 99.5% at a heating temperature of 80° C. to prepare a scandium chloride solution. Configure NaCl, KCl and NH 4 Cl mixed solution, and then mixed the scandium chloride solution with the chloride mixed solution, where Sc 2 o 3 , (KCl+NaCl) and NH 4 The mass ratio of Cl is 1:3:6, and the residue is filtered off after stirring to obtain a scandium chloride molten salt solution, and KCl and NaCl are added in equimolar amounts. Heat the scandium chloride molten salt solution prepared above to 150°C, evaporate excess HCl and about 92% of free water to obtain aqueous scandium chloride molten salt, which contains NH 4 Cl, free water, and water of crystallization. Put the hydrated scandium chloride molten salt into an oven, raise the temperature to 90°C, keep it warm for 6 hours, dry and completely remove the remaining free water and crystal water in the molten...

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Abstract

The invention provides a preparation method of anhydrous scandium chloride molten salt. The preparation method comprises the following steps: S1, dissolving scandium oxide by using concentrated hydrochloric acid to prepare a scandium chloride solution; S2, mixing a mixed solution of NaCl, KCl and NH4Cl with the scandium chloride solution to obtain a scandium chloride mixed molten salt solution; S3, carrying out first heating on the scandium chloride molten salt solution to evaporate HCl and 90% or more of free water, so as to obtain water-containing scandium chloride molten salt; S4, subjecting the water-containing scandium chloride molten salt to second heating to remove free water and crystal water in the water-containing scandium chloride molten salt, so as to obtain anhydrous scandium chloride molten salt, wherein the second heating temperature is 90-120 DEG C, and the heat preservation time is 3-6 hours; and S5, subjecting the anhydrous scandium chloride fused salt to third heating in a tubular furnace under a vacuum condition so as to remove NH4Cl, wherein the set temperature of the tubular furnace is 400-600 DEG C. The method has no toxic gas leakage and can realize safe production.

Description

technical field [0001] The invention relates to the field of preparation of anhydrous scandium chloride, in particular to a preparation method of anhydrous scandium chloride molten salt. Background technique [0002] The ions of rare earth scandium in aqueous solution are trivalent, Sc +3 The ionic radius of scandium is small, so scandium compounds have a stronger hydrolysis tendency than corresponding other rare earth compounds. ScCl 3 It has strong water absorption, and scandium chloride containing crystal water is easily hydrolyzed to form water-insoluble ScOCl during the heating process, which seriously affects the practical application of scandium chloride. Anhydrous scandium chloride is the precursor of organic complexes for the preparation of rare earth metals or rare earth alloys, and has received more and more attention. Therefore, it is very important to further study the method for preparing anhydrous scandium chloride which is easy to operate, safe and has high...

Claims

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Application Information

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IPC IPC(8): C01F17/10C01F17/271
CPCC01F17/10C01F17/271
Inventor 韩国强王玮玮付云枫李晓艳
Owner CHINA ENFI ENGINEERING CORPORATION
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