Preparation method for micron scandium fluoride
A scandium fluoride, micron-scale technology, applied in the field of material chemistry, can solve the problems of low yield and complicated process of submicron scandium fluoride, and achieve the effect of good shape, strong surface activity and guaranteed purity
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[0017] As described in the background art, the existing methods for preparing submicron scandium fluoride have the problems of complicated process and low yield of submicron scandium fluoride. In order to solve the above technical problems, the application provides a method for preparing micron scandium fluoride, the preparation method comprising: saponifying ammonia water and an organic carboxylic acid extractant to obtain an ammonium saponification extractant; partially ammonium saponification extractant Extract with scandium-containing solution to obtain scandium-containing organic phase and raffinate; mix the remaining ammonium saponification extractant with ammonium fluoride to obtain fluorine-containing mixed solution; carry out precipitation reaction between scandium-containing organic phase and fluorine-containing mixed solution, Obtain micron scandium fluoride.
[0018] The organic carboxylic acid extractant has surface activity because of its own hydrophilic and lipo...
Embodiment 1
[0050] In the extraction reactor, add 1000mL kerosene solution containing 1mol / L sec-octylphenoxyacetic acid-10% n-butanol (phase regulator), then add ammonia water and sec-octylphenoxyacetic acid (CA-12) A saponification reaction occurs to obtain an ammonium saponification extractant (the first water / oil microemulsion type organic phase), and the degree of saponification is 90%.
[0051] Mix 500mL ammonium saponification extractant with 500mL scandium chloride solution containing 0.3mol / L scandium to extract scandium in the scandium-containing hydrochloric acid solution, use ammonia water to control the extraction end point pH of the scandium-containing solution to be 2.5, and separate and remove the raffinate. Obtain scandium-containing organic phase (the second water / oil microemulsion type organic phase);
[0052] Add 80mL of 5mol / L ammonium fluoride solution (wherein the molar ratio of fluoride ion to scandium ion is 5.33) to 500mL of the above-mentioned first water / oil mi...
Embodiment 2
[0056] In the extraction reactor, add 1000mL n-heptane solution containing 3mol / L naphthenic acid extractant-20% isooctyl alcohol (phase regulator), add ammonia water and naphthenic acid extractant for saponification reaction, and obtain ammonium saponification extraction agent (the first water / oil microemulsion type organic phase), the degree of saponification is 60%.
[0057] Mix 500mL of ammonium saponification extractant with 500mL of scandium chloride solution containing 0.3mol / L scandium to extract scandium in the scandium-containing hydrochloric acid solution, control the pH of the extraction end point of the scandium-containing solution to 3.5 with ammonia water, and separate and remove the raffinate. A scandium-containing organic phase (second water / oil microemulsion type organic phase) is obtained.
[0058] Add 40 mL of 8 mol / L ammonium fluoride solution to 500 mL of the above-mentioned ammonium saponification extractant to form a fluorine-containing mixed liquid (th...
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