A kind of preparation method of silver hexafluoroantimonate
A technology of silver hexafluoroantimonate and hexafluoroantimonate, applied in antimonate/antimonite and other directions, can solve the problems of low product purity, complicated impurity removal process and high cost of raw materials, and achieve high purity and purification method. Simple, high removal rate of impurities
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Embodiment 1
[0049] 1) Preparation of hexafluoroantimonic acid: at 60°C, mix antimony trioxide with 40% hydrogen fluoride in acetic acid solution, and then dropwise add mass percent at a rate of 1 mL / min under stirring at 60 r / min. The concentration is 30% hydrogen peroxide, and hexafluoroantimonic acid solution is obtained after reacting for 1 hour; wherein, the mass volume ratio of antimony trioxide to the acetic acid solution of hydrogen fluoride is 1:1g / ml, and the mass volume ratio of antimony trioxide to hydrogen peroxide is 1:1g / ml;
[0050] 2) Preparation of silver hexafluoroantimonate mother liquor: react silver hexafluoroantimonate mother liquor in silver hexafluoroantimonate solution for 0.5h at 60°C to obtain silver hexafluoroantimonate mother liquor; the amount of silver carbonate and antimony trioxide equal amounts of substances;
[0051] 3) Silver hexafluoroantimonate mother liquor concentration and cooling crystallization: the silver hexafluoroantimonate mother liquor was ...
Embodiment 2
[0055] 1) Preparation of hexafluoroantimonic acid: at 100°C, mix antimony trioxide with 40% hydrogen fluoride in acetic acid solution, and then dropwise add 100% by mass at a rate of 30mL / min under stirring at 80r / min. The concentration is 30% hydrogen peroxide, and hexafluoroantimonic acid solution is obtained after reacting for 2 hours; wherein, the mass volume ratio of antimony trioxide to acetic acid solution of hydrogen fluoride is 1:1.5g / ml, and the mass volume ratio of antimony trioxide to hydrogen peroxide 1:1g / ml;
[0056] 2) Preparation of silver hexafluoroantimonate mother liquor: Silver carbonate in hexafluoroantimonic acid solution was reacted for 1 hour at 100°C to obtain silver hexafluoroantimonate mother liquor; wherein the amount of silver carbonate was the same as that of antimony trioxide equal amounts of substances;
[0057] 3) Silver hexafluoroantimonate mother liquor concentration and cooling crystallization: the silver hexafluoroantimonate mother liquor...
Embodiment 3
[0060] 1) Preparation of hexafluoroantimonic acid: at 120°C, mix antimony trioxide with 40% hydrogen fluoride in acetic acid solution, and then dropwise add 100% by mass at a rate of 5mL / min under stirring at 100r / min. The concentration is 30% hydrogen peroxide, and hexafluoroantimonic acid solution is obtained after reacting for 4 hours; wherein, the mass volume ratio of antimony trioxide to the acetic acid solution of hydrogen fluoride is 1:2g / ml, and the mass volume ratio of antimony trioxide to hydrogen peroxide is 1:1g / ml;
[0061] 2) Preparation of silver hexafluoroantimonate mother liquor: silver carbonate in hexafluoroantimonic acid solution, after reacting for 1 hour at 120° C., to obtain silver hexafluoroantimonate mother liquor; wherein the amount of silver carbonate is the same as that of antimony trioxide equal amounts of substances;
[0062] 3) Silver hexafluoroantimonate mother liquor is concentrated and cooled to crystallize: the silver hexafluoroantimonate mo...
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