Preparation method of high-purity lithium tetrafluoroborate
A technology of high-purity lithium tetrafluoroborate and lithium tetrafluoroborate, which is applied in the field of preparation of high-purity lithium tetrafluoroborate, can solve the problems of high production cost and environmental pollution, and achieves low water content, strong operability, and no The effect of three wastes discharge
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Embodiment 1
[0024] A preparation method of high-purity lithium tetrafluoroborate, comprising the following steps:
[0025] (1) Under the condition of -10°C, boric acid is slowly added to a hydrofluoric acid solution with a mass percentage concentration of 10%, and the molar ratio of boric acid to anhydrous hydrofluoric acid is: H 3 BO 3 : HF=1:4, then continue to stir, react for 2h, and prepare fluoroboric acid solution;
[0026] (2) At -10°C, add lithium carbonate to the fluoroboric acid solution prepared in step (1) according to the molar ratio Li:B=1.05, and stir for 0.5 h to obtain a lithium tetrafluoroborate solution;
[0027] (3) The lithium tetrafluoroborate solution is concentrated at -0.05MPa and 90°C to 1 / 8 of the original volume of the lithium tetrafluoroborate solution, then cooled to crystallize at room temperature at 20°C, filtered, and the obtained solid is four Lithium fluoroborate crystal;
[0028] (4) Lithium tetrafluoroborate crystals were preliminarily dried at 60°C...
Embodiment 2
[0032] A preparation method of high-purity lithium tetrafluoroborate, comprising the following steps:
[0033] (1) Under the condition of 10 DEG C, boric acid is slowly added to the hydrofluoric acid solution whose mass percent concentration is 60%, and the molar ratio of boric acid to anhydrous hydrofluoric acid is: H 3 BO 3 : HF=1:6, then continue to stir, react for 0.5h, and prepare fluoboric acid solution;
[0034] (2) under the condition of 15° C., lithium hydroxide was added into the fluoroboric acid solution prepared in step (1) according to the molar ratio Li:B=1.5, and the reaction was stirred for 5 hours to obtain a lithium tetrafluoroborate solution;
[0035] (3) The lithium tetrafluoroborate solution is concentrated at -0.09MPa and 50°C to 1 / 3 of the original volume of the lithium tetrafluoroborate solution, then cooled to crystallize at room temperature at 20°C, filtered, and the obtained solid is four Lithium fluoroborate crystal;
[0036] (4) Lithium tetraflu...
Embodiment 3
[0040] A preparation method of high-purity lithium tetrafluoroborate, comprising the following steps:
[0041] (1) Under the condition of 0 DEG C, boric acid is slowly added into the hydrofluoric acid solution whose mass percent concentration is 30%, and the molar ratio of boric acid to anhydrous hydrofluoric acid is: H 3 BO 3 : HF=1:4.5, then continue to stir, react for 5h, and prepare fluoboric acid solution;
[0042] (2) Add lithium bicarbonate into the fluoroboric acid solution prepared in step (1) according to the ratio of molar ratio Li:B=1.2 at 0° C., and stir for 2 hours to obtain a lithium tetrafluoroborate solution;
[0043] (3) Lithium tetrafluoroborate solution was concentrated at -0.08MPa and 70°C to 1 / 5 of the original volume of the lithium tetrafluoroborate solution, then cooled to room temperature at 20°C for cooling and crystallization, and filtered to obtain a solid of four Lithium fluoroborate crystal;
[0044] (4) Lithium tetrafluoroborate crystals were ...
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