Preparation method of lithium hexafluorozirconate
A technology of lithium fluorozirconate and fluorozirconate, which is applied in the field of preparation of lithium fluorozirconate, can solve the problems of unfavorable large-scale production and application of lithium fluorozirconate, low purity of lithium fluorozirconate, etc., and achieve a stable and controllable reaction process , is conducive to the formation and growth of crystal nuclei, and reduces the effect of volatilization loss
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Embodiment 1
[0035] This embodiment is a preparation method of lithium fluorozirconate, comprising the following steps:
[0036] S1, zirconium oxychloride (1mol) is added to hydrogen fluoride solution (mass concentration is 30%, hydrogen fluoride is 6.5mol) and water, makes fluozirconic acid (H 2 ZrF 6 ) solution (mass concentration is 105g / L);
[0037] Lithium carbonate (1.05mol) is dissolved in water, makes lithium carbonate solution;
[0038] S2. Add the fluorozirconate solution in step S1 to 1 / 4 part of the lithium carbonate solution (parts by mass), and control the temperature to 40°C; then add the rest of the lithium source solution, and react at 40°C for 6h; the reaction ends Finally, separate the solid from the liquid, collect the solid phase, wash with water until the pH of the washing solution is 7, and dry at 80°C for 4 hours to obtain lithium fluorozirconate (Li 2 ZrF 6 ).
[0039] The purity of the lithium hexafluorozirconate powder prepared in this example is 99.8%.
Embodiment 2
[0041] This embodiment is a preparation method of lithium fluorozirconate, comprising the following steps:
[0042] S1, adding zirconium oxychloride (1mol) to hydrogen fluoride solution (mass concentration is 35%, hydrogen fluoride is 6.5mol) and water, makes fluorozirconic acid (H 2 ZrF 6 ) solution (mass concentration is 110g / L);
[0043] Lithium hydroxide (2.2mol) was dissolved in water to obtain lithium hydroxide solution;
[0044] S2. Add the fluorozirconate solution in step S1 to 1 / 4 part of the lithium hydroxide solution (parts by mass), and control the temperature to 40°C; then add the rest of the lithium source solution, and react at 50°C for 6h; react After the end, separate the solid from the liquid, collect the solid phase, wash with water until the pH of the washing solution is 7, and dry at 80°C for 4 hours to obtain lithium fluorozirconate (Li 2 ZrF 6 ).
[0045] The purity of the lithium hexafluorozirconate powder prepared in this example is 99.7%.
Embodiment 3
[0047] This embodiment is a preparation method of lithium fluorozirconate, comprising the following steps:
[0048] S1, zirconium oxychloride (1mol) is added to hydrogen fluoride solution (mass concentration is 40%, hydrogen fluoride is 6.5mol) and water, makes fluozirconic acid (H 2 ZrF 6 ) solution (mass concentration is 130g / L);
[0049] Lithium carbonate (1.05mol) is dissolved in water, makes lithium carbonate solution;
[0050] S2. Add the fluorozirconate solution in step S1 to 1 / 4 part of the lithium carbonate solution (parts by mass), and control the temperature to 40°C; then add the rest of the lithium source solution, and react at 60°C for 5h; the reaction ends Finally, separate the solid from the liquid, collect the solid phase, wash with water until the pH of the washing solution is 7, and dry at 80°C for 4 hours to obtain lithium fluorozirconate (Li 2 ZrF 6 ).
[0051] The purity of the lithium hexafluorozirconate powder prepared in this example is 99.8%.
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