Preparation method of lithium tetrafluoroborate
A technology of lithium tetrafluoroborate and lithium fluoride, which is applied in the direction of tetrafluoroboric acid, boron halide compounds, electrochemical generators, etc., can solve the problem of difficult control of solid dosing, difficult control of reaction process, strong corrosion and irritation and other issues, to achieve good economic value and social value, easy to operate and control, and easy to operate
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Embodiment 1
[0023] Embodiment 1, a kind of preparation method of lithium tetrafluoroborate mentioned in the present invention, comprises the following steps:
[0024] 1) Add 2400g of dimethyl carbonate to the reaction device in an airtight manner, and then put in 100g of lithium fluoride. The lithium fluoride is high-purity lithium fluoride with a high purity greater than 99.5%. Under normal temperature and pressure, start stirring at a speed of 10~40rpm, to obtain lithium fluoride suspension (mass fraction is 4%);
[0025] 2) Slowly inject 310 g of boron trifluoride gas into the lithium fluoride suspension obtained in step 1), and the reaction time is 80 minutes to obtain a reaction solution; the mass fraction of lithium tetrafluoroborate in the obtained reaction solution is 13.09%;
[0026] 3) The reaction solution obtained in step 2) is introduced into the filter device under the protection of nitrogen, and the filtrate is introduced into the concentrator under the protection of nitrog...
Embodiment 2
[0030] Embodiment 2, a kind of preparation method of lithium tetrafluoroborate mentioned in the present invention, comprises the following steps:
[0031] 1) Sealedly add 2500g of ethyl methyl carbonate to the reaction device, and then put in 220g of lithium fluoride. The lithium fluoride is high-purity lithium fluoride with a high purity greater than 99.5%. Under normal temperature and pressure, start stirring at a speed of 30rpm, get 8.09% lithium fluoride suspension;
[0032] 2) Slowly inject 590 g of boron trifluoride gas into the lithium fluoride suspension obtained in step 1), and the reaction time is 110 minutes to obtain a reaction liquid; the mass fraction of lithium tetrafluoroborate in the obtained reaction liquid is 24.12%;
[0033] 3) The reaction solution obtained in step 2) is introduced into the filter device under the protection of nitrogen, and the filtrate is introduced into the concentrator under the protection of nitrogen.
[0034]4) Heat up the filtrate ...
Embodiment 3
[0037] Embodiment 3, a kind of preparation method of lithium tetrafluoroborate mentioned in the present invention, comprises the following steps:
[0038] 1) Airtightly add 1350g of the mother liquor filtered in Example 1 into the reaction device, then add 1100g of dimethyl carbonate, and then add 180g of lithium fluoride, the lithium fluoride is high-purity lithium fluoride, and its high purity is greater than 99.5 %, under normal temperature and pressure, start stirring, and the rotating speed is 40rpm to obtain lithium fluoride suspension;
[0039] 2) Slowly inject 480g of boron trifluoride gas into the lithium fluoride suspension obtained in step 1), and the reaction time is 100min to obtain a reaction solution; the mass fraction of lithium tetrafluoroborate in the obtained reaction solution is 23.23%;
[0040] 3) The reaction solution obtained in step 2) is introduced into the filter device under the protection of nitrogen, and the filtrate is introduced into the concentr...
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