Method for preparing high purity lithium hexafluorophosphate
A lithium hexafluorophosphate, high-purity technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high production cost, corrosion of battery materials, high energy consumption, etc., and achieves fast reaction speed, no pollution to the environment, simple craftsmanship
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Embodiment 1
[0020] Weigh industrial calcium fluoride and phosphorus pentoxide at a mass ratio of 0.5:1.0, seal them in a ceramic ball mill mixer, ball mill and mix them for 2 hours under the protection of argon, and quickly transfer the mixture into a stainless steel airtight pressure heating furnace ( In the phosphorus pentafluoride generation furnace), the air in the furnace is driven away by argon gas, the furnace temperature is controlled at 280°C±5°C, the heating time is 4h, and the phosphorus pentafluoride generated by the reaction is drawn out under pressure; the solid high-purity nano-lithium fluoride and The anhydrous acetonitrile purified by rectification is put into another stainless steel airtight pressure heating furnace (lithium hexafluorophosphate production furnace) at the same time, and after the air in the furnace is driven away with argon, it is stirred under airtight conditions to form a suspension, and the five products generated in the previous step are mixed. Phospho...
Embodiment 2
[0023] Industrial calcium fluoride and phosphorus pentoxide were weighed according to the mass ratio of 0.3:1.0, sealed in a ceramic ball mill mixer, ball milled and mixed for 5 hours under the protection of argon, and the mixture was quickly transferred into a stainless steel airtight pressure heating furnace ( In the phosphorus pentafluoride generation furnace), the air in the furnace is driven away with argon, the furnace temperature is controlled at 300°C±5°C, the heating time is 8h, and the phosphorus pentafluoride generated by the reaction is extracted under pressure; the solid high-purity nano-lithium fluoride and The anhydrous acetonitrile purified by rectification is put into another stainless steel airtight pressure heating furnace (lithium hexafluorophosphate production furnace) at the same time, and after the air in the furnace is driven away with argon, it is stirred under airtight conditions to form a suspension, and the five products generated in the previous step...
Embodiment 3
[0026] According to the conditions described in Example 2, after the reaction is completed, the product obtained by vacuum drying is then dissolved and recrystallized by acetonitrile, the dissolution temperature is 70°C, the dissolution time is 6h, and the filtrate is filtered while it is hot, cooled and crystallized at -20°C, and then filtered to obtain The cake was vacuum-dried at 60°C to obtain the product.
[0027] The reaction yield is more than 98%, and the obtained product lithium hexafluorophosphate can meet the requirements for the use of lithium-ion battery electrolyte, and the specific indicators can be met: the product is high-purity grade, LiPF 6 The content is greater than 99.95%, the water content is less than 10ppm, the HF content is less than 5ppm, and the total impurity metal content is less than 10ppm.
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