A kind of method for preparing lithium difluorophosphate
A technology of lithium difluorophosphate and boric acid, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of difficult purification, high requirements for reaction conditions, and many by-products, so as to improve cycle stability and reaction The effect of mild conditions and good interfacial compatibility
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Embodiment 1
[0047] Embodiment 1 provides the method for preparing lithium difluorophosphate, comprises the following steps:
[0048] At room temperature, add 69.6g (1.0mol) of diboron trioxide into 720g of anhydrous acetonitrile, slowly add 239.3g (1.575mol) of lithium hexafluorophosphate solid with a solid feeder under stirring, then raise the temperature to 70°C for 5 hours, Lower the temperature to normal temperature to filter out a small amount of insoluble matter, then concentrate the filtrate under normal pressure until it is thicker with stirring, add 720g of dry 1,2-dichloroethane, and then slowly cool the system to 20°C, the product gradually turns white and fine Precipitate in the form of granular solids, filter the mother liquor, and wash the product with 240g of dry acetonitrile and 1,2-dichloroethane mixed solvent (mass ratio: 1:4), and dry the obtained product in vacuum at 60°C for 5 hours, 152.0 g of white powder lithium difluorophosphate was obtained, the molar yield was 9...
Embodiment 2
[0050] Embodiment 2 provides the method for preparing lithium difluorophosphate, comprises the steps:
[0051] At normal temperature, 24.85g (0.5mol) of lithium metaborate and 76.0g (0.5mol) of lithium hexafluorophosphate were added to 380g of dry tetrahydrofuran, the temperature was raised to reflux for 5 hours under stirring, and a small amount of insoluble matter was filtered off at normal temperature. Concentrate the filtrate under normal pressure until it is relatively viscous when stirring, add 380g of dry dichloromethane, then slowly cool the system to 20°C, the product gradually precipitates in the form of white fine particle solids, filter the mother liquor, and use 76g of dry tetrahydrofuran Wash the product with a mixed solvent of dichloromethane (mass ratio is 1:4), and dry the resulting product in vacuum at 60°C for 5 hours to obtain 47.3g of white powdery lithium difluorophosphate, with a molar yield of 87.7%. Chromatographically determined purity was 99.0%.
Embodiment 3
[0053] Embodiment 3 provides the method for preparing lithium difluorophosphate, comprises the steps:
[0054] At room temperature, 84.6g (0.5mol) of anhydrous Li 2 B 4 o 7 Add 265.8g (1.75mol) of lithium hexafluorophosphate to 797g of dry ethylene glycol dimethyl ether, heat up to 60°C under stirring and react for 6 hours, drop to normal temperature and filter out a small amount of insoluble matter, and concentrate the filtrate under normal pressure until it is relatively viscous when stirred 797g of dry toluene was added, then the system was slowly cooled to 20°C, the product gradually precipitated, the mother liquor was filtered off, and the product was washed with 266g of dry ethylene glycol dimethyl ether and toluene mixed solvent (mass ratio: 1:4), The obtained product was vacuum-dried at 60° C. for 5 hours to obtain 166.3 g of white powdery lithium difluorophosphate, the molar yield was 88.1%, and the purity determined by ion chromatography was 99.5%.
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