Preparation method of high-purity lithium oxalyldifluoroborate
A technology of pure lithium oxalate difluoroborate and lithium oxalate, which is applied in chemical instruments and methods, compounds containing Group 3/13 elements of the periodic table, organic chemistry, etc., can solve the complex process, long reaction time and high price and other problems, to achieve the effect of broad application prospects, short response time, and low equipment investment
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Embodiment 1
[0032] Add 300 mL of acetonitrile into the dry reactor, add 10 g of lithium oxalate and 12.38 mL of boron trifluoride ether at the same time, stir and mix thoroughly. Under stirring, 1 mL of boron trichloride (BCl 3 ) was slowly added dropwise into the reactor at a constant temperature of 20°C for 1 h. The by-reaction solids and unreacted lithium oxalate were removed by filtration to obtain a solution containing LiODFB. The obtained solution was distilled under reduced pressure at 30°C for 30 minutes to remove acetonitrile, crystallized at -20°C for 60 minutes, and dried in vacuum at 40°C and -0.095MPa for 6 hours to obtain 13.3 g of pure LiODFB solid with a purity of 99.9% and a yield of 94%. .
Embodiment 2
[0034] Add 100 mL of propylene carbonate into the dry reactor, add 10 g of lithium oxalate and 37.5 mL of boron trifluoride ether at the same time, stir and mix thoroughly. Under stirring, 10g of aluminum trichloride (AlCl 3 ) was slowly added dropwise into the reactor at a constant temperature of 100°C for 12 hours. The by-reaction solids and unreacted lithium oxalate were removed by filtration to obtain a solution containing LiODFB. The obtained solution was distilled under reduced pressure at 80°C for 300min to remove propylene carbonate, crystallized at -20°C for 300min, and dried in vacuum at 150°C and -0.05MPa for 24h to obtain 13.1g of pure LiODFB solid with a purity of 99.9%. The yield was 93%.
Embodiment 3
[0036] Add 500 mL of dimethyl carbonate, 10 g of lithium oxalate and 24.76 mL of boron trifluoride diethyl ether into the dry reactor, stir and mix thoroughly. Under stirring, 8 mL of silicon tetrachloride (SiCl 4) was slowly added dropwise into the reactor at a constant temperature of 40°C for 2h. The by-reaction solids and unreacted lithium oxalate were removed by filtration to obtain a solution containing LiODFB. The obtained solution was distilled under reduced pressure at 50°C for 60min to remove dimethyl carbonate, crystallized at 10°C for 10min, and dried in vacuum at 70°C and -0.85MPa for 48h to obtain 12.9g of pure LiODFB solid with a purity of 99.9%. The yield was 91%.
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