A kind of lithium oxalate phosphate and preparation method thereof
A lithium oxalate phosphate and solvent technology, which is applied in chemical instruments and methods, final product manufacturing, sustainable manufacturing/processing, etc., can solve the problems of shortened battery life, easy decomposition reactions, poor chemical stability, etc. Short, good capacity recovery rate, low internal resistance effect
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[0026] A kind of lithium oxalate phosphate, it is characterized in that: the chemical formula of described lithium oxalate phosphate is
[0027] Li C 2 o 4 PO 2 , its structure is
[0028] The second purpose of the present invention is to be achieved through the following technical solutions:
[0029] A preparation method for lithium oxalate phosphate, characterized in that:
[0030] (1) Mix and dissolve lithium difluorophosphate and lithium oxalate with a molar ratio of 0.5-2:1 into a polar aprotic solvent, and control the reaction temperature at 25-120°C;
[0031] (2) After the reaction was completed, the insolubles were removed by filtration, and then the solvent was removed under reduced pressure to finally obtain the lithium oxalate phosphate crude product;
[0032] (3) dissolving the crude lithium oxalate phosphate obtained in the above steps into a polar aprotic solvent, then adding a weak polar solvent for recrystallization, and obtaining pure lithium oxalate ph...
Embodiment 1
[0041]
[0042] Step 1: Add 108g (1mol) lithium difluorophosphate, 200mL dry dimethyl carbonate, and 102g (1mol) anhydrous lithium oxalate to a 1L autoclave, heat the reaction system to 60°C, and control the reaction pressure at 0.2MPa , reacted for 6 hours.
[0043] Step 2: Stand still, remove the insoluble matter in the reaction system by suction filtration under reduced pressure, and obtain a dimethyl carbonate solution of lithium oxalate phosphate. Lithium oxalate phosphate was obtained as a white solid after removal of the solvent under reduced pressure.
[0044] Step 3: Add the above crude lithium oxalate phosphate product into a 1L reaction kettle, add anhydrous dimethyl carbonate, raise the temperature to 100°C, and add dichloromethane to carry out recrystallization operation after all dissolved. Crystals were precipitated, filtered after cooling, and dried at a temperature of 80° C. under vacuum to obtain 136 g of a white solid with a yield of 86%.
Embodiment 2
[0046]
[0047] Step 1: Add 108g (1mol) lithium difluorophosphate, 200mL dry anhydrous acetonitrile, 112g (1.1mol) anhydrous lithium oxalate to a 1L autoclave, heat the reaction system to 90°C, and control the reaction pressure at 0.2MPa , reacted for 4 hours.
[0048] Step 2: Stand still, remove the insoluble matter in the reaction system by suction filtration under reduced pressure to obtain a dimethyl carbonate solution of lithium oxalate phosphate, and remove the solvent under reduced pressure to obtain a white solid of lithium oxalate phosphate.
[0049] Step 3: Add the crude lithium oxalate phosphate product above into a 1L reaction kettle, add anhydrous acetonitrile, raise the temperature to 90°C, add n-hexane to carry out recrystallization operation after all dissolved. Crystals were precipitated, filtered after cooling, and dried at a temperature of 80° C. under vacuum to obtain 139 g of a white solid with a yield of 88%.
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