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Lithium difluorobisoxalate phosphate preparation method, non-aqueous electrolyte and battery

A technology of difluorobis-oxalate lithium phosphate and bis-oxalate lithium phosphate, which is applied to non-aqueous electrolyte batteries, secondary batteries, lithium batteries, etc. , the product is difficult to purify and other problems, to achieve the effect of simple process, small internal resistance and electrochemical stability

Active Publication Date: 2019-05-31
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the problems in the prior art that the preparation of lithium difluorobisoxalate phosphate is complicated, the product is difficult to purify, and the chlorine compounds and free acids are relatively high, the present invention proposes a relatively simple technical solution for preparing lithium difluorobisoxalate phosphate

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  • Lithium difluorobisoxalate phosphate preparation method, non-aqueous electrolyte and battery

Examples

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Effect test

Embodiment 1

[0037] In a glove box, take 30 g of synthesized lithium bisoxalate borate with a moisture content below 200 ppm in a 500 mL three-necked flask, and add 309 mL of acetonitrile with a moisture content below 50 ppm dried over molecular sieves. Move it out of the glove box, immerse it in the set 60°C oil bath and stir it well, when the temperature in the flask is 60°C, pass into phosphorus pentafluoride gas (make the mixture of bisoxalate lithium borate and phosphorus pentafluoride The molar ratio is 1:1.05), and the total feeding time is controlled within 2-3 hours. After the gas feeding is completed, continue to stir for 2 hours to react. After the reaction is completed, remove insoluble impurities by filtration to obtain a lithium difluorobisoxalate phosphate solution. After vacuum distillation at 90-110°C, dichloromethane is added to the concentrated solution for crystallization to obtain a crude product of lithium difluorobisoxalate phosphate. Dry in a vacuum drying oven at a...

Embodiment 2

[0039]In the glove box, take 35.8 g of synthesized lithium bisoxalate borate with a moisture content below 200 ppm in a 250 mL three-necked flask, and add 185 ml of acetonitrile with a moisture content below 50 ppm dried with molecular sieves. Move it out of the glove box, immerse it in the set 80°C oil bath and stir it fully. When the temperature in the flask is 80°C, pass in phosphorus pentafluoride gas (make the mixture of bisoxalate lithium borate and phosphorus pentafluoride The molar ratio is 1:2), and the total feeding time is controlled at 2-3 hours. After the gas feeding is completed, continue to stir for 2 hours to react. After the reaction is completed, remove insoluble impurities by filtration to obtain a lithium difluorobisoxalate phosphate solution. After vacuum distillation at 90-110°C, dichloromethane is added to the concentrated solution for crystallization to obtain a crude product of lithium difluorobisoxalate phosphate. Dry in a vacuum drying oven at a temp...

Embodiment 3

[0041] In a glove box, take 36.5 g of synthesized lithium bisoxalate borate with a moisture content below 200 ppm in a 250 mL three-necked flask, and add 125 ml of tetrahydrofuran with a moisture content below 30 ppm dried with molecular sieves. Move it out of the glove box, immerse it in the set 80°C oil bath and stir it fully. When the temperature in the flask is 80°C, pass in phosphorus pentafluoride gas (make the mixture of bisoxalate lithium borate and phosphorus pentafluoride The molar ratio is 1:2.5), and the total feeding time is controlled at 2-3 hours. After the gas feeding is completed, continue to stir for 2 hours to react. After the reaction is completed, remove insoluble impurities by filtration to obtain a lithium difluorobisoxalate phosphate solution. After vacuum distillation at 90-110°C, dichloromethane is added to the concentrated solution for crystallization to obtain a crude product of lithium difluorobisoxalate phosphate. Dry in a vacuum drying oven at a ...

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Abstract

The invention relates to the technical field of energy storage batteries, and provides a lithium difluorobisoxalate phosphate preparation method which includes the steps: dissolving lithium difluoroborate by non-aqueous solvents to obtain first solution; heating the first solution to reach the temperature of 50-130 DEG C, leading phosphorus pentafluoride gas into the first solution and performingreaction to obtain lithium difluorobisoxalate phosphate solution; performing reduced pressure distillation on the lithium difluorobisoxalate phosphate solution and adding inert solvent crystals to obtain lithium difluorobisoxalate phosphate. Raw materials needed by the preparation method are low in cost and easy to obtain, and a reaction product is the lithium difluorobisoxalate phosphate, so thatthe prepared product is high in purify and yield. The technological process of the method is simple, requirements for equipment and environments are low, and the method is suitable for industrial production and application. The invention further provides non-aqueous electrolyte and a battery comprising the same. The non-aqueous electrolyte comprises the lithium difluorobisoxalate phosphate prepared by the method. The non-aqueous electrolyte is good in conductivity and electrochemically stable.

Description

technical field [0001] The present invention relates to the technical field of energy storage batteries, and more specifically, relates to a method for preparing lithium difluorobisoxalate phosphate, a non-aqueous electrolyte containing lithium difluorobisoxalate phosphate prepared by the above method, and A battery comprising the non-aqueous electrolyte. Background technique [0002] Lithium difluorobisoxalate phosphate is mainly used as an additive in the electrolyte of lithium batteries, and has good conductivity and electrochemical stability. Lithium difluorobisoxalate phosphate is mainly aimed at modifying the electrolyte, and has a good performance in improving the discharge rate of the battery and reducing the internal resistance of the battery. At present, there are relatively few studies on the synthesis of lithium difluorobisoxalate phosphate. As a manufacturing method of lithium difluorobisoxalate phosphate, the patent CN102216311B proposes to use lithium hexaflu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574H01M10/0567H01M10/052
CPCY02E60/10
Inventor 冯天明余意何凤荣
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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