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A kind of preparation method of lithium difluorobisoxalate phosphate, non-aqueous electrolyte and battery

A technology of lithium difluorobis oxalate phosphate and extraction liquid, which is applied to secondary batteries, chemical instruments and methods, circuits, etc. and other problems, to achieve the effect of simple steps, convenient operation, and prevention of deterioration

Active Publication Date: 2022-05-27
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the problems of difficulty in purification and product deterioration caused by post-treatment at high temperature in the preparation process of lithium difluorobisoxalate phosphate in the prior art, especially the problem that lithium difluorobisoxalate phosphate is difficult to separate from lithium difluorophosphate, the inventors The purification process of the crude product was studied, and an improved preparation method of lithium difluorobisoxalate phosphate was proposed

Method used

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  • A kind of preparation method of lithium difluorobisoxalate phosphate, non-aqueous electrolyte and battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Take 300 mL of the reacted dimethyl carbonate mixed solution containing lithium difluorobis oxalate phosphate, and the theoretical yield of lithium difluorobis oxalate phosphate is 132 g; the mixed solution is filtered to remove insolubles, and the obtained filtrate is concentrated by distillation under reduced pressure at 50 ° C , until concentrated to an oil.

[0067] In the oil, 50 mL of methanol was added first, then 150 mL of hexane was added, and after stirring for 30 min, the solution was divided into upper and lower layers after extraction, wherein methanol was in the lower layer and hexane was in the upper layer. The methanol layer and the hexane layer were put into different beakers respectively, and the content ratio of lithium difluorophosphate and lithium difluorobisoxalate phosphate in the methanol phase was detected by nuclear magnetic fluoride spectrum was 76%: 24%; The content ratio of lithium bis-oxalate phosphate to lithium difluorophosphate is 91%: 9...

Embodiment 2

[0071] Take 500 mL of the ethyl methyl carbonate mixed solution containing lithium difluorobis oxalate phosphate after the reaction, and the theoretical yield of lithium difluorobis oxalate phosphate is 331 g; this mixed solution is filtered to remove insolubles, and the obtained filtrate is concentrated by vacuum distillation at 50 ° C , until concentrated to an oil.

[0072] In the oil, 150 mL of dimethyl sulfoxide was added first, then 600 mL of cyclohexane was added, and after stirring for 50 min, the solution was extracted into two layers, the lower layer and the upper layer were dimethyl sulfoxide. The dimethyl sulfoxide layer and the cyclohexane layer were put into different beakers respectively, and the content ratio of lithium difluorophosphate and lithium difluorobisoxalate phosphate in the dimethyl sulfoxide phase was detected by nuclear magnetic fluoride spectrum was 83%. : 17%; the content ratio of lithium difluorobisoxalate to lithium difluorophosphate in the cyc...

Embodiment 3

[0075] Take 200 mL of the propylene carbonate solution containing lithium difluorobis oxalate phosphate that has been reacted, and the theoretical yield of lithium difluorobis oxalate phosphate is 99 g; the mixed solution is filtered to remove insolubles, and the obtained filtrate is concentrated under reduced pressure distillation at 50 ° C until Concentrated to an oil.

[0076] In the oil, 40 mL of dimethylformamide was added first, followed by 150 mL of heptane, and after stirring for 60 min, the solution was extracted into upper and lower layers, wherein dimethylformamide was in the lower layer and heptane was in the upper layer. The dimethylformamide layer and the heptane layer were put into different beakers, and the content ratio of lithium difluorophosphate and lithium difluorobisoxalate phosphate in the dimethylformamide phase was 69%: 31% after nuclear magnetic detection. ; The content ratio of lithium difluorobisoxalate to lithium difluorophosphate in the heptane ph...

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Abstract

The present invention relates to the technical field of energy storage batteries, and provides a method for preparing lithium difluorobisoxalate phosphate. The method includes: S1, providing a concentrated solution of lithium difluorobisoxalate phosphate and lithium difluorophosphate; Add solvent A and solvent B to the concentrated solution for extraction, collect phase B extract, carry out vacuum distillation, and dry to obtain lithium difluorobisoxalate phosphate solid. The preparation method of the invention solves the problem that lithium difluorobisoxalate phosphate is difficult to separate from lithium difluorobisoxalate phosphate, and the obtained lithium difluorobisoxalate phosphate product has high purity and low free acid content, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to the technical field of energy storage batteries, and more particularly, to a method for preparing lithium difluorobisoxalate phosphate, a non-aqueous electrolyte solution comprising the lithium difluorobisoxalate phosphate prepared by the above method, and A battery containing the non-aqueous electrolyte. Background technique [0002] Lithium difluorobisoxalate phosphate is mainly used as an additive for non-aqueous electrolyte batteries such as lithium-ion batteries and lithium-ion capacitors. After the additive is added, the electrolyte has excellent high temperature and high pressure performance, and a more stable solid electrolyte boundary film structure can be formed on the surface of the positive electrode material, thereby improving the cycle performance of the battery. [0003] At present, the preparation methods of the additive mainly include the following two: [0004] CN102216311B adopts lithium hexafluorop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574H01M10/0568
CPCC07F9/65748H01M10/0568Y02E60/10
Inventor 冯天明陈步天余意李菲何凤荣
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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