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Method for synthesizing an electrolyte lithium salt: lithium difluoro(oxalate)borate

A technology of lithium difluorooxalate borate and synthesis method, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., and can solve the problem of low oxidation potential, poor thermal stability, and influence on electrolyte Performance and other issues, to achieve the effect of high reaction conversion rate and easy industrial production

Active Publication Date: 2018-02-16
浙江圣持新材料科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

LiPF 6 It is the largest category at present and has the advantage of high electrical conductivity, but the disadvantage is that it is easy to absorb moisture and hydrolyze, and has poor thermal stability; while LiBF 4 than LiPF 6 It has better low-temperature performance, but its oxidation potential is lower; LiBOB has better high-temperature performance and film-forming performance, but its solubility and conductivity in carbonate solvents are lower than LiPF 6
In this route, the conversion rate of lithium tetrafluoroborate is high, the reaction conditions are mild, the raw materials are simple, and it is easy to industrialized production. However, HCl is generated in the reaction process, which causes corrosion to the reaction equipment on the one hand, and inevitably introduces more chlorine on the other hand. Ionic impurities, affecting the performance of the electrolyte
[0008] At present, limited by the preparation cost, lithium difluorooxalate borate has not been applied on a large scale, and it is mainly used as an additive for lithium-ion battery electrolyte

Method used

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  • Method for synthesizing an electrolyte lithium salt: lithium difluoro(oxalate)borate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: the synthesis of lithium difluorooxalate borate (LiODFB)

[0037] (1) Synthesis of condensate of silane oxalic acid

[0038] In a flask equipped with a magnetic stirrer, a thermometer, a reflux condenser and a nitrogen conduit, add 50 g of oxalic acid, stir and raise the temperature to 80°C, then slowly add 71.7 g of dimethyldichlorosilane, and the reaction ends after 24 hours. The reaction system was distilled off the solvent under reduced pressure at 120° C. to obtain 80.1 g of a colorless viscous product, which was a condensate of silane oxalic acid. The obtained product was analyzed, and the result showed that the purity was 99.3% (calculated by nuclear magnetic spectrum).

[0039] (2) Synthesis of lithium difluorooxalate borate (LiODFB)

[0040] Weigh 20g lithium tetrafluoroborate, 32.7g condensate of silane oxalic acid in the above-mentioned step (1), 150g dimethyl carbonate in the glove box, join in the three-necked flask that magnetic stirring, t...

Embodiment 2

[0042] Embodiment 2: the synthesis of lithium difluorooxalate borate (LiODFB)

[0043] (1) Synthesis of condensate of silane oxalic acid

[0044] In a flask equipped with a magnetic stirrer, a thermometer, a reflux condenser and a nitrogen conduit, add 50 g of oxalic acid, stir and raise the temperature to 50 ° C, then slowly add 52.5 g of dimethyl monochlorosilane, and the reaction ends after 24 hours. The reaction system was distilled off the solvent under reduced pressure at 120° C. to obtain 78.6 g of a colorless viscous product, which was a condensate of silane oxalic acid. The obtained product was analyzed, and the result showed that the purity was 99.1% (calculated by nuclear magnetic spectrum).

[0045] (2) Synthesis of lithium difluorooxalate borate (LiODFB)

[0046] In the glove box, take by weighing 30g lithium tetrafluoroborate, the condensate of silane oxalic acid in the above step (1) of 49.1g, the diethyl carbonate of 240g, join in the three-necked flask that ...

Embodiment 3

[0048] Embodiment 3: the synthesis of lithium difluorooxalate borate (LiODFB)

[0049] (1) Synthesis of condensate of silane oxalic acid

[0050] In a flask equipped with a magnetic stirrer, a thermometer, a reflux condenser and a nitrogen conduit, add 50g of oxalic acid, stir and raise the temperature to 60°C, then slowly add 120.7g of trimethylchlorosilane, and the reaction ends after 30h. The reaction system was distilled off the solvent under reduced pressure at 120° C. to obtain 123.5 g of a colorless viscous product, which was a condensate of silane oxalic acid. The obtained product was analyzed, and the result showed that the purity was 98.7% (calculated by nuclear magnetic spectrum).

[0051] (2) Synthesis of lithium difluorooxalate borate (LiODFB)

[0052] Weigh 20g lithium tetrafluoroborate, 51.6g condensate of silane oxalic acid in the above-mentioned step (1), 150g diethyl carbonate in the glove box, join in the three-necked flask that magnetic stirring, thermome...

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Abstract

The invention relates to a method for synthesizing an electrolyte lithium salt: lithium difluoro(oxalate)borate. The method comprises the following steps: 1) performing reaction on a silane compound with oxalic acid to obtain a condensation compound of silane and oxalic acid; 2) performing reaction on lithium tetrafluoroborate with the condensation compound of the silane and oxalic acid in a solvent to obtain a crude product; and 3) performing recrystallization on the crude product to the obtain lithium difluoro(oxalate)borate. The synthesizing method not only can be used to obtain the high-purity lithium difluoro(oxalate)borate, but also can effectively reduce the acidity and Cl content of the lithium difluoro(oxalate)borate.

Description

technical field [0001] The invention relates to the field of electrolyte preparation, in particular to a method for synthesizing electrolyte lithium salt lithium difluorooxalate borate. Background technique [0002] Lithium-ion battery is a secondary battery with superior performance, which is currently widely used in 3C fields, new energy vehicles, military products and other fields. Its four key materials include positive electrode, negative electrode, diaphragm and electrolyte. The electrolyte plays a role in conducting current between the positive and negative electrodes of the battery. It is called the "blood" of lithium-ion batteries and plays a decisive role in lithium batteries. effect. [0003] The types of lithium-ion battery electrolytes include liquid organic electrolytes, gel polymer electrolytes, and solid polymer electrolytes. Among them, the liquid organic electrolyte is currently the most commercially used type, and its main components include organic solv...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 王志光吴宪宏官宝红汪贤玉周转忠金宇芬
Owner 浙江圣持新材料科技有限公司
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