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Preparation method of lithium difluoro (oxalato) borate

A technology of lithium difluorooxalate borate and lithium oxalate, which is applied in chemical instruments and methods, secondary batteries, lithium batteries, etc., and can solve the problems of complicated LiODFB method and complicated impurity removal operation

Pending Publication Date: 2022-01-25
湖南法恩莱特新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing methods for preparing LiODFB are relatively complicated, especially the impurity removal operation is relatively complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] This embodiment has prepared a kind of LiODFB, and specific process is:

[0062] S1. Preparation of BF 3 :

[0063] S1a. First reduce the vacuum degree of the reactor with polytetrafluoroethylene lining to below 0.01MPa, then pass high-purity nitrogen gas (purity ≥ 99.999%) to normal pressure, and then vacuumize again, and repeat three times in order to remove Oxygen, moisture and other impurities in the reactor;

[0064] S1b. Add 1mol B to the system in step S1a 2 o 3 (purchased from Sigma-Aldrich Co.LLC, purity ≥ 99.98%), after nitrogen replacement in turn, vacuumize to below 0.01MPa, and then feed F into the system 2 (purchased from Shandong Ruihua Fluorine Industry Co., Ltd., purity ≥ 99.99%) to close to 0.02MPa;

[0065] Access F 2 Will and B 2 o 3 Gas-solid reaction occurs, which will cause the temperature and pressure of the system to rise during the process; during the reaction process, the temperature of the control process is about 85°C;

[0066] S1c....

Embodiment 2

[0074] This embodiment has prepared a kind of LiODFB, and the difference of specific process and embodiment 1 is:

[0075] (1) In step S1c, the temperature of the cold trap is set to -98°C.

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Abstract

The invention discloses a preparation method of lithium difluoro (oxalato) borate, which comprises the following steps of s1, reacting fluorine gas with diboron trioxide to obtain boron fluoride; and s2, reacting the boron fluoride with lithium oxalate, and purifying the mixture to obtain the lithium difluoro (oxalato) borate. According to the preparation method of the LiODFB provided by the invention, the preparation process can be simplified by matching the preparation raw materials and adjusting the charging sequence, especially the purification process of an intermediate product and a final product, so that the high-purity LiODFB can be obtained.

Description

technical field [0001] The invention belongs to the technical field of secondary battery electrolyte, and in particular relates to a preparation method of lithium difluorooxalate borate. Background technique [0002] With the continuous development of the new energy field, secondary batteries, especially lithium-ion secondary batteries, occupy most of the market; electrolyte is an important part of secondary batteries, and its quality directly affects the optimization and improvement of battery performance . As the core component of the electrolyte, the electrolyte must have the advantages of high conductivity, good chemical and electrochemical stability, a wide range of usable temperature, and good safety. [0003] The most widely used electrolyte is lithium hexafluorophosphate (LiPF 6 ), lithium bisoxalate borate (LiBOB) and lithium tetrafluoroborate (LiBF 4 )Wait. LiPF 6 With its good comprehensive performance, it has been widely used. But LiPF 6 It is very sensiti...

Claims

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Application Information

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IPC IPC(8): C07F5/02H01M10/052H01M10/0568
CPCC07F5/022H01M10/052H01M10/0568H01M2300/0025Y02E60/10
Inventor 邵俊华李海杰孔东波张利娟龚国斌王郝为郭飞闫国锋宋东亮王亚洲侯红歧韩飞
Owner 湖南法恩莱特新能源科技有限公司
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