Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of lithium difluorooxalate borate

A technology of lithium difluorooxalate borate and anhydrous oxalic acid is applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc. Acid gas and tail gas treatment are cumbersome and other problems, to achieve the effects of low cost, improved purity and mild reaction

Active Publication Date: 2022-04-08
ZHANGJIAGANG HUASHENG CHEM CO LTD
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that a large amount of acid gas will be produced in the reaction process, and the tail gas treatment is cumbersome; moreover, the raw material lithium tetrafluoroborate is expensive and the cost is high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of lithium difluorooxalate borate of this embodiment 1, comprises the steps:

[0027] Get anhydrous oxalic acid 100g (1.11mol) and anhydrous lithium chloride 42.5g (1mol), be placed in the reaction vessel of dry band stirrer, under nitrogen atmosphere, add 285g acetonitrile (moisture content is 210ppm), the reaction raw materials in the reaction vessel were stirred under normal pressure and temperature conditions of 15°C, and reacted for 12 hours. During the reaction, a small amount of acid gas escaped, and the tail gas was absorbed by water; anhydrous oxalic acid and anhydrous Lithium chloride water reacts to generate lithium hydrogen oxalate; after the above reaction is completed, add boron trifluoride etherate complex (boron trifluoride content is 47%) 145g in the reaction vessel, continue to stir and react for 12 hours, generate difluoro Lithium oxalate borate; after the reaction is completed, under a nitrogen atmosphere, filter the reac...

Embodiment 2

[0029] A kind of preparation method of lithium difluorooxalate borate of this embodiment 2, comprises the steps:

[0030] Get anhydrous oxalic acid 180g (2mol) and anhydrous lithium chloride 42.5g (1mol), be placed in the reaction vessel of dry band stirrer, under nitrogen atmosphere, add 1200g dimethyl carbonate (moisture content) again in reaction vessel content of 120ppm), the reaction raw materials in the reaction vessel were stirred under normal pressure and temperature conditions of 80°C, and reacted for 1 hour. During the reaction, a small amount of acid gas escaped, and the tail gas was absorbed by water; the anhydrous oxalic acid React with anhydrous lithium chloride to generate lithium hydrogen oxalate; After the above reaction is completed, add boron trifluoride dimethyl carbonate complex (boron trifluoride content is 43%) 160g in the reaction vessel, continue stirring reaction 1.5 hour, generate difluorooxalate lithium borate; after the reaction is completed, drop ...

Embodiment 3

[0032] A kind of preparation method of lithium difluorooxalate borate of this embodiment 3 comprises the steps:

[0033] Get anhydrous oxalic acid 90g (1mol) and anhydrous lithium chloride 42.5g (1mol), be placed in the reaction vessel of dry band stirrer, under nitrogen atmosphere, add 420g acetone (moisture content is 283ppm ), the reaction raw materials in the reaction vessel were stirred under normal pressure and at a temperature of 55°C, and reacted for 3 hours. During the reaction, a small amount of acid gas escaped, and the tail gas was absorbed by water; the anhydrous oxalic acid and anhydrous Lithium chloride reacts to generate lithium hydrogen oxalate; after the above reaction is completed, add boron trifluoride carbonic acid acetonitrile complex (boron trifluoride content is 62%) 120g in the reaction vessel, continue stirring reaction 3 hours, generate difluoro Lithium oxalate borate; after the reaction is completed, cool down to room temperature, and under a nitrog...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of lithium difluorooxalate borate, which comprises the following steps: (1) take anhydrous oxalic acid and anhydrous lithium chloride, place them in a reaction vessel, and add them to the reaction vessel under a nitrogen atmosphere Aprotic polar solvent, react at 10-80°C and under stirring for 1-12 hours; react anhydrous oxalic acid with anhydrous lithium chloride to generate lithium hydrogen oxalate; (2) add boron trifluoride to the reaction vessel Compound, continue to react for 1 to 12 hours to generate lithium difluorooxalate borate; (3) filter the reaction solution after the reaction of step (2) at room temperature, remove the incompletely reacted solid raw material, and then filter to obtain The filtrate is concentrated and recrystallized, then washed and filtered with a non-polar solvent, and finally dried to obtain a solid lithium difluorooxalate borate product. The method has mild reaction, simple process, low production cost, and is economical and environment-friendly, can obtain high-purity lithium difluorooxalate borate, and is relatively suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of electrolyte lithium salt used in the lithium ion battery industry, and in particular relates to a preparation method of lithium difluorooxalate borate. Background technique [0002] Lithium difluorooxalate borate is a new type of material to replace the existing electrolyte lithium salt. Its unique chemical structure combines the advantages of lithium bisoxalate borate and lithium tetrafluoroborate, making it have better high and low temperature performance and higher electrical conductivity. efficiency and good thermal stability, while improving the abuse resistance of lithium-ion batteries. Due to its excellent electrochemical properties, lithium difluorooxalate borate has become a research hotspot of new materials for lithium batteries and has broad market application prospects. [0003] At present, the preparation method of lithium difluorooxalate borate mainly contains following two kin...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 杨志勇沈鸣李伟锋张先林陆海媛
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD