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Catalytic synthesis method of lithium difluoro(oxalato)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 problems such as complicated process, difficult operation, and high price , to achieve broad application prospects, avoid tail gas pollution, and improve the effect of reaction speed

Inactive Publication Date: 2017-01-25
LUOYANG HEMENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the raw material LiBF4 is expensive, more sensitive to moisture, difficult to operate, and the purity of the obtained samples is low
[0006] S.S.Zhang et al. used boron trifluoride diethyl ether and lithium oxalate as raw materials to directly react the crude product of LiODFB, and then used dimethyl carbonate as solvent to purify the sample by extraction and recrystallization. The yield is low, the purity of the LiODFB sample obtained is low, and the process is complicated
[0007] The method for obtaining lithium tetrafluoroborate and lithium difluorooxalate borate disclosed in Chinese patent CN102702243B requires two kinds of catalysts, complex process, many steps and low product yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. First replace all production reaction vessels with high-purity nitrogen, then pass in high-purity nitrogen, and add materials under the protection of nitrogen;

[0027] 2. Add 30.57 kilograms of dried lithium oxalate anhydrous and 65 kilograms of boron trifluoride dimethyl carbonate complex into a 1000-liter stainless steel stirring reactor equipped with 300 kilograms of dimethyl carbonate, and stir to dissolve;

[0028] 3. Then add 0.9 kg of 1,8-diazabicyclo[5.4.0]undec-7-ene into the stirred reactor as a catalyst; heat while stirring, control the reaction temperature to 80°C, fully React for 7 hours to obtain a mixed solution of lithium difluorooxalate borate and lithium tetrafluoroborate;

[0029] 4. Under nitrogen protection, add 27 kg of anhydrous oxalic acid to the mixed solution of lithium difluorooxalate borate and lithium tetrafluoroborate, control the reaction temperature at 75°C, and the pressure at an absolute pressure of 60KPa, and react for 6 hours to m...

Embodiment 2

[0032] 1. First replace all production reaction vessels with high-purity nitrogen, then pass in high-purity nitrogen, and add materials under the protection of nitrogen;

[0033] 2. Add 30.57 kilograms of dried lithium oxalate anhydrous and 65 kilograms of boron trifluoride dimethyl carbonate complex into a 1000-liter stainless steel stirring reactor equipped with 300 kilograms of dimethyl carbonate, and stir to dissolve;

[0034] 3. Then add 0.8 kg of 1,5-diazabicyclo[4,3,0]nonene-5 into the stirred reactor as a catalyst; heat while stirring, control the reaction temperature to 70°C, and fully react After 8 hours, a mixed solution of lithium difluorooxalate borate and lithium tetrafluoroborate was obtained;

[0035] 4. Under the protection of high-purity nitrogen, add 27 kg of anhydrous oxalic acid to the mixed solution of lithium difluorooxalate borate and lithium tetrafluoroborate, control the reaction temperature at 60°C, and the pressure at an absolute pressure of 60KPa, ...

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Abstract

The invention relates to a catalytic synthesis method of lithium difluoro(oxalato)borate, belonging to the technical fields of new energy material preparation and chemical industry. The method comprises the following steps: (1) after all production reaction vessels are replaced with high-purity nitrogen, adding materials in a high-purity nitrogen protective atmosphere; (2) in a closed dry reactor, adding a certain amount of dry waterless lithium oxalate and a certain amount of boron trifluoride complex into an organic solvent reactor, and dissolving to prepare a solution; (3) adding a certain amount of catalyst, and sufficiently reacting at specified temperature to obtain a lithium difluoro(oxalato)borate-lithium tetrafluoroborate mixed solution; (4) adding a certain amount of waterless oxalic acid into the lithium difluoro(oxalato)borate-lithium tetrafluoroborate mixed solution, and sufficiently reacting under the control of specified temperature, specified pressure and a tail gas absorption solution, thereby obtaining the lithium difluoro(oxalato)borate solution. The catalytic synthesis method of lithium difluoro(oxalato)borate has the advantages of short reaction time, high product yield, low equipment investment, no pollution and wide application prospects, and is simple to operate.

Description

technical field [0001] The invention relates to a catalytic synthesis method of lithium difluorooxalate borate, belonging to the technical field of lithium ion battery material synthesis. Background technique [0002] Lithium-ion battery electrolyte is an important part of lithium-ion batteries and a key core component of the electrolyte. The electrolyte must have the advantages of high conductivity, good chemical and electrochemical stability, wide usable temperature range, and good safety. [0003] At present, the commonly used electrolytes mainly include lithium hexafluorophosphate (LiPF6), lithium bisoxalate borate (LiBOB), and lithium tetrafluoroborate (LiBF4), among which LiPF6 has been widely used because of its good comprehensive performance. Because LiPF6 is very sensitive to moisture, the preparation process is complicated. In addition, LiPF6 itself has a low thermal decomposition temperature (200°C), and it is easy to decompose in organic solvents (about 80°C); it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02H01M10/0568
CPCC07F5/022H01M10/0568Y02E60/10
Inventor 李绍通
Owner LUOYANG HEMENG TECH CO LTD