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Preparation method of lithium ion battery electrolyte salt LiODFB (lithium oxalyldifluroborate)

A technology of lithium oxalate difluoroborate and lithium oxalate difluoroborate is applied in the field of complete process for the preparation of lithium oxalate difluoroborate (LiODFB), which can solve the problems of unfavorable industrialization, high equipment requirements, and low sample purity. Achieve the effect of avoiding waste and improving utilization

Inactive Publication Date: 2015-05-20
HUNAN ZHENGYUAN ENERGY STORAGE MATERIALS & DEVICE INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, HCl is produced in the reaction of this method, which requires high equipment and is not conducive to industrialization. Moreover, the purity of the sample obtained by this patent is low, and LiODFB needs to be purified before it can be used as an electrolyte for lithium-ion batteries.

Method used

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  • Preparation method of lithium ion battery electrolyte salt LiODFB (lithium oxalyldifluroborate)
  • Preparation method of lithium ion battery electrolyte salt LiODFB (lithium oxalyldifluroborate)
  • Preparation method of lithium ion battery electrolyte salt LiODFB (lithium oxalyldifluroborate)

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 300ml of dimethyl carbonate (DMC) into the reaction kettle, add 10g of lithium oxalate, 12.38ml of boron trifluoride ether at the same time, mix well, then slowly add 1ml of boron trichloride (BCl3), react at 40°C for 12h, A liquid phase mixture is obtained. Then vacuum distillation, 40 ° C, distillation for 1 h, and then at -20 ° C, insulation for 1 h to precipitate crystals. The crude product of lithium oxalate difluoroborate (LiODFB) was obtained by filtration, and the crude product was recrystallized to obtain a high-purity lithium oxalate difluoroborate (LiODFB) product. At the same time, collect the filtered mother liquor and recrystallized mother liquor, add 5.6g oxalic acid and 0.4g aluminum trichloride (AlCl3), react at 40°C for 12h, and return the obtained liquid phase mixture to the evaporation crystallization step. Finally, the lithium oxalate difluoroborate (LiODFB) solid obtained after drying at 40°C for 1 h has a purity of 99.9% and a yield of 90%. ...

Embodiment 2

[0027] Add 100ml of acetonitrile (AN) into the reaction kettle, add 10g of lithium oxalate, 37.5ml of boron trifluoride ether at the same time, mix well, then slowly add 10g of aluminum trichloride (AlCl3), react at 100°C for 24h, and obtain a liquid phase mixture. Then vacuum distillation, 80 ° C, distillation 5h, and then at 10 ° C, insulation 12h to precipitate crystals. The crude product of lithium oxalate difluoroborate (LiODFB) was obtained by filtration, and the crude product was recrystallized to obtain a high-purity lithium oxalate difluoroborate (LiODFB) product. At the same time, collect the filtered mother liquor and recrystallized mother liquor, add 28.2g oxalic acid, 0.32mL silicon tetrachloride (SiCl4), react at 100°C for 24h, and return the obtained liquid phase mixture to the evaporation crystallization step. Finally, the lithium oxalate difluoroborate (LiODFB) solid obtained after drying at 150°C for 48 hours had a purity of 99.9% and a yield of 92%.

Embodiment 3

[0029] Add 500ml of ethyl methyl carbonate (EMC) into the reaction kettle, add 10g of lithium oxalate, 24.76ml of boron trifluoride ether at the same time, mix well, then slowly add 5mL of silicon tetrabromide (SiBr4), react at 70°C for 18h, A liquid phase mixture is obtained. Then vacuum distillation, 60 ℃, distillation 3h, and then at -5 ℃, insulation 6.5h to precipitate crystals. The crude product of lithium oxalate difluoroborate (LiODFB) was obtained by filtration, and the crude product was recrystallized to obtain a high-purity lithium oxalate difluoroborate (LiODFB) product. At the same time, collect the filtered mother liquor and recrystallized mother liquor, add 16.9g oxalic acid and 1.6g aluminum trichloride (AlCl3), react at 70°C for 18h, and return the obtained liquid phase mixture to the evaporation crystallization step. Finally, the lithium oxalate difluoroborate (LiODFB) solid was obtained after drying at 95°C for 24.5 hours, with a purity of 99.9% and a yield ...

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Abstract

The invention relates to a preparation method of lithium ion battery electrolyte salt LiODFB (lithium oxalyldifluroborate). The method comprises the following steps: performing catalytic synthesis of lithium oxalate and boron trifluoride diethyl ether in a solvent of DMC (dimethyl carbonate) and the like to obtain a liquid-phase mixture and a little unreacted lithium oxalate solid, performing filtration, and then performing evaporative crystallization to obtain crude LiODFB; recrystallizing the crude LiODFB to meet the requirement of lithium ion battery electrolyte salt; and collecting filtered mother liquid and crystallization mother liquid, adding oxalate and a catalyst, performing catalytic conversion to obtain a liquid-phase mixture which mainly contains LiODFB, and performing evaporative crystallization again. The technological process is low in cost, the purity of the prepared LiODFB is above 99.9%, the yield is above 90%, and the method is convenient to operate, has favorable economic benefits and environmental benefits and is suitable for industrial production.

Description

technical field [0001] The invention relates to a complete process flow for the preparation of lithium-ion battery electrolyte salts, in particular to a complete process flow for the preparation of lithium oxalate difluoroborate (LiODFB), which belongs to the technical field of lithium-ion battery materials. Background technique [0002] Electrolyte salt is an important part of lithium-ion batteries, and its research and development is very important to the performance and development of lithium-ion secondary batteries. Lithium oxalate difluoroborate (LiODFB) can be regarded as half lithium oxalate borate (LiBOB) and half lithium tetrafluoroborate (LiBF4) in terms of chemical structure, and its performance cleverly combines the advantages of both. Lithium oxalate difluoroborate (LiODFB) has excellent high and low temperature performance, and has good electrochemical performance at -20°C and 60°C; it can well support current collector copper foil and aluminum foil; it has goo...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/025
Inventor 周宏明孙文佼李荐
Owner HUNAN ZHENGYUAN ENERGY STORAGE MATERIALS & DEVICE INST
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