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Series one-pot synthesis method of lithium oxalyldifluroborate

A technology of lithium difluoroborate oxalate and its 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 silyl oxalate synthesis route that is not suitable for rapid production requirements Complicated and complicated problems, to achieve the effect of fast response and low energy consumption

Active Publication Date: 2015-03-04
周阳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis route of silyl oxalate is cumbersome and complicated, and it is not suitable for rapid production requirements

Method used

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  • Series one-pot synthesis method of lithium oxalyldifluroborate

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Experimental program
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Effect test

Embodiment 1

[0031] Lithium oxalate difluoroborate was prepared from boron trifluoride ether solution, lithium oxalate, trimethylmethoxysilane and oxalic acid. In a reaction flask equipped with a magnetic stirrer, 101.9 g of lithium oxalate was added, 500 mL of acetonitrile was added, stirring was started, and 288 g of boron trifluoride-diethyl ether solution was slowly added dropwise therein. Continue to stir after the dropwise addition is complete. After all the solid materials are dissolved, add 90g of oxalic acid and slowly dropwise add 208.4g of trimethylmethoxysilane. The reaction pressure is 0.1Mpa, and the reaction is carried out at 20°C for 10 hours. To fully convert the raw materials. Stop heating and cool to room temperature naturally. The solvent and by-products were distilled off under reduced pressure. The reaction solution was concentrated and crystallized, and filtered under nitrogen protection. The filter cake was vacuum-dried at a temperature of 60-80° C. for 48...

Embodiment 2

[0034] Lithium oxalate difluoroborate was prepared from boron trifluoride ether solution, lithium fluoride, trimethylethoxysilane and oxalic acid.

[0035] In a reactor equipped with a heating and magnetic stirring device, 25.9 g of lithium fluoride and 500 mL of dimethyl carbonate were added, stirring was started, and 144.2 g of boron trifluoride-diethyl ether solution was slowly added dropwise therein. After the dropwise addition is completed, continue to stir until all solid materials are dissolved. Add 90g of oxalic acid, slowly add 236.5g of trimethylethoxysilane at room temperature, the reaction pressure is 0.2Mpa, heat to 80°C, and react for 2 hours. To fully convert the raw materials. Stop heating and cool to room temperature naturally.

[0036] The reaction solution was concentrated and crystallized, and filtered under nitrogen protection. The filter cake was vacuum-dried at a temperature of 60-80° C. for 48 hours. Finally, 115 g of white powd...

Embodiment 3

[0039] Lithium oxalate difluoroborate was prepared from boron trifluoride acetonitrile solution, lithium fluoride, boron trichloride and oxalic acid.

[0040] In a reactor equipped with a heating and magnetic stirring device, 77.7 g of lithium fluoride and 1000 mL of diethyl carbonate were added, stirring was started, and 144.2 g of boron trifluoride-diethyl ether solution was slowly added dropwise therein. After the dropwise addition, continue to stir until all solid materials are dissolved, slowly add 235.4g of boron trichloride and 270g of oxalic acid at room temperature, the reaction pressure is 0.15Mpa, heat to 60°C, and react for 4 hours. To fully convert the raw materials. Stop heating and cool to room temperature naturally.

[0041] The reaction solution was concentrated and crystallized, and filtered under nitrogen protection. The filter cake was vacuum-dried at a temperature of 60-80° C. for 48 hours. Finally, 388.2 g of white powdery solids w...

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Abstract

The invention discloses a series one-pot synthesis method of lithium oxalyldifluroborate. The method is characterized by comprising the following steps: sequentially adding a solvent, a lithium salt, boron fluoride or complex thereof, oxalic acid, reaction assistants and other raw materials into a reaction kettle, and reacting at 0-100 DEG C for 2-10 hours; after the reaction finishes, discharging the solvent and byproduct out of the reaction kettle by distillation, and recovering by condensation; and recrystallizing the product, and drying to directly obtain the product with the purity of greater than 99%. The method has the advantages of high production efficiency, safe and simple operation process and no need of complicated purification by recrystallization, and is a lithium oxalyldifluroborate preparation technique suitable for industrial production.

Description

[0001] technical field [0002] The invention relates to the production, manufacture and purification technology of lithium ion battery electrolyte salt, in particular to a serial one-pot synthesis method of electrolyte salt-lithium oxalic acid difluoroborate. Background technique [0003] At present, lithium-ion batteries are the best power supply option for electric vehicles. Electrolyte is an important part of lithium-ion batteries, which determines the capacity, life and discharge rate of batteries. The electrolyte is composed of lithium salt, solvent and additives. The traditional electrolyte uses lithium hexafluorophosphate as the main lithium salt. Lithium hexafluorophosphate has a low decomposition temperature and poor conductivity at low temperatures, which limits the application of lithium-ion batteries in the field of electric vehicles. [0004] Lithium oxalate difluoroborate—LiDFOB is a new type of lithium salt. It has a high decomposition temperature, good lo...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 周阳
Owner 周阳
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