Method for producing lithium tetrafluoroborate solution

一种四氟硼酸锂、制造方法的技术，应用在四氟硼酸、最终产品制造、可持续制造/加工等方向，能够解决危险、水分残留、无法用锂电池用途等问题，达到反应收率高、反应的控制容易的效果

Active Publication Date: 2014-04-16
ZHEJIANG SINO NITROGEN KANGPENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to dehydrate the hydrated salt, heating at about 200°C is required, so not only the decomposition of lithium tetrafluoroborate (LIBF 4 →LIF+BF 3 ), the purity is reduced, and moisture remains, so it cannot be used for lithium batteries
In the ether method, the anhydrous salt is obtained through the reaction of the complex of boron trifluoride and methyl ether or ether and lithium fluoride. Since lithium tetrafluoroborate is insoluble in ether, it has the following disadvantages: it is difficult to obtain lithium batteries that meet the requirements. Lithium tetrafluoroborate of the quality used; in addition to the use of dangerous ethers; etc.

Method used

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  • Method for producing lithium tetrafluoroborate solution
  • Method for producing lithium tetrafluoroborate solution
  • Method for producing lithium tetrafluoroborate solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In a 500 mL three-necked glass flask, 18.8 g of lithium fluoride was added to 350.0 g of diethyl carbonate for mixing and dispersion. 4.1 g (27.0 mmol) of lithium hexafluorophosphate was added to the mixed dispersion liquid, cooled and maintained at 15°C, and boron trifluoride gas diluted with nitrogen to 62% by volume was passed through a gas introduction tube equipped with a mass flow controller. bubbling. The reaction was terminated when 44.7 g of boron trifluoride was consumed. Among them, the content of lithium hexafluorophosphate was 17 times the molar ratio of 1.56 mmol which is 0.028 g (moisture concentration: 68 mass ppm) of the total water contained in diethyl carbonate, lithium fluoride, and boron trifluoride. Lithium fluoride and boron trifluoride are reacted through the above steps to generate lithium tetrafluoroborate while removing water. The reaction solution obtained at this time had an acidic impurity concentration of 78 mass ppm, a water concentrati...

Embodiment 2

[0048] In a 500 mL three-necked glass flask, 18.8 g of lithium fluoride was added to 350.0 g of ethyl methyl carbonate, and mixed and dispersed. 4.1 g (27.0 mmol) of lithium hexafluorophosphate was added to the mixed dispersion liquid, cooled and maintained at 15°C, and boron trifluoride gas diluted with nitrogen to 63% by volume was passed through a gas introduction tube equipped with a mass flow controller. bubbling. The reaction was terminated when 44.8 g of boron trifluoride was consumed. Among them, the content of lithium hexafluorophosphate was 17 times the molar ratio of 1.61 mmol which is 0.029 g (moisture concentration: 70 mass ppm) of the total water contained in ethyl methyl carbonate, lithium fluoride, and boron trifluoride. Lithium fluoride and boron trifluoride are reacted through the above steps to generate lithium tetrafluoroborate while removing water. The reaction solution obtained at this time had an acidic impurity concentration of 84 mass ppm, a water co...

Embodiment 3

[0050] In a 500 mL three-necked glass flask, 18.8 g of lithium fluoride was added to 350.0 g of dimethyl carbonate for mixing and dispersion. 4.1 g (27.0 mmol) of lithium hexafluorophosphate was added to the mixed dispersion liquid, cooled and maintained at 15°C, and boron trifluoride gas diluted with nitrogen to 62% by volume was passed through a gas introduction tube equipped with a mass flow controller. bubbling. The reaction was terminated when 44.7 g of boron trifluoride was consumed. Among them, the content of lithium hexafluorophosphate was 15 times the molar ratio of 1.84 mmol which was 0.033 g (moisture concentration: 80 mass ppm) of the total water contained in dimethyl carbonate, lithium fluoride, and boron trifluoride. Lithium fluoride and boron trifluoride are reacted through the above steps to generate lithium tetrafluoroborate while removing water. The reaction solution obtained at this time had an acidic impurity concentration of 69 mass ppm, a water concentr...

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Abstract

This method for producing a lithium tetrafluoroborate solution for lithium battery electrolyte solutions comprises: a reaction step wherein lithium fluoride and boron trifluoride are reacted with each other in a chain carbonic acid ester that serves as a solvent, thereby producing lithium tetrafluoroborate and obtaining a reaction solution that is obtained by dissolving the lithium tetrafluoroborate in the solvent; a water removal step wherein a water remover is added into the reaction solution; an acidic impurity removal step wherein acidic impurities are removed by concentrating the reaction solution after the water removal step; and a dilution step wherein the concentrated solution after the acidic impurity removal step is diluted. This production method is capable of providing a method for producing a lithium tetrafluoroborate solution for lithium battery electrolyte solutions, said lithium tetrafluoroborate solution having an acidic impurity concentration reduced to 50 ppm by mass or less and a water concentration reduced to 15 ppm by mass or less.

Description

technical field [0001] The present invention relates to a method for producing a solution of lithium tetrafluoroborate useful as an electrolyte for lithium batteries. Background technique [0002] Two known methods for synthesizing lithium tetrafluoroborate (LIBF4) include a wet method and an ether method. In the wet method, hydrated salts (LIBF 4 ·H 2 O). In order to dehydrate the hydrated salt, heating at about 200°C is required, so not only the decomposition of lithium tetrafluoroborate (LIBF 4 →LIF+BF 3 ), the purity is reduced, and moisture remains, so it cannot be used for lithium batteries. In the ether method, the anhydrous salt is obtained through the reaction of the complex of boron trifluoride and methyl ether or ether and lithium fluoride. Since lithium tetrafluoroborate is insoluble in ether, it has the following disadvantages: it is difficult to obtain lithium batteries that meet the requirements. use of lithium tetrafluoroborate of high quality; in addit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0568C01B35/06H01M10/0569
CPCH01M10/0569H01M10/0568Y02E60/12H01M10/052C01B35/06H01M2300/0028Y02E60/122C01B35/066Y02E60/10Y02P70/50
Inventor 新免益隆辻冈章一太郎良哲佐藤敬二森中孝敬
Owner ZHEJIANG SINO NITROGEN KANGPENG CHEM CO LTD
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