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Preparation method of electronic-grade lithium difluoro bis-oxalate phosphate

A technology of lithium difluorobis oxalate phosphate and lithium hexafluorophosphate, which is applied in chemical instruments and methods, circuits, lithium compounds, etc., can solve problems such as adverse effects on battery characteristics of non-aqueous electrolyte batteries, unsuitable for industrial production, etc. High quality, avoiding many reaction steps, simple and convenient operation

Active Publication Date: 2018-11-30
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product prepared by this method is difficult to remove because it contains higher chlorine compounds and free acid, which will have a negative impact on the battery characteristics of the non-aqueous electrolyte battery, and is not suitable for industrialized production.

Method used

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Examples

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Effect test

preparation example Construction

[0017] A method for preparing electronic-grade lithium difluorobisoxalate phosphate, the method comprising the following steps: weighing oxalic acid and lithium hexafluorophosphate and placing them in a reaction device, adding a non-aqueous solvent, adding hexamethyldisilazane dropwise, and fully stirring for reaction , The resulting reaction solution was filtered, and then concentrated under reduced pressure to obtain a solid product, which was further recrystallized to obtain electronic grade lithium difluorobisoxalate phosphate.

[0018] The non-aqueous solvent is a high-purity organic solvent through dewatering treatment, the purity of the organic solvent is greater than 99.95%, and the water content is less than 10ppm; the organic solvent is dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, One or more of diethyl ether, ethylene glycol dimethyl ether, ethanol, acetonitrile, dichloromethane, and 1,2-dichloromethane.

[0019] The recrystallization method is to ...

Embodiment 1

[0029] In a glove box with a dew point of -50°C, add 200 g of diethyl carbonate dehydrated to 10 ppm into a three-necked reaction flask, and add 30.4 g of lithium hexafluorophosphate and 37.8 g of lithium oxalate at the same time. The molar ratio of lithium hexafluorophosphate to oxalic acid is 1:2.1. The reaction bottle was taken out of the glove box, and placed on a constant temperature magnetic stirring device, and 67.8g of hexamethyldisilazane was accurately weighed. The molar ratio of lithium hexafluorophosphate to hexamethyldisilazane was 1:2.1. The dropping funnel was added dropwise into the reaction bottle, and the reaction was fully stirred, and the reaction was completed after 4 hours of reaction. The reaction solution was filtered and concentrated under reduced pressure to obtain 69.7 g of crude product. The resulting product was added to 250 g of ether, dissolved and filtered to obtain a product quality of 46.4 g, a theoretical yield of 50.8 g, and a product yield o...

Embodiment 2

[0031] In a glove box with a dew point of -50°C, 250 g of dimethyl carbonate dehydrated to 10 ppm was added to a three-necked reaction flask, and 36.3 g of lithium hexafluorophosphate and 44.0 g of oxalic acid were added at the same time. The molar ratio of lithium hexafluorophosphate to oxalic acid was 1:2.05. The three-necked reaction bottle was taken out of the glove box, and placed on a constant temperature magnetic stirring device, and 81.0 g of hexamethyldisilazane was accurately weighed. The molar ratio of lithium hexafluorophosphate to hexamethyldisilazane was 1:2.1. The constant pressure dropping funnel was added dropwise into the reaction bottle, and the reaction was fully stirred, and the reaction was completed after 4 hours of reaction. The reaction solution was filtered and concentrated under reduced pressure to obtain 77.2 g of crude product, which was added to 150 g of dichloromethane, dissolved and filtered to obtain a product quality of 53.9 g, a theoretical yi...

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Abstract

The invention discloses a preparation method of electronic-grade lithium difluoro bis-oxalate phosphate. The method comprises the following steps: weighing oxalic acid and lithium hexafluorophosphatein a reaction apparatus, adding a non-aqueous solvent, dropping hexamethyl-disilazane, fully stirring the materials for a reaction to obtain a reaction solution, filtering the reaction solution, performing vacuum concentration after filtering to obtain a solid product, and performing recrystallization to obtain the electronic-grade lithium difluoro bis-oxalate phosphate. The preparation method employs the raw materials with low cost to prepare the lithium difluoro bis-oxalate phosphate, the method has the advantages of easy and convenient operation, avoids the defects of multiple reaction stepand complex operation of the other methods, and excessive impurities of the final product, guarantees the purity and quality of the product, and the product having high quality and high purity can beobtained, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of additives for nonaqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors, in particular to a method for preparing electronic-grade lithium difluorobisoxalate phosphate. Background technique [0002] Lithium difluorobisoxalate phosphate is mainly used as an additive for non-aqueous electrolyte batteries such as lithium-ion batteries and lithium-ion capacitors. After adding this additive, the electrolyte has excellent high temperature and high pressure resistance, and a more stable solid electrolyte boundary membrane structure can be formed on the surface of the positive electrode material to improve the cycle performance of the battery. The currently known preparation methods of this additive mainly include the following types. [0003] Patent No. US201000267984 proposes mixing lithium hexafluorophosphate and lithium oxalate in a pressure-resistant container, then heating to 150°C-180...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00H01M10/0567H01M10/42H01G11/64
CPCC01D15/00C01P2006/40C01P2006/80H01G11/64H01M10/0567H01M10/4235Y02E60/10
Inventor 赵经纬洪果信勇孙安乐
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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