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Lithium tetrafluoro oxalate-phosphate preparation method

A technology of lithium tetrafluorooxalate phosphate and lithium hexafluorophosphate, which is applied in the field of lithium-ion batteries, can solve the problems of low product purity, bad battery characteristics affecting chlorine compounds, and unsuitability for industrial production, and achieves simple preparation methods, simple and convenient production processes, and overcoming The effect of multiple reaction steps

Active Publication Date: 2016-01-06
TIANJIN JINNIU POWER SOURCES MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product prepared by this method also contains lithium difluorobis(oxalato)phosphate, and the purity of the product is low, and the product prepared by this method also contains chlorine compounds that adversely affect the characteristics of the battery, which is not suitable for industrial production.

Method used

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  • Lithium tetrafluoro oxalate-phosphate preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] At room temperature, add 101.9g of lithium oxalate and 1300g of HF into reaction vessel A with a jacket, and stir overnight to completely dissolve lithium oxalate in HF. 200g of anhydrous HF was passed into the reaction kettle B in advance, and then 416.46g of phosphorus pentachloride was slowly added, and a low-temperature cooling medium was passed into the jacket to control the temperature, and then the phosphorus pentafluoride generated in the process was passed into the reaction In container A, the gas export rate is controlled at 2L / Min. During this process, pay attention to the temperature change at all times, and control the temperature below 30°C. After the gas is introduced, continue to stir for 4 hours. After filtration, 400.23 g of the product was obtained by evaporation and crystallization, and 369.28 g of the product was obtained after rapid drying. Finally, 550 g of DMC was added to the obtained product, and the product quality obtained after dissolving an...

Embodiment 2

[0026] At room temperature, add 101.9g of lithium oxalate and 1300g of HF into a jacketed reaction vessel 1, and stir overnight to completely dissolve lithium oxalate in HF. In the reaction kettle 2, 200g of anhydrous HF was introduced in advance, and then 416.46g of phosphorus pentachloride was slowly added, and a low-temperature cooling medium was introduced into the jacket to control the temperature, and then the phosphorus pentafluoride produced in the process was introduced into the reaction In container 1, the gas export rate was controlled to be 2L / Min. During this process, attention was paid to temperature changes at all times, and the temperature was controlled below 30°C. After the gas was introduced, the stirring was continued for 4 hours. After filtration, 401.23 g of the product was obtained by evaporation and crystallization, and 368.72 g of the product was obtained after rapid drying. Finally, 500 g of ether was added to the obtained product, and after dissolvin...

Embodiment 3

[0029] At room temperature, add 101.9g of lithium oxalate and 1300g of HF into a jacketed reaction vessel 1, and stir overnight to completely dissolve lithium oxalate in HF. In the reaction kettle 2, 200g of anhydrous HF was introduced in advance, and then 416.46g of phosphorus pentachloride was slowly added, and a low-temperature cooling medium was introduced into the jacket to control the temperature, and then the phosphorus pentafluoride produced in the process was introduced into the reaction In container 1, the gas export rate was controlled to be 2L / Min. During this process, attention was paid to temperature changes at all times, and the temperature was controlled below 30°C. After the gas was introduced, the stirring was continued for 4 hours. After filtration, 401.23g of the product was obtained by evaporation and crystallization, and 368.85g of the product was obtained after rapid drying. Finally, 700g of ethanol was added to the obtained product, and the product qual...

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Abstract

The invention provides a lithium tetrafluoro oxalate-phosphate preparation method which is simple and practical and can be applied to large-scale industrial production. The lithium tetrafluoro oxalate-phosphate preparation method provided by the invention is characterized by comprising the specific steps: firstly, weighing lithium oxalate, putting weighed lithium oxalate into a 316L stainless-steel reactor A with a jacket and a filtrating device, and thoroughly stirring weighed lithium oxalate for 2-6 hours, so as to fully dissolve weighed lithium oxalate into anhydrous HF; and then, adding phosphorus pentachloride and hydrogen fluoride into another 316L stainless-steel reactor B with a jacket and a filtrating device, and carrying out reaction. The lithium tetrafluoro oxalate-phosphate preparation method has the advantages that lithium tetrafluoro oxalate-phosphate is prepared from low-cost raw materials, the preparation method is simple, the disadvantages of other methods that the number of reaction steps is large, the consumption of reaction is high and impurities in the final product are too many are overcome, and thus the cost can be greatly reduced.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a method for preparing lithium tetrafluorooxalate phosphate which can be used as an additive for nonaqueous electrolytes of lithium ion batteries. Background technique [0002] Lithium tetrafluorooxalate phosphate is mainly used as an additive for nonaqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors. After adding this additive, the electrolyte has excellent high temperature resistance, and a more stable solid electrolyte interfacial film structure can be formed on the surface of the positive electrode material, improving the cycle performance of the battery. The currently known preparation methods of this additive mainly include the following types. [0003] Patent No. US20100267984 proposes to mix lithium hexafluorophosphate and lithium oxalate in a pressure vessel, then heat to 150°C-180°C, dissolve the resulting product in acetonitrile...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C55/07
CPCC07C51/412C07C55/07
Inventor 赵庆云王坤孙新华桑俊利刘大凡袁莉张丽红
Owner TIANJIN JINNIU POWER SOURCES MATERIAL
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