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Manufacturing method of lithium difluorophosphate

A technology of lithium difluorophosphate and a manufacturing method, which is applied to chemical instruments and methods, secondary batteries, phosphorus compounds, etc., can solve problems such as electrolyte deterioration, and achieve the effects of reducing the mixing of impurities and improving performance

Active Publication Date: 2021-02-23
CENT GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to increase the reaction rate, a method of increasing the reaction temperature is also considered, but when it exceeds 60°C, the decomposition of lithium hexafluorophosphate begins to occur, leading to the deterioration of the electrolyte, so there is also a problem.

Method used

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  • Manufacturing method of lithium difluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Dissolve 152g (1mol) of LiPF in 530g of ethyl methyl carbonate 6 And 258.1g (2mol) of dimethyl dichlorosilane, cooled to 0°C. Next, after adding 36 g (2 mol) of water over 2 hours, it heated up to 25 degreeC and stirred for 1 hour. As a result of analyzing the thus obtained reaction solution by 19F-NMR and 31P-NMR, the reaction solution contained 108 g (1 mol) of lithium difluorophosphate, and it was confirmed that the reaction proceeded substantially quantitatively.

[0075] Next, a pre-degassing step was performed to remove hydrogen chloride and dimethyldifluorosilane generated in the reaction liquid under reduced pressure conditions of 30° C. and an absolute pressure of 30 kPa. The amount of chlorine contained in the degassed solution was analyzed by turbidimetry, and it was 3100 ppm relative to the amount of the reaction solution. Hydrogen chloride can be almost completely removed by the degassing treatment, therefore, the basic total amount of chlorine contained ...

Embodiment 2、3

[0080] The same procedure as in Example 1 was performed except that 3 equivalents or 5 equivalents of hydrogen fluoride was added to the solution after the pre-degassing step relative to the chlorine atoms in the solution.

Embodiment 4

[0082] Dissolve 152g (1mol) of LiPF in 530g of ethyl methyl carbonate 6 and 245.2g (1.9mol) of dimethyldichlorosilane, cooled to 0°C. Next, after adding 34 g (1.9 mol) of water over 2 hours, it heated up to 25 degreeC and stirred for 1 hour. Analysis of the reaction solution thus obtained by 19F-NMR and 31P-NMR revealed that the reaction solution contained LiPF 6 7.6 g (0.05 mol) and 102.5 g (0.95 mol) of lithium difluorophosphate were confirmed to react substantially quantitatively.

[0083] Next, a pre-degassing step was performed to remove hydrogen chloride and dimethyldifluorosilane generated in the reaction liquid under reduced pressure conditions of 30° C. and an absolute pressure of 30 kPa. The amount of chlorine contained in the degassed solution was analyzed by turbidimetry and found to be 2700 ppm relative to the amount of the reaction solution. Hydrogen chloride can be almost completely removed by the degassing treatment, therefore, the basic total amount of chl...

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Abstract

The present invention relates to a method for producing lithium difluorophosphate. It is an object of the present invention to provide a method for industrially producing lithium difluorophosphate, which is an additive effective for improving the performance of nonaqueous electrolyte batteries, while reducing contamination of impurities. The production method using lithium difluorophosphate is characterized in that the production method includes: a reaction step of making LiPF 6 Reacting with water and the halide represented by the following general formula (1) in a non-aqueous solvent; Adding process, adding hydrogen fluoride to the solution after the reaction process; and, Degassing process, performing degassing treatment on the solution after the adding process. R p SiX q (1) (In the general formula (1), R is independently a hydrocarbon group with 1 to 10 carbon atoms optionally having a heteroatom or a halogen atom (when the carbon number is 3 or more, a branched or cyclic structure can also be used) hydrocarbon group). X is each independently any one selected from the group consisting of Cl, Br and I. p represents an integer of 1 to 3, q ​​represents an integer of 1 to 3, p+q=4).

Description

technical field [0001] The present invention relates to a method for producing an industrially and economically excellent lithium difluorophosphate used in a nonaqueous electrolyte battery, and a method for producing an electrolyte solution for a nonaqueous electrolyte battery containing the lithium difluorophosphate produced by the method. Background technique [0002] In recent years, power storage systems for small, high-energy-density applications such as information-related equipment and communication equipment, that is, computers, video cameras, digital cameras, and mobile phones; auxiliary power supplies for electric vehicles, hybrid vehicles, and fuel cell vehicles, power storage systems Large-scale power storage systems such as these have attracted attention. As one of the candidates, non-aqueous electrolyte batteries such as lithium ion batteries, lithium batteries, and lithium ion capacitors have been actively developed. [0003] Many of these non-aqueous electro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/455H01M10/0567
CPCC01B25/455H01M10/0567Y02E60/10H01M10/0566
Inventor 森高神代将克西村夏哉
Owner CENT GLASS CO LTD