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Method for producing difluorophosphate, nonaqueous electrolyte solution, and nonaqueous electrolyte secondary battery

A technology of difluorophosphate and non-aqueous electrolyte, applied in non-aqueous electrolyte storage battery, non-aqueous electrolyte, secondary battery, etc., can solve the complicated operation of electrolyte composition adjustment, unfavorable industrial production, and inability to obtain difluorophosphoric acid Lithium and other problems, to achieve the effect of improving cycle characteristics and low-temperature discharge characteristics, and excellent performance

Active Publication Date: 2011-04-27
STELLA CHEMIFA CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, lithium difluorophosphate can only be obtained as a mixture with lithium hexafluorophosphate, and lithium difluorophosphate alone cannot be obtained.
In addition, lithium difluorophosphate can only be obtained in the state of being dissolved in a solution, and the operation of adjusting the composition of the electrolyte is complicated, which is disadvantageous in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0206] The production method of the specific carbonate is not particularly limited, and a known method can be selected arbitrarily.

[0207] In the nonaqueous electrolytic solution, one specific carbonate may be contained alone, or two or more specific carbonates may be contained in any combination and ratio.

[0208] The compounding amount of the specific carbonate is not limited, as long as the effect of the present invention is not significantly impaired, it is arbitrary. With respect to the non-aqueous electrolyte solution, the compounding amount of the specific carbonate is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, especially Preferably it is 0.3 mass % or more. In addition, it is preferably 70% by mass or less, more preferably 50% by mass or less, particularly preferably 40% by mass or less.

[0209] When the compounding quantity of a specific carbonate is more than the said minimum, the non-aqueous electrolyte secondary battery can exhibit s...

Embodiment 1-1

[0560] 2.9 g of phosphorus pentoxide was weighed into a 250 ml PFA container, and 3.4 g of lithium hexafluorophosphate (reagent: manufactured by Stella Chemifa Corporation) was added. Then, 8.9 g of a 15% (mass % concentration, the same below) dimethyl hydrogen carbonate solution was added, and the mixture was refluxed for 1 hour while blowing nitrogen gas under the condition of 110°C. The insoluble components in the reaction solution were removed by filtration, and then heated at 130° C. for 17 hours, and excess solvent and reaction by-products were distilled off. Then, it was cooled to room temperature to obtain lithium difluorophosphate crystals. The obtained lithium difluorophosphate crystals were subjected to anion analysis by ion chromatography (DX-500 manufactured by Dionex Corporation, column AS-23), and the relative area ratio of difluorophosphate ions was regarded as the purity of lithium difluorophosphate. . The purity (in terms of relative area) of the obtained l...

Embodiment 1-2

[0562] Measure 7.0 g of lithium hexafluorophosphate (reagent: manufactured by Stella Chemifa Corporation) into a 250 ml PFA container, and add 3.4 g of lithium carbonate (reagent: manufactured by Wako Pure Chemical Industries) and 6.5 g of phosphorus pentoxide (reagent: manufactured by Wako Pure Chemical Industries) . Then, 35 g of a 10% hydrogen fluoride dimethyl carbonate solution was added, and the mixture was refluxed for 1 hour while bubbling nitrogen gas under the condition of 110°C. The insoluble components in the reaction solution were removed by filtration, and then heated at 130° C. for 17 hours, and excess solvent and reaction by-products were distilled off. Then, it was cooled to room temperature to obtain lithium difluorophosphate crystals. Anion analysis was carried out in the same manner as in Example 1-1, and the purity (in terms of relative area) of the obtained lithium difluorophosphate crystal was 95%.

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Abstract

A method for producing a high-purity difluorophosphate by simple processes; a method for producing an electrolyte solution using a difluorophosphate obtained by the method; an electrolyte solution; and a secondary battery. Specifically disclosed is a method for producing a difluorophosphate, which comprises the following step (1) or (2). (1) A step wherein (A) at least one substance selected froma group consisting of phosphorus oxo acids, oxo acid anhydrides and oxyhalides is reacted with (B) a hexafluorophosphate in the presence of hydrogen fluoride. (2) A step wherein at least one halide selected from a group consisting of alkali metal halides, alkaline earth metal halides, aluminum halides and onium halides is reacted with difluorophosphoric acid in the presence of a hexafluorophosphate. Also disclosed are a nonaqueous electrolyte solution containing the thus-obtained difluorophosphate, and a nonaqueous electrolyte secondary battery comprising the nonaqueous electrolyte solution.

Description

technical field [0001] The present invention relates to a method for producing difluorophosphate, a nonaqueous electrolytic solution containing the difluorophosphate produced by the production method, and a nonaqueous electrolyte secondary battery having the nonaqueous electrolytic solution. Background technique [0002] In recent years, the application field of lithium secondary batteries has expanded from electronic equipment such as mobile phones, personal computers, and digital cameras to automotive equipment. Along with this, for lithium secondary batteries, further efforts have been made to improve output density and energy density and suppress capacity loss. High performance continues to evolve. In particular, automotive applications are likely to be exposed to harsher environments than consumer applications, and thus require high reliability in terms of cycle life and storage performance. [0003] Conventionally, a non-aqueous electrolyte obtained by dissolving a li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M10/052H01M10/0567
CPCH01M10/0567Y02E60/122H01M10/0569H01M10/052H01M2300/0025C01B25/455H01M2300/0091Y02E60/10Y02P70/50
Inventor 西田哲郎富崎惠正神和彦中岛秀纪铃木裕文藤井隆
Owner STELLA CHEMIFA CORP
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