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Method for producing difluorophosphate

A technology of difluorophosphate and manufacturing method, which is applied in the direction of final product manufacturing, chemical instruments and methods, sustainable manufacturing/processing, etc., can solve the problems of product purity, not high efficiency, etc., and achieve the effect of high utilization value

Active Publication Date: 2014-10-22
STELLA CHEMIFA CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction temperature of this method is about 170° C., which is stable compared with the reaction conditions of Patent Document 1, and it is also easy to implement industrially. However, due to the waste treatment of a large amount of by-produced ammonia gas and a large amount of residual ammonium fluoride, Not efficient, also has problems with the purity of the product obtained

Method used

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Examples

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Embodiment

[0063] Hereinafter, suitable examples of this invention will be described in detail as examples. However, the materials, compounding amounts, and the like described in the examples are not intended to limit the scope of the invention to these, unless there is a particularly restrictive description, and are merely illustrative examples.

reference example 1

[0064] Reference Example 1: Distillation and purification of difluorophosphoric acid

[0065] In order to increase the purity of difluorophosphoric acid used as a crystallization solvent, purification by distillation was performed. 400 g of difluorophosphoric acid (reagent: manufactured by Fluorochem) was weighed in a PTFE round bottom flask, and distilled under reduced pressure at 40°C to obtain a fraction of 313 g in a PTFE round bottom flask cooled to -20°C. This fraction was analyzed for anions by ion chromatography (DX-500 manufactured by DIONEX, column AS-23), and the relative area ratio of difluorophosphate ions was defined as the purity of difluorophosphoric acid. The purity of the obtained difluorophosphoric acid was 99% by relative area.

Embodiment 1

[0067] In a 500 ml PFA container, 300 g of difluorophosphoric acid obtained by the distillation operation in Reference Example 1 was weighed, and 25 g of lithium chloride (reagent: manufactured by Wako Pure Chemical Industries) was added. The reaction solution was filtered to remove insoluble components, and the obtained filtrate was cooled from 25°C to -30°C to precipitate crystals. The crystal obtained by solid-liquid separation of the slurry was dried at 40° C. under reduced pressure using a PTFE round-bottomed flask. The obtained lithium difluorophosphate crystals were analyzed for anions by ion chromatography (DX-500 manufactured by DIONEX, column AS-23), and the relative area ratio of difluorophosphate ions was defined as the purity of lithium difluorophosphate. The purity of the obtained lithium difluorophosphate crystal was 97% in terms of relative area.

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Abstract

Provided is a method for producing difluorophosphate which is characterized by obtaining the difluorophosphate by reacting at least one salt, as a raw material, selected from a halide salt, a carbonate, a phosphate, a hydroxide and an oxide of an alkali metal, an alkali earth metal or an onium with a difluorophosphoric acid in the difluorophosphoric acid, then separating a precipitate from the difluorophosphoric acid by solid liquid separation, the precipitate being precipitated by crystallization operation in the difluorophosphoric acid, and distilling the difluorophosphoric acid contained in the precipitate.

Description

technical field [0001] The present invention relates to a kind of production method of difluorophosphate. Background technique [0002] In recent years, salts having a melting point near normal temperature or salts (ionic liquids) having a melting point below normal temperature have been discovered. Ionic liquids are composed of cations and anions, and since their pulling forces are very weak, they appear liquid even at room temperature. If the structures of cations and anions are designed so that the pulling force becomes weak, the melting point of the salt can be changed to obtain an ionic liquid. Furthermore, it is said that the physical properties of ionic liquids can be intentionally controlled by changing the combination of cations and anions or by introducing substituents to the respective ions. [0003] Ionic liquids are characterized by being difficult to volatilize and existing stably at high temperatures of several hundred degrees Celsius or higher. It is also ...

Claims

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Application Information

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IPC IPC(8): C01B25/455
CPCC01B25/455H01M10/052H01M10/0568H01M2300/0045Y02E60/10H01M10/0566Y02P70/50
Inventor 西田哲郎正神和彦佐藤友哉
Owner STELLA CHEMIFA CORP
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