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Process for producing bis(fluorosulfonyl)imide anion compound, and ion-pair compound

A technology of iminium anion and fluorosulfonyl group, which is applied in chemical instruments and methods, nitrogen and non-metallic compounds, chemical/physical processes, etc., can solve the problems of low yield and insufficient purity of products, etc. achieve low cost

Inactive Publication Date: 2011-05-04
DAI ICHI KOGYO SEIYAKU CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Furthermore, a reaction in which chlorosulfonic acid is used instead of fluorosulfonic acid, which is difficult to use industrially, is also disclosed, but the reaction takes more than 24 hours, and in the fluorination reaction, the reaction bath needs to be at 120° C. or even 170° C. to 180° C., and The purity of the product is not sufficient due to side reactions, and many steps are involved in the purification, so the yield is estimated to be low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 30g (0.31 moles) of sulfamic acid (purity of 99.5% or more produced by Wako Pure Chemical Industries) was dried in a heating dryer at 50° C. for 1 hour, and the moisture after drying was 1500 ppm. Heat and dry the 300ml flask with reflux condenser, thermometer, stirring device, heating device and dry gas inlet pipe, after cooling to room temperature, put into dried 30g (0.31 mole) sulfamic acid and 38g (0.33 mole) chlorosulfonic acid (the purity of Wako Pure Chemicals is more than 97%), slowly drop 106g (0.77 moles) of phosphorus trichloride (the purity of Wako Pure Chemicals is more than 99%), and introduce dry nitrogen at 0.02 liters / minute (the dew point is -60°C) Below) 60 minutes. Next, the container was heated up to 110° C. over 4 hours, and the reaction temperature was maintained for 10 hours, and then cooled to room temperature to obtain 90 g of a reactant A-1 containing bis(chlorosulfonyl)imidic acid.

[0056] Next, 90 g (1.55 moles) of potassium fluoride (spr...

Embodiment 2

[0058] 30 g (0.31 mol) of sulfamic acid (purity of 99.5% or more manufactured by Wako Pure Chemical Industries, Ltd.) was dried at room temperature under a reduced pressure of 1.6 kPa for 8 hours, and the moisture after drying was 600 ppm. Heat and dry the 300ml flask with reflux condenser, thermometer, stirring device, heating device and dry gas inlet pipe, after cooling to room temperature, put into dried 30g (0.31 mole) sulfamic acid, 38g (0.33 mole) chlorosulfonic acid (the purity prepared by Wako Pure Chemicals is more than 97%), slowly add 130g (0.61 moles) of phosphorus pentachloride (the purity prepared by Wako Pure Chemicals is more than 99%), and introduce dry nitrogen at 0.02 liters / minute (the dew point is -60°C) Below) 60 minutes. Next, the container was heated up to 110° C. over 4 hours, and the reaction temperature was maintained for 16 hours, and then cooled to room temperature to obtain 115 g of a reactant A-2 containing bis(chlorosulfonyl)imidic acid.

[005...

Embodiment 3

[0061] 30g (0.31 moles) of sulfamic acid (purity of 99.5% or more produced by Wako Pure Chemical Industries) was dried in a heating dryer at 50° C. for 1 hour, and the moisture after drying was 1500 ppm. Heat and dry the 300ml flask with reflux condenser, thermometer, stirring device, heating device and dry gas inlet pipe, after cooling to room temperature, put into dried 30g (0.31 mole) sulfamic acid and 35g (0.30 mole) chlorosulfonic acid (the purity of Wako Pure Chemicals is more than 97%), add 146g (1.08 moles) of thionyl chloride (the purity of Wako Pure Chemicals is more than 95%), and introduce dry nitrogen (dew point below -60°C) at 0.02 liters per minute for 60 minute. Next, the container was heated up to 130° C. over 8 hours, and the reaction temperature was maintained for 4 hours, then cooled to room temperature to obtain 65 g of a reactant A-3 containing bis(chlorosulfonyl)imidic acid.

[0062] Next, 65 g (1.12 moles) of potassium fluoride (a spray-dried product m...

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PUM

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Abstract

A process for producing a bis(fluorosulfonyl)imide anion compound by substituting a bis(chlorosulfonyl)imide anion compound, obtained from sulfamic acid, chlorosulfonic acid, and a halogenating agent, with fluorine is used as a process for producing a fluorine compound for use, for example, in the synthesis of battery electrolytes and ionic liquids. According to the above process, the inclusion of impurities can be reduced, and a high-purity fluorine compound of a bis(fluorosulfonyl)imide compound can be efficiently produced at a high yield. A base catalyst can be used in the reaction for substituting the bis(chlorosulfonyl)imide anion with fluorine. The base catalyst is preferably a nitrogen-containing compound.

Description

technical field [0001] The present invention relates to a method for producing a bis(fluorosulfonyl)imide anion compound used in the synthesis of battery electrolytes or ionic liquids, and an ion pair compound containing the bis(fluorosulfonyl)imide anion compound obtained by the production method . Background technique [0002] Anionic compounds containing fluorine elements are useful and there are many reports, but their synthesis methods almost all require the use of special equipment such as electrolysis of fluorine. The methods for producing bis(fluorosulfonyl)imide anions, which are fluorine-containing element anions, are mostly methods using very expensive raw materials such as fluorosulfonic acid or fluoroisocyanate, or methods using reactions with low yields. situation. Alternatively, a gas that is not easy to handle is used, which is not preferable in terms of cost as production by a general industrial technique. [0003] For example, JP-A-8-511274 discloses the...

Claims

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Application Information

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IPC IPC(8): C01B21/086B01J27/24H01M10/36
CPCC01B21/086H01M10/052H01M10/0568Y02E60/10
Inventor 菊田学北尾真大
Owner DAI ICHI KOGYO SEIYAKU CO LTD
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