Method for producing imide salt

A technology of imide salt and thionyl chloride, applied in chemical instruments and methods, iminodisulfonic acid/nitrilotrisulfonic acid, nitrosyl chloride, etc., can solve problems such as time-consuming

Inactive Publication Date: 2014-06-25
SUMITOMO ELECTRIC IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This is because conventional manufacturing methods require many steps to obtain the desired product from raw materials and are time-consuming due to lengthy fluorination reactions.

Method used

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  • Method for producing imide salt

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (first step)

[0037] Sulfamic acid, chlorosulfonic acid, and thionyl chloride were mixed at a molar ratio of 1.0:1.0:2.4 in an inert atmosphere, and heated under reflux. The temperature was 130°C.

[0038] The reaction of sulfamic acid with chlorosulfonic acid and thionyl chloride gives HN(SO 2 Cl) 2 . The reaction also produces by-products including sulfur dioxide, sulfuric acid and hydrochloric acid. Sulfur dioxide is produced from the reaction of thionyl chloride with sulfamic acid. Therefore, the production of sulfur dioxide indicates the continuation of the reaction. Therefore, the above heating is continued until the formation of sulfur dioxide ceases.

[0039] After the reaction was completed, a calcium chloride tube was carefully attached to the vapor outlet of the reaction system so that moisture was not introduced into the reaction system, and the entire reaction system was cooled. Thus, preventing HN(SO 2 Cl) 2 of hydrolysis.

[0040] (second step)...

Embodiment 2

[0052] describes the manufacture of KN(SO 2 F) 2 Methods.

[0053] In Example 2, fluorosulfonic acid was used instead of chlorosulfonic acid in Example 1.

[0054] In the first step, sulfamic acid, fluorosulfonic acid and thionyl chloride are reacted to give HN(SO 2 Cl)(SO 2 F). That is, the substance generated during the second step process of Example 1 was obtained in this step. This can be attributed to the sulfonation reaction with fluorosulfonic acid of the intermediate obtained by substituting chlorine for the OH group in sulfamic acid.

[0055] In the second step, potassium fluoride (KF) is added to the first intermediate product obtained in the first step from which excess thionyl chloride has been removed to allow a reaction to proceed. Thereby, almost the entire amount of by-products, namely sulfuric acid and hydrochloric acid, are converted into salts.

[0056] In the third step, water is added to the second intermediate product of the second step. Thus KN(S...

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Abstract

A first intermediate product is produced by thermally reacting a mixture of sulfamic acid, a halogenated sulfonic acid, and thionyl chloride. Next, a second intermediate product is produced by reacting the first intermediate product and an alkali metal fluoride (MF). Then, MN(SO2F)2 (M is an alkali metal), which is the target product, is obtained by reacting the second intermediate product and the alkali metal fluoride (MF) in a polar solvent.

Description

technical field [0001] The present invention relates to a process for the manufacture of imide salts. Background technique [0002] In recent years, imide salts such as LiN(SO 2 F) 2 Attention has been drawn as a supporting salt to be added to electrolyte solutions for lithium ion secondary batteries. KN(SO 2 F) 2 or NaN(SO 2 F) 2 Or their mixtures have also attracted attention as electrolytes for molten salt batteries. [0003] The manufacture of KN(SO 2 F) 2 and KN(SO 2 F) 2 Methods. In Non-Patent Document 1, HN(SO 2 Cl) 2 , which is then reacted with KF in nitromethane or dichloromethane solvents to give KN(SO 2 F) 2 . [0004] At the same time, there is a demand for a method for producing imide salts, which typically include LiN(SO 2 F) 2 , KN(SO 2 F) 2 , NaN(SO 2 F) 2 Wait. This is because conventional manufacturing methods require many steps to obtain desired products from raw materials and are time-consuming due to lengthy fluorination reactions...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086C01D13/00
CPCC01B21/0935C01B21/086C01D13/00
Inventor 福永笃史稻泽信二新田耕司酒井将一郎
Owner SUMITOMO ELECTRIC IND LTD
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