Nippon Shokubai Co., Ltd.

Ntt Advanced Technology Corporation

Morita Chemical Industries Co., Ltd.

Yasunori Okumura

Shimpei Sato

Yuichi Sato

Hiromoto Katsuyama

Masayoshi Kuwabara

Osamu Kaieda

Takayuki Kobatake

Naohiko Itayama

Hiroyuki Mizuno

Masayuki Okajima

Go Masuda

Yukihiro Fukata

Shinji Nishimae

Kiyoshi Masuda

Kozo Tajiri

Shoji Ito

Minoru Aoki

Kazuo Takei

Tohru Matsuura

Yasuyuki Miyoshi

Noriyoshi Yamada

Yuhiko Yamashita

Kunio Kimura

Hirotsugu Shimizu

Yasuhiro Higuchi

Takahiro Yamauchi

Kenji Yamada

An electrolytic solution comprising N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl)imide or di(fluorosulfonyl)imide, from which a residual solvent that affects the properties of the electrolyte solution material is reduced, is provided. A method for producing an electrolyte solution material containing fluorosulfonyl imide salt represented by the following general formula (1) and an electrolyte solution preparation solvent comprises decompressing and/or heating a solution containing the fluorosulfonyl imide salt and the electrolyte solution preparation solvent to volatilize a production solvent for the fluorosulfonyl imide salt. In general formula (1), Rrepresents a fluorine atom or a fluorinated alkyl group having 1 to 6 carbon atoms, Rrepresents an alkali metal ion.

Method for manufacturing electrolyte solution material

An electrolytic solution comprising N-(fluorosulfonyl)-N-(fluoroalkylsulfonyl)imide or di(fluorosulfonyl)imide, from which a residual solvent that affects the properties of the electrolyte solution material is reduced, is provided. A method for producing an electrolyte solution material containing fluorosulfonyl imide salt represented by the following general formula (1) and an electrolyte solution preparation solvent comprises decompressing and/or heating a solution containing the fluorosulfonyl imide salt and the electrolyte solution preparation solvent to volatilize a production solvent for the fluorosulfonyl imide salt.  In general formula (1), Rrepresents a fluorine atom or a fluorinated alkyl group having 1 to 6 carbon atoms, Rrepresents an alkali metal ion.

In the present invention, a bis (fluorosulfonyl) imide metal salt is an alkali metal salt of bis (fluorosulfonyl) imide or an alkaline earth metal salt of bis (fluorosulfonyl) imide. The bis (fluorosulfonyl) imide metal salt has an average particle diameter of not less than 0.1 mm, or has an average moisture absorption rate of not more than 2.5 mass ppm/cm&#xb7;min when sealed in a PE bag having a thickness of 80 &#x3bc;m and left for 30 minutes at 23&#xb0; C. and 65% humidity.

Bis(fluorosulfonyl) imide metal salt and method for preparing same

Provided is a method the enables easy production of bis(fluorosulfonyl)imide suitable for a non-aqueous electrolytic solution for a lithium ion secondary battery, etc. The method for producing a bis(fluorosulfonyl)imide alkali metal salt according to the present invention comprises reacting bis(fluorosulfonyl)imide with an alkali metal compound in a reaction solution containing an organic solvent, wherein the organic solvent includes at least one organic solvent (A) selected from the group consisting of carbonate solvents, cyclic ether solvents, linear ether solvents having two or more oxygen atoms in the molecule, cyclic ester solvents, sulfolane solvents, N,N-dimethyl formamide, dimethyl sulfoxide, and N-methyl oxazolidinone.

Method for producing bis(fluorosulfonyl)imide alkali metal salt and method for producing non aqueous electrolytic solution

The present invention provides an alkali metal salt of fluorosulfonyl imide having favorable heat resistance and a reduced content of specific impurities and a water content, and provides a method for producing an alkali metal salt of fluorosulfonyl imide, which is capable of easily removing a solvent from a reaction solution. An alkali metal salt of fluorosulfonyl imide of the present invention is represented by the following general formula (I) and has a mass loss rate of 2% or less when the alkali metal salt of fuluorosulufonyl imide is kept at 100&#xb0; C. for 8 hours under an air current. A method for producing an alkali metal salt of fluorosulfonyl imide of the present invention comprises a step of concentrating a solution of the alkali metal salt of fulorosulfonyl imide by bubbling a gas into a reaction solution containing the alkali metal salt of fulorosulfonyl imide, and/or concentrating a solution of the alkali metal salt of fulorosulfonyl imide by thin layer distillation. 

Alkali metal salt of fluorosulfonyl imide, and production method therefor

The present invention provides a method for producing a fluorisulfonylimide salt, which enables reducing the impurity content and continuous operation for a long time, and a fluorosulfonyl imide salt. The fluorosulfonyl imide salt of the present invention has a K content of 10,000 ppm or less. The method for producing a fluorosulfonyl imide salt of the present invention is that after a fluorination reaction of chlorosulfonyl imde or a salt thereof, the reaction solution is brought into contact with an aqueous alkaline solution so as to remove impurities. The fluorosulfonyl imide salt of the present invention, in which various impirities are reduced to extremely low levels, is useful as an electrolyte used in a lithium secondary battery, a capacitor or the like, an ionic liquid, or an intermediate for a sulfonyl imide salt, and the like. It is expected that use of the fluorosulfonyl imide salt of the present invention as an electrolyte leads to a high-performance electrochemical device.

Fluorosulfonyl imide salt and method for producing fluorosulfonyl imide salt

The present invention provides an alkali metal salt of fluorosulfonyl imide having favorable heat resistance and a reduced content of specific impurities and a water content, and provides a method for producing an alkali metal salt of fluorosulfonyl imide, which is capable of easily removing a solvent from a reaction solution. An alkali metal salt of fluorosulfonyl imide of the present invention is represented by the following general formula (I) and has a mass loss rate of 2% or less when the alkali metal salt of fluorosulfonyl imide is kept at 100&#xb0; C. for 8 hours under an air current. A method for producing an alkali metal salt of fluorosulfonyl imide of the present invention comprises a step of concentrating a solution of the alkali metal salt of fluorosulfonyl imide by bubbling a gas into a reaction solution containing the alkali metal salt of fluorosulfonyl imide, and/or concentrating a solution of the alkali metal salt of fluorosulfonyl imide by thin layer distillation. 

The present invention provides a method for producing fluorosulfonylimides more safely, rapidly and efficiently, which enables suppression of production of by-products, and fluorosulfonylimides. The method for producing a fluorosulfonylimide salt of the present invention includes a step of reacting a fluoride compound containing at least one element selected from the group consisting of elements of Group 11 to Group 15 and Period 4 to Period 6 (excluding arsenic and antimony) with a compound represented by the following general formula (I) to give a fluorosulfonylimide salt represented by the general formula (II): [Chemical Formula 1] wherein Rdenotes at least one element selected from the group consisting of elements of Group 11 to Group 15 and Period 4 to Period 6 (excluding arsenic and antimony); Rdenotes fluorine, chlorine or a fluorinated alkyl group having 1 to 6 carbon atoms; Rdenotes fluorine or a fluorinated alkyl group having 1 to 6 carbon atoms; and m denotes an integer of 2 or 3.

Sulfonylimide salt and method for producing the same

A method for the production of a fluorinated phenylenediamine is provided which comprises steps of reacting a diamide represented by the following formula with NaOCl at a molar ratio of the NaOCl to the diamide in the range of 2.0-6.0 and NaOH at a molar ratio of the NaOH to the diamide in the range of 1.8-6.0 is provided. According to this invention, the fluorinated phenylenediamine can be produced conveniently in a high yield. 

Method for production of fluorinated phenylenediamine

It is an object of the present invention to provide fluorinated bis(phthalic anhydride) which has less coloration and higher solubility in comparison with conventional compounds, and a method for producing the same. Further, it is also an object of the present invention to provide a method for producing a fluorinated bis(phthalonitrile) compound, which is an intermediate raw material compound of the method for producing the fluorinated bis(phthalic anhydride), and a polyamic acid and a polyimide, which are produced from the fluorinated bis(phthalic anhydride). A fluorinated bis(phthalic anhydride) of the present invention is the fluorinated bis(phthalic anhydride) represented by the following formula (I), wherein its specific surface area is 3.0 m/g or larger. It is also characterized in that its molar absorption coefficient is 0.6 L/mol&#xb7;cm or less at a wavelength of 360 nm. [wherein, m and n independently represent integers of 1 to 3, and Zrepresents a single bond group or a bivalent organic group.]

Fluorinated bis (phthalic anhydride) and method for producing the same

The present invention relates to halogen-containing aromatic compounds and methods thereof. The present invention relates a halogen-containing aromatic acid dianhydride, halogen-containing aromatic tetranitrile compound, halogen-containing m-phenylenediamine compound and fluorine compound, and a method thereof.

Halogen-containing aromatic compound

A polyimide excelling in heat resistance, chemical resistance, water repellency, dielectric characteristics, electrical characteristics, and optical characteristics and a polyamide acid useful as the raw material therefor are provided. Specifically, a polyamide acid containing a chlorine atom and a fluorine atom and comprising a repeating unit represented by the following formula (1):(wherein X and X' independently denote a divalent organic group; Y and Y&#x2032; independently denote a chlorine, bromine, or iodine atom; p and p&#x2032; denote independently denote the number of fluorine atom {F in the formula (1)} bonded to the relevant benzene ring, representing an integer of 0-3; q and q&#x2032; independently denote an integer of 0-3; and p+q total 3, and p&#x2032;+q&#x2032; total 3).

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Suita, Japan

Yasunori Okumura