PURIFICATION OF BIS (FLUOROSULFONYL) IMIDE SALT

    公开(公告)号:US20230373788A1

    公开(公告)日:2023-11-23

    申请号:US18044742

    申请日:2021-09-10

    申请人: Solvay SA

    IPC分类号: C01B21/086

    CPC分类号: C01B21/086

    摘要: The present invention relates to a method for purifying a salt of bis (fluorosulfonyl) imide which is economically feasible at industrial scale and provides a high-purity product. Said method comprises the steps of providing a crude salt of bis (fluorosulfonyl) imide, dissolving the crude salt of bis (fluorosulfonyl) imide in at least one first solvent, crystallizing the salt of bis (fluorsulfonyl) imide by means of at least one second solvent and separating the crystallized salt of bis (fluorsulfonyl) imide, which can optionally be further reacted with an alkali salt, to obtain an alkali salt of bis (fluorosulfonyl) imide.

    Method for producing disulfonylamine alkali metal salt

    公开(公告)号:US09950929B2

    公开(公告)日:2018-04-24

    申请号:US14773964

    申请日:2014-03-05

    摘要: The present invention provides a method for producing a disulfonylamine alkali metal salt, including a step of subjecting a disulfonylamine onium salt represented by formula [I] (wherein each of R1 and R2 independently represents a fluorine atom or a fluorinated alkyl group having 1 to 6 carbon atoms, provided that at least one of R1 and R2 represents a fluorine atom, and each of R3, R4, R5 and R6 independently represents a hydrogen atom or the like) to a cation exchange reaction in an organic solvent, thereby producing a disulfonylamine alkali metal salt represented by formula [II] (wherein M+ represents an alkali metal cation, and R1 and R2 are as defined in formula [I]), and a step of filtering the organic solvent solution containing the disulfonylamine alkali metal salt through a filter having a particle retention size of 0.1 to 10 μm to obtain a filtrate.

    Method for producing imide salt
    5.
    发明授权
    Method for producing imide salt 有权
    生产酰亚胺盐的方法

    公开(公告)号:US09352966B2

    公开(公告)日:2016-05-31

    申请号:US14352175

    申请日:2012-09-25

    IPC分类号: C01B21/086 C01D13/00

    CPC分类号: C01B21/086 C01D13/00

    摘要: A mixture of sulphamic acid, a halogenated sulphonic acid and thionyl chloride is heated to allow the reaction to proceed, to thereby produce first intermediate products. The first intermediate products are then subjected to reaction with an alkali metal fluoride MF to produce second intermediate products. The second intermediate products is then subjected to reaction with the alkali metal fluoride MF in a polar solvent to obtain a desired product MN(SO2F)2 (where M is an alkali metal).

    摘要翻译: 将氨基磺酸,卤代磺酸和亚硫酰氯的混合物加热以使反应进行,从而产生第一中间产物。 然后将第一中间产物与碱金属氟化物MF反应以产生第二中间产物。 然后将第二中间产物在极性溶剂中与碱金属氟化物MF反应,得到所需产物MN(SO2F)2(其中M为碱金属)。

    METHOD FOR PREPARING IMIDE SALTS CONTAINING A FLUOROSULPHONYL GROUP
    6.
    发明申请
    METHOD FOR PREPARING IMIDE SALTS CONTAINING A FLUOROSULPHONYL GROUP 有权
    用于制备含有氟代膦酸基团的酰胺的方法

    公开(公告)号:US20150246812A1

    公开(公告)日:2015-09-03

    申请号:US14370696

    申请日:2013-11-19

    申请人: ARKEMA FRANCE

    IPC分类号: C01B21/086

    摘要: A fluorination process for obtaining fluorinated compounds including at least one fluorosulfonyl group. More particularly, a process for preparing a fluorinated compound of formula (II), including at least one step of reacting a compound of formula (I) with anhydrous hydrofluoric acid in at least one organic solvent, in which R1 is equal to R2 except in the specific case where R1=Cl, then R2=F, and when R1 is equal to R2, R1 and R2 represent an electron-withdrawing group which has a Hammett parameter op of greater than 0, such as F, CF3, CHF2, CH2F, C2HF4, C2H2F3, C2H3F2, C2F5, C3F7, C3H2F5, C3H4F3, C3HF6, C4F9, C4H2F7, C4H4F5, C5F11, C3F5OCF3, C2F4OCF3, C2H2F2OCF3, CF2OCF3, C6F13, C7F15, C8F17 or C9F19, and M represents a hydrogen atom, an alkali metal, an alkaline-earth metal or a quaternary ammonium cation.

    摘要翻译: 一种用于获得包含至少一个氟磺酰基的氟化化合物的氟化方法。 更具体地,涉及一种制备式(II)的含氟化合物的方法,包括至少一个步骤:使式(I)化合物与无水氢氟酸在至少一种有机溶剂中反应,其中R 1等于R 2, 其中R1 = Cl,然后R2 = F的具体情况,当R1等于R2时,R1和R2表示具有大于0的Hammett参数op的吸电子基团,例如F,CF 3,CHF 2,CH 2 F ,C2HF4,C2H2F3,C2H3F2,C2F5,C3F7,C3H2F5,C3H4F3,C3HF6,C4F9,C4H2F7,C4H4F5,C5F11,C3F5OCF3,C2F4OCF3,C2H2F2OCF3,CF2OCF3,C6F13,C7F15,C8F17或C9F19,M表示氢原子,碱 金属,碱土金属或季铵阳离子。

    ALKALI METAL SALT OF FLUOROSULFONYL IMIDE, AND PRODUCTION METHOD THEREFOR
    7.
    发明申请
    ALKALI METAL SALT OF FLUOROSULFONYL IMIDE, AND PRODUCTION METHOD THEREFOR 审中-公开
    氟烷基氟化物的碱金属盐及其生产方法

    公开(公告)号:US20150086466A1

    公开(公告)日:2015-03-26

    申请号:US14560315

    申请日:2014-12-04

    IPC分类号: C01D15/00

    摘要: 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° 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.

    摘要翻译: 本发明提供了具有良好的耐热性,降低的特定杂质含量和含水量的氟磺酰亚胺的碱金属盐,提供了能够容易地除去溶剂的氟磺酰亚胺的碱金属盐的方法 反应溶液。 本发明的氟代磺酰亚胺的碱金属盐由以下通式(I)表示,当氟磺酰亚胺的碱金属盐在100℃保持8小时时质量损失率为2%以下 在气流下。 制备本发明的氟磺酰亚胺碱金属盐的方法包括通过将气体鼓入含氟氟磺酰亚胺的碱金属盐的反应溶液中浓缩氟磺酰亚胺的碱金属盐的溶液和/或 通过薄层蒸馏浓缩氟磺酰亚胺的碱金属盐的溶液。

    PROCESS FOR THE PREPARATION OF LITHIUM OR SODIUM BIS(FLUOROSULPHONYL)IMIDE
    8.
    发明申请
    PROCESS FOR THE PREPARATION OF LITHIUM OR SODIUM BIS(FLUOROSULPHONYL)IMIDE 审中-公开
    制备锂或钠(氟化膦)的方法

    公开(公告)号:US20140369919A1

    公开(公告)日:2014-12-18

    申请号:US14476106

    申请日:2014-09-03

    申请人: ARKEMA FRANCE

    发明人: Grégory SCHMIDT

    摘要: A process for the preparation of a bis(sulphonato)imide salt of formula: (III) (SO3−)—N−—(SO3−) 3C+ where C+ represents a monovalent cation, comprising the reaction of amidosulphuric acid of formula: (I) (OH)—SO2—NH2 with a halosulphonic acid of formula: (II) (OH)—SO2—X where X represents a halogen atom, and comprising a reaction with a base which is a salt formed with the cation C. Also, a process for the preparation of bis(fluorosulphonyl)imide acid of formula: (V) F—(SO2)—NH—(SO2)—F and to a process for the preparation of lithium bis(fluorosulphonyl)imide salt of formula: (VII) F—(SO2)—N−−(SO2)—F Li+.

    摘要翻译: 一种制备式(III)(SO 3 - ) - N - (SO 3 - )3 C +的双(磺酸根)酰亚胺盐的方法,其中C +代表一价阳离子,包括下式的酰胺硫酸:(I )(OH)-SO 2 -NH 2与式(II)(OH)-SO 2 -X的卤代磺酸反应,其中X表示卤素原子,并且与与阳离子C形成的盐的碱反应。另外 ,(V)F-(SO 2)-NH-(SO 2)-F的双(氟磺酰基)酰亚胺酸的制备方法和制备下式的双(氟磺酰基)亚胺盐的方法: (Ⅶ)F-(SO2)-N - (SO2)-FLi +。

    Method for producing imidic acid salt
    9.
    发明授权
    Method for producing imidic acid salt 有权
    生产酰亚胺酸盐的方法

    公开(公告)号:US08840856B2

    公开(公告)日:2014-09-23

    申请号:US13322782

    申请日:2010-06-01

    摘要: To provide an imide salt represented by the formula wherein, R represents a halosulfonyl group (—SO2X1 where X1 is a halogen such as fluorine, chlorine, bromine and iodine) or dihalophosphoryl group (—POX2X3 where X2 and X3 are the same or different halogens such as fluorine, chlorine, bromine and iodine), and M represents an alkali metal; with high selectivity and high efficiency by using a low-cost starting material. In the production of an imide salt, an alkali metal fluoride, a sulfuryl halide or phosphoryl halide, and ammonia or an ammonium salt are reacted. According to this method, a desired imide salt can be produced with high yield, while greatly suppressing the production of a by-product.

    摘要翻译: 提供由下式表示的酰亚胺盐:其中,R表示卤代磺酰基(-SO2X1,其中X1是氟,氯,溴和碘等卤素)或二卤代磷酰基(-POX2X3,其中X2和X3是相同或不同的卤素 例如氟,氯,溴和碘),M表示碱金属; 通过使用低成本起始材料,具有高选择性和高效率。 在制备酰亚胺盐时,使碱金属氟化物,硫酰卤或磷酰卤,以及氨或铵盐反应。 根据该方法,可以高产率地制造所需的酰亚胺盐,同时大大抑制副产物的生成。

    FLUOROSULFONYL IMIDE SALT AND METHOD FOR PRODUCING FLUOROSULFONYL IMIDE SALT
    10.
    发明申请
    FLUOROSULFONYL IMIDE SALT AND METHOD FOR PRODUCING FLUOROSULFONYL IMIDE SALT 有权
    氟代膦酸盐及其生产氟磺酰氟盐的方法

    公开(公告)号:US20120041233A1

    公开(公告)日:2012-02-16

    申请号:US13264244

    申请日:2010-11-26

    IPC分类号: C07C235/70

    摘要: 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.

    摘要翻译: 本发明提供一种能够使杂质含量长时间持续运转的氟磺酰亚胺盐的制造方法和氟磺酰亚胺盐。 本发明的氟磺酰亚胺盐的K含量为10,000ppm以下。 本发明的氟磺酰亚胺盐的制造方法是在氯磺酰基imde或其盐的氟化反应后,使反应溶液与碱性水溶液接触以除去杂质。 本发明的氟磺酰亚胺盐,其各种有害作用降低至极低水平,可用作锂二次电池,电容器等中使用的电解质,离子液体或磺酰亚胺盐的中间体 ,等等。 预期使用本发明的氟磺酰亚胺盐作为电解液导致高性能的电化学装置。