FR3059994B1 - Procede de sechage et de purification de lifsi - Google Patents

Procede de sechage et de purification de lifsi Download PDF

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Publication number
FR3059994B1
FR3059994B1 FR1662130A FR1662130A FR3059994B1 FR 3059994 B1 FR3059994 B1 FR 3059994B1 FR 1662130 A FR1662130 A FR 1662130A FR 1662130 A FR1662130 A FR 1662130A FR 3059994 B1 FR3059994 B1 FR 3059994B1
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FR
France
Prior art keywords
fluorosulfonyl
imide
bis
lithium salt
salt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
FR1662130A
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English (en)
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FR3059994A1 (fr
Inventor
Gregory Schmidt
Remy Teissier
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Arkema France SA
Original Assignee
Arkema France SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to FR1662130A priority Critical patent/FR3059994B1/fr
Application filed by Arkema France SA filed Critical Arkema France SA
Priority to CN201780068664.3A priority patent/CN109982966B/zh
Priority to PCT/FR2017/053447 priority patent/WO2018104675A1/fr
Priority to JP2019515208A priority patent/JP6917447B2/ja
Priority to EP17816998.3A priority patent/EP3494086A1/fr
Priority to KR1020197009225A priority patent/KR102337612B1/ko
Priority to US16/331,242 priority patent/US11084723B2/en
Publication of FR3059994A1 publication Critical patent/FR3059994A1/fr
Application granted granted Critical
Publication of FR3059994B1 publication Critical patent/FR3059994B1/fr
Priority to US17/358,819 priority patent/US20210323823A1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/082Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/086Compounds containing nitrogen and non-metals and optionally metals containing one or more sulfur atoms
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/22Evaporating by bringing a thin layer of the liquid into contact with a heated surface
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/082Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/087Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
    • C01B21/093Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
    • C01B21/0935Imidodisulfonic acid; Nitrilotrisulfonic acid; Salts thereof
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/056Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566Liquid materials
    • H01M10/0568Liquid materials characterised by the solutes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/04Solvent extraction of solutions which are liquid
    • B01D11/0492Applications, solvents used
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00Electrolytes
    • H01M2300/0017Non-aqueous electrolytes
    • H01M2300/0025Organic electrolyte
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/133Renewable energy sources, e.g. sunlight

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Secondary Cells (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

La présente invention concerne un procédé de séchage et purification d'un sel de lithium de bis(fluorosulfonyl)imide en solution dans un solvant organique S1, ledit procédé comprenant les étapes suivantes : a) addition d'eau désionisée pour dissoudre et extraire le sel lithium de bis(fluorosulfonyl)imide, formant une solution aqueuse dudit sel ; b) extraction du sel de lithium de bis(fluorosulfonyl)imide à partir de ladite solution aqueuse, avec un solvant organique S2, cette étape étant répétée au moins une fois; c) concentration du sel de lithium de bis(fluorosulfonyl)imide par évaporation dudit solvant organique S2 et de l'eau, dans un évaporateur à film mince à court trajet, dans les conditions suivantes : - température comprise entre 30°C et 95°C; - pression comprise entre 10-3 mbar abs et 5 mbar abs ; - temps de séjour inférieur ou égal à 15 min ; d) éventuellement cristallisation du sel de lithium de bis(fluorosulfonyl)imide. La présente invention concerne également un sel de lithium de bis(fluorosulfonyl)imide, et ses utilisations dans les batteries Li-ion.
FR1662130A 2016-12-08 2016-12-08 Procede de sechage et de purification de lifsi Active FR3059994B1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
FR1662130A FR3059994B1 (fr) 2016-12-08 2016-12-08 Procede de sechage et de purification de lifsi
PCT/FR2017/053447 WO2018104675A1 (fr) 2016-12-08 2017-12-07 Procédé de séchage et de purification de lifsi
JP2019515208A JP6917447B2 (ja) 2016-12-08 2017-12-07 LiFSIを乾燥及び精製するための方法
EP17816998.3A EP3494086A1 (fr) 2016-12-08 2017-12-07 Procédé de séchage et de purification de lifsi
CN201780068664.3A CN109982966B (zh) 2016-12-08 2017-12-07 干燥和纯化LiFSI的方法
KR1020197009225A KR102337612B1 (ko) 2016-12-08 2017-12-07 Lifsi 의 건조 및 정제 방법
US16/331,242 US11084723B2 (en) 2016-12-08 2017-12-07 Method for drying and purifying LiFSI
US17/358,819 US20210323823A1 (en) 2016-12-08 2021-06-25 METHOD FOR DRYING AND PURIFYING LiFSI

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1662130 2016-12-08
FR1662130A FR3059994B1 (fr) 2016-12-08 2016-12-08 Procede de sechage et de purification de lifsi

Publications (2)

Publication Number Publication Date
FR3059994A1 FR3059994A1 (fr) 2018-06-15
FR3059994B1 true FR3059994B1 (fr) 2021-03-19

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
FR1662130A Active FR3059994B1 (fr) 2016-12-08 2016-12-08 Procede de sechage et de purification de lifsi

Country Status (7)

Country Link
US (2) US11084723B2 (fr)
EP (1) EP3494086A1 (fr)
JP (1) JP6917447B2 (fr)
KR (1) KR102337612B1 (fr)
CN (1) CN109982966B (fr)
FR (1) FR3059994B1 (fr)
WO (1) WO2018104675A1 (fr)

Families Citing this family (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3059993A1 (fr) * 2016-12-08 2018-06-15 Arkema France Procede de sechage et de purification du sel de lithium de bis(fluorosulfonyl)imide
CN110540176B (zh) * 2018-05-28 2021-05-18 浙江蓝天环保高科技股份有限公司 一种提高双氟磺酰亚胺锂纯度的方法
FR3081857B1 (fr) * 2018-06-01 2022-05-06 Arkema France Composition de sel de lithium de bis(fluorosulfonyl)imide
KR20210077773A (ko) * 2018-11-16 2021-06-25 에스이에스 홀딩스 피티이. 엘티디. 리튬 이온 및 리튬 금속 배터리 내의 애노드에 대해 안정한 유기 용매를 사용하여 리튬 비스(플루오로설포닐)이미드 (LiFSI)로부터 반응성 용매를 제거하는 방법
US10967295B2 (en) * 2018-11-16 2021-04-06 Ses Holdings Pte. Ltd. Processes for removing reactive solvent from lithium bis(fluorosulfonyl)imide (LiFSI) using organic solvents that are stable toward anodes in lithium-ion and lithium-metal batteries
US10926190B2 (en) * 2018-11-16 2021-02-23 Ses Holdings Pte. Ltd. Purified lithium bis(fluorosulfonyl)imide (LiFSI) products, methods of purifying crude LiFSI, and uses of purified LiFSI products
US10734664B1 (en) * 2019-03-01 2020-08-04 Ses Holdings Pte. Ltd. Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude HFSI, and uses of purified HFSI products
KR102181108B1 (ko) 2019-09-11 2020-11-20 (주)부흥산업사 리튬 비스(플루오로술포닐)이미드와 그 제조방법
CN110697668B (zh) 2019-11-20 2021-08-06 上海如鲲新材料有限公司 一种高纯度双氟磺酰亚胺盐的制备方法
JP7340685B2 (ja) * 2020-02-27 2023-09-07 株式会社日本触媒 組成物、電解液材料及び電解液
CN111547689A (zh) * 2020-04-26 2020-08-18 广州理文科技有限公司 一种双亚胺锂的化学干燥与纯化的方法
JP2023541873A (ja) * 2020-09-10 2023-10-04 ソルヴェイ(ソシエテ アノニム) ビス(フルオロスルホニル)イミド塩の精製
KR102693113B1 (ko) * 2021-07-08 2024-08-09 주식회사 천보 고순도 리튬 비스(플루오로설포닐)이미드의 제조방법
CN113666346B (zh) * 2021-08-23 2022-11-25 泰兴华盛精细化工有限公司 一种双氟磺酰亚胺锂短程蒸馏高效提纯装置及其提纯方法
WO2023046720A1 (fr) 2021-09-23 2023-03-30 Rhodia Operations Méthode de production de bis(chlorosulfonyl)imide ultra pur
CN113562710B (zh) * 2021-09-24 2021-12-28 江苏华盛锂电材料股份有限公司 降低双氟磺酰亚胺锂盐中溶剂残留的方法
CN118434672A (zh) * 2021-12-23 2024-08-02 法国特种经营公司 用于从双(氟磺酰基)亚胺溶液中去除水的方法
CN117246982A (zh) * 2022-06-10 2023-12-19 时代思康新材料有限公司 双氟磺酰亚胺锂和提纯双氟磺酰亚胺锂的方法
WO2024125980A1 (fr) 2022-12-15 2024-06-20 Specialty Operations France Procédé pour fabriquer une solution de sels de bis(fluoro sulfonyl)imide
CN116022748B (zh) * 2022-12-16 2024-02-27 山东惟普新能源有限公司 一种含水双氟磺酰亚胺锂的除水方法

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JP5443118B2 (ja) * 2009-03-31 2014-03-19 三菱マテリアル株式会社 ビス(フルオロスルホニル)イミド塩の製造方法、ビス(フルオロスルホニル)イミド塩及びフルオロ硫酸塩の製造方法、並びにビス(フルオロスルホニル)イミド・オニウム塩の製造方法
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FR2975694B1 (fr) 2011-05-24 2013-08-02 Arkema France Procede de preparation de bis(fluorosulfonyl)imidure de lithium
JP6208929B2 (ja) * 2011-08-12 2017-10-04 株式会社日本触媒 フッ素原子を含むイオン性化合物またはフッ素原子を含むイオン性化合物含有組成物を包装してなる包装体
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JP6139944B2 (ja) * 2013-04-01 2017-05-31 株式会社日本触媒 フルオロスルホニルイミドのアルカリ金属塩の製造方法
JP6368466B2 (ja) * 2013-09-09 2018-08-01 株式会社日本触媒 フルオロスルホニルイミドの包装体の製造方法
FR3020060B1 (fr) * 2014-04-18 2016-04-01 Arkema France Preparation d'imides contenant un groupement fluorosulfonyle
FR3022695A1 (fr) * 2014-06-18 2015-12-25 Rhodia Operations Procede de recuperation d'un sel d'electrolyte
CN105523530B (zh) * 2014-10-23 2018-09-07 浙江蓝天环保高科技股份有限公司 一种双(氟磺酰)亚胺钾的制备方法
JP2016088809A (ja) * 2014-11-05 2016-05-23 株式会社日本触媒 フルオロスルホニルイミド塩の製造方法
JP6792394B2 (ja) * 2016-09-27 2020-11-25 株式会社日本触媒 ビス(フルオロスルホニル)イミドのアルカリ金属塩と有機溶媒とを含む電解液材料の製造方法
JP6806514B2 (ja) * 2016-09-27 2021-01-06 株式会社日本触媒 ビス(フルオロスルホニル)イミドのアルカリ金属塩と有機溶媒とを含む電解液材料の製造方法
FR3059993A1 (fr) * 2016-12-08 2018-06-15 Arkema France Procede de sechage et de purification du sel de lithium de bis(fluorosulfonyl)imide

Also Published As

Publication number Publication date
KR20190040348A (ko) 2019-04-17
CN109982966A (zh) 2019-07-05
US20210323823A1 (en) 2021-10-21
US11084723B2 (en) 2021-08-10
FR3059994A1 (fr) 2018-06-15
JP6917447B2 (ja) 2021-08-11
CN109982966B (zh) 2022-11-01
EP3494086A1 (fr) 2019-06-12
US20190292053A1 (en) 2019-09-26
JP2020500132A (ja) 2020-01-09
WO2018104675A1 (fr) 2018-06-14
KR102337612B1 (ko) 2021-12-08

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