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WO2025032030A1 - Bis(fluorosulfonyl)imide d'ammonium de haute pureté et son procédé de fabrication - Google Patents

Bis(fluorosulfonyl)imide d'ammonium de haute pureté et son procédé de fabrication Download PDF

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Publication number
WO2025032030A1
WO2025032030A1 PCT/EP2024/072107 EP2024072107W WO2025032030A1 WO 2025032030 A1 WO2025032030 A1 WO 2025032030A1 EP 2024072107 W EP2024072107 W EP 2024072107W WO 2025032030 A1 WO2025032030 A1 WO 2025032030A1
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ppm
composition
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comp
fsi
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Inventor
Joo-Hee KANG
Philippe Carvin
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Specialty Operations France SAS
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Specialty Operations France SAS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/086—Compounds containing nitrogen and non-metals and optionally metals containing one or more sulfur atoms
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
    • C01B21/093—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more sulfur atoms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries

Definitions

  • Bis(fluorosulfonyl)imide and salts thereof, in particular the lithium salt of bis(fluorosulfonyl)imide (LiFSI), are useful compounds in a variety of technical fields, including in battery electrolytes.
  • LiFSI lithium salt of bis(fluorosulfonyl)imide
  • the presence of impurities is an important issue, both in the final compound (e.g. LiFSI) and in the intermediate compounds (e.g. NH4FSI).
  • patent documents JP 2016124735 in the name of Nippon Catalytic Chem Ltd.
  • JP 2016145147 in the name of Nippon Catalytic Chem Ltd.
  • JP 2016124735 discloses a method for producing a fluorosulfonyl imide compound comprising the reaction of a chlorosulfonyl imide compound with NH 4 F(HF) p , wherein p is 0 to 10.
  • the fluorosulfonyl imide compound may be reacted with an alkali metal compound to produce an alkali metal salt of fluorosulfonyl imide.
  • EP 3381923 discloses a method for producing lithium bis(fluorosulfonyl)imide, which consists in reacting bis(chlorosulfonyl)imide with a fluorinating reagent in a solvent, followed by treatment with an alkaline reagent, thereby producing ammonium bis(fluorosulfonyl)imide, and then reacting the ammonium bis(fluorosulfonyl)imide with a lithium base to produce lithium bis(fluorosulfonyl)imide.
  • WO 2016/093399 in the name of Chun Bo.
  • EP 2674395 discloses a process for producing a fluorosulfonyl imide ammonium salt with maximum suppression of the contamination of metal impurities. This process consists in reacting a specific chlorosulfonyl imide ammonium salt with hydrogen fluoride. The fluorosulfonyl imide ammonium salt obtained therefrom is then reacted with an alkali metal compound to obtain a fluorosulfonylimide alkali metal salt.
  • WO 2020/099527 discloses a process for producing an alkali salt of bis(fluorosulfonyl)imide economically feasible at industrial scale and which provides a high-purity product.
  • Said process consists in reacting bis(chlorosulfonyl)imide or salts thereof with ammonium fluoride to produce ammonium salt of bis(fluorosulfonyl)imide, crystallizing by adding at least one precipitation solvent and separating the ammonium salt of bis(fluorosulfonyl)imide and reacting the crystallized ammonium salt of bis(fluorosulfonyl)imide with an alkali salt to obtain alkali salt of bis(fluorosulfonyl)imide.
  • KR 2020/0061058 discloses a method for purifying ammonium bis(fluorosulfonyl)imide via the reaction between HCSI and NH4-F, which is then neutralized with a neutralization agent (eg. NR4OHH) followed by re- crystallization in an organic solvent, thus reaching a purity of 99.50%.
  • a neutralization agent eg. NR4OHH
  • WO 2021/082450 discloses a method for purifying HFSI by using sCO2, wherein the method requires the addition of a strong acid to the HFSI composition. At the end of such method, the sCO2 extracts the final product and not the impurities.
  • an object of the present invention relates to a process for purifying an ammonium salt of bis(fluorosulfonyl)imide (NH 4 FSI), which is economically feasible at industrial scale and which provides a high-purity product.
  • NH 4 FSI bis(fluorosulfonyl)imide
  • the Applicant surprisingly manufactured a composition comprising ammonium salt of bis(fluorosulfonyl)imide, such composition being characterized by the presence of a specific compound in a determined amount.
  • such compound has never been disclosed in the art as an ingredient in a composition comprising ammonium bis(fluorosulfonyl)imide.
  • Figure 1 represents a scheme of the laboratory setup used in Example 1.
  • composition (COMP) comprising: - an ammonium salt of bis(fluoro sulfonyl)imide [NH4FSI]; and - at least one compound of formula (I) as represented below or an ammonium salt thereof (I) in an amount up to 200 ppm, as measured by ion chromatography.
  • composition (COMP) comprises said compound of formula (I) or an ammonium salt thereof in an amount below 100 ppm, more preferably below 75 ppm, even more preferably below 50 ppm and still more preferably below 25 or below 15 ppm or even below 5 ppm.
  • composition (COMP) comprises said compound of formula (I) or an ammonium salt thereof in an amount of at least 0.1 ppm, more preferably of at least 0.5 ppm, even more preferably of at least 1.0 ppm.
  • composition (COMP) can comprise further compounds and/or ingredients. 6 SPOP 2023/006 [0022]
  • composition (COMP) can comprise at least one salt of FSO3- in an amount up to 100 ppm, as measured by ion chromatography.
  • composition (COMP) comprises said at least one salt of FSO 3 - in an amount from 0.1 ppm to 100 ppm, preferably from 0.5 ppm to 50 ppm, more preferable from 0.5 ppm to 20 ppm and even more preferably from 0.5 ppm to 5 ppm.
  • composition (COMP) can comprise at least one compound of formula (II) or a salt thereof: (II) .
  • said compound of formula (II) is in an amount up to 100 ppm as measured by ion chromatography.
  • composition (COMP) comprises said compound (II) in an amount up to 50 ppm and more preferably up to 10 ppm, as measured by ion chromatography.
  • compounds (I) and (II) exist as represented above or in their deprotonated forms.
  • compound (I) exists as follows: 7 SPOP 2023/006 .
  • (II) exists as follows: .
  • composition (COMP) comprises NH4FSI salt in an amount above 99.50%, preferably more than 99.60%, more preferably more than 99.80%, and even more preferably more than 99.95%, as measured by 19 F- NMR.
  • the composition according to the present invention further comprises: - fluoride (F-), in an amount up to 50 ppm, for example less than 40 ppm, less than 30 ppm, less than 25 ppm and even more preferably less than 10 ppm as measured by Ion Chromatography (IC); and/or - chloride (Cl-), in an amount up to 50 ppm, for example less than 40 ppm, less than 30 ppm, less than 20 ppm, less than 10 ppm or even less than 5 ppm as measured by IC; and/or - sulfate (SO 4 2- ), in an amount up to 50 ppm, for example less than 40 ppm, less than 30 ppm, less than 25 ppm and even more preferably less than 10 ppm as measured by IC; and/or 8 SPOP 2023/006 - acid substances different from sulfate (SO4 2- ), in an amount up to 100 ppm, for example less than 50
  • said acid substances different from sulfate (SO 4 2- ) are selected from NH 2 SO 3 - and/or FSO 3 -.
  • said acid substances different from sulfate (SO4 2- ) are in the following amounts: - less than 50 ppm of sulfamate (NH 2 SO 3 -), for example less than 40 ppm, less than 30 ppm, less than 20 ppm, less than 10 ppm or even less than 5 ppm as measured by IC; and/or - less than 50 ppm of fluorosulfonate (FSO 3 -), for example less than 40 ppm, less than 30 ppm, less than 20 ppm, less than 10 ppm or even less than 5 ppm as measured by IC.
  • composition (COMP) is further characterized in that it contains less than 50 ppm of water, as measured by the KF analysis (oven method), preferably, less than 40 ppm, less than 30 ppm, less than 20 ppm, less than 10 ppm or even less than 5 ppm of water.
  • said composition (COMP) is a solid composition.
  • composition (COMP) can be provided as a liquid composition.
  • composition (COMP) further comprises at least one solvent [solvent (S1)].
  • said at least one solvent (S1) is selected in the group comprising, more preferably consisting of: ethylene carbonate, propylene carbonate, butylene carbonate, ⁇ -butyrolactone, ⁇ -valerolactone, dimethoxymethane, 1,2-dimethoxyethane, tetrahydrofuran, 2-methyltetrahydrofuran, 1,3-dioxane, 9 SPOP 2023/006 4-methyl-1,3- dioxolane, methyl formate, methyl acetate, methyl propionate, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, sulfolane, 3- methylsulfolane, dimethylsulfoxide, N,N-dimethylformamide, N-methyl oxazolidinone, acetonitrile, valeronitrile, benzonitrile, ethyl acetate, isopropyl acetate, n
  • said solvent (S1) is selected from ethylene carbonate, propylene carbonate, butylene carbonate, tetrahydrofuran, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, isopropyl acetate and n-butyl acetate, even more preferred solvents include dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, isopropyl acetate and n-butyl acetate.
  • said solvent (S1) is selected from ethyl methyl carbonate and n-butyl acetate.
  • a second object of the present invention relates to a method for purifying an ammonium salt of bis(fluorosulfonyl)imide (NH 4 FSI), said method comprising the steps of: (a) providing a crude composition [crude NH 4 FSI] comprising NH 4 FSI and at least one other compound; (b) contacting said crude NH4FSI with at least one supercritical fluid; and (c) recovering a composition comprising NH4FSI and at least one other compound in an amount lower than the crude NH 4 FSI.
  • the term “crude composition” (hereinafter referred to as “crude NH4FSI”) hereby means that the composition comprises NH4FSI molecules in admixture with at least one other compound, which is an undesired compound negatively affecting the properties of the NH 4 FSI when used - for example - as an intermediate for the production of high purity LiFSI electrolyte for battery applications.
  • at least one other compound can be referred to as an “impurity”.
  • Said impurity comprises for example ions, solvent(s), water and/or reaction by-products.
  • the crude 10 SPOP 2023/006 NH4FSI may comprise from 80 to 99 wt.% of NH4FSI, preferably 85-98 wt.%, more preferably 90-97 wt.% by weight, the rest being impurities to be removed through the process of the present invention.
  • the crude NH 4 FSI can be in the form of a solid, such as powder, or of a slurry or of a liquid, such as a solution.
  • the term “contacting” hereby means that the crude NH 4 FSI is put in contact with the at least one supercritical fluid.
  • such contacting takes place in a vessel, under specific conditions of pressure and temperature, for a period of time sufficient for the fluid to remove at least part of the impurities present in the crude NH4FSI, preferably more than 80.00%, more than 90.00%, more than 95.00%, more than 99.00%, more than 99.50% or even more than 99.90%. More preferentially, all the impurities are removed and the NH 4 FSI salt presents a purity above 99.95%, or even above 99.99%.
  • the term “recovering” hereby means that the purified NH4FSI, preferably in solid form, is removed or extracted from the vessel in which step b) is carried out.
  • the expression “supercritical fluid” hereby means a gas (or a mixture of at least two gasses) in its supercritical state.
  • the pressures and temperatures to be used in the vessel in which the contact between the solution and the supercritical fluid takes place are properly selected. More precisely, in order to be in a supercritical state, the gas employed in step b) is held at or above its critical temperature and critical pressure.
  • at least one supercritical fluid is used to extract a purified NH 4 FSI salt from the crude NH 4 FSI, with several advantages.
  • step (a) is carried out in batch, semi-continuously or continuously.
  • said at least one other compound present in the crude NH4FSI is selected from the group comprising, more preferably consisting of: water (H 2 O), fluoride (F-), chloride (Cl-), sulfate (SO 4 2- ), sulfamate (NH 2 SO 3 -), flurosulfonate (FSO3-), [NH(SO2F)(SO2NH2)] or an ammonium salt thereof, and/or [NH(SO3H)(SO2F)] or an ammonium salt thereof.
  • the crude NH 4 FSI to be purified may contain at least one of the following impurities: NH4Cl, NH4F, NH4HF2, NH4FSO3, NH4SO3NH2, [NH(SO2F)(SO2NH2)] or an ammonium salt thereof, and/or [NH(SO 3 H)(SO 2 F)] or an ammonium salt thereof.
  • the parameters of the process according to the present invention can be properly selected and optimized based for example on the starting material (in particular, on the amount of the other compound(s) in the crude NH 4 FSI) and on the scale at which the process is performed, for example is the process is performed at industrial scale or at laboratory scale.
  • step (b) is carried out at a pressure (p) of at least 80 bars.
  • step (b) is carried out at a temperature (T) between 30oC and 90oC.
  • T temperature between 30oC and 90oC.
  • a particular advantage of the process of the present invention is that the contacting time under step (b) is short. Also, advantageously, the contacting time under step (b) can be properly selected for example on the basis of the starting material and the desired yield.
  • the contacting time under step (b) varies between a few seconds, for example 5 seconds, and 24 hours.
  • the contacting time 12 SPOP 2023/006 under step d) varies between 1 minute and 12 hours, for example between 5 minutes and 10 hours or between 10 minutes and 5 hours or between 20 minutes and 3 hours.
  • step (b) the crude NH 4 FSI is contacted with at least one supercritical fluid.
  • step (b) takes place in a vessel.
  • the term “vessel” hereby means a container which is well-suited for the process of the present invention, that-is-to-say which is adapted to withstand the pressures and temperatures used in the process of the present invention, as well as to the possible corrosive character of the reactants and products involved in this process.
  • step (b) consists in contacting the crude NH 4 FSI of step (a) with at least one supercritical fluid in a vessel.
  • the crude NH4FSI is contacted with one fluid in a supercritical state.
  • the crude NH 4 FSI is contacted with two or more fluids in a supercritical state. Said two or more fluids may be mixed or may be contacted with the crude NH4FSI sequentially.
  • the crude NH 4 FSI may be contacted with a mixture of at least two supercritical fluids.
  • at least one other component also called herein modifier, may be mixed to the supercritical fluid(s).
  • said at least one other component is selected from polar solvents having a solubility in the supercritical fluid below 10 wt.% based on the total weight of the supercritical fluids and the other component(s).
  • said at least one other component is in an amount ranging from 0.1 to 10 wt.%, for example from 0.5 to 8 wt.% or from 1 to 6 wt.%, based on the total weight of the supercritical fluids and the other component(s).
  • said at least one other component is selected from polar solvents, more preferably, in the group comprising: alcohol, toluene, dimethyl sulfoxide (DMSO), acetonitrile, and the like.
  • said polar solvent is alcohol. Even more preferably, said alcohol is ethanol.
  • step (b) may be repeated one or several times.
  • the process according to the present invention comprises a first step (b) and a second step (b’), wherein the same or different supercritical fluid(s), or a mixture of at least two supercritical fluids, are used in each of said step (b) and said step (b’).
  • the vessel which is preferably used to contact the crude NH 4 FSI with the at least one supercritical fluid under step (b) is at a pressure (p) of at least 73 bars (7.3 MPa) during the extraction.
  • the vessel which is preferably used to contact the crude NH4FSI with the at least one supercritical fluid under step (b) is at a temperature (T) between 30 oC and 90 oC during the extraction.
  • the temperature (T) in the vessel may vary between 37 oC and 75 oC, for example between 38 oC and 70 oC or between 40 oC and 65 oC.
  • the pressure (p) in the vessel may be at least 80 bars (8.0 MPa), at least 100 bars (10.0 MPa), at least 130 bars (13.0 MPa), at least 150 bars (15.0 MPa) or at least 200 bars (20.0 MPa).
  • step (b) is carried out by injection of the crude NH4FSI in the vessel, which is already pressurized.
  • said crude NH 4 FSI is in a solid form, preferably in the form of powder.
  • said crude NH4FSI is in a liquid form, such as a solution comprising NH4FSI and an organic aprotic solvent.
  • said organic aprotic solvent is selected in the group comprising ethylene carbonate, propylene carbonate, butylene carbonate, ⁇ - butyrolactone, ⁇ -valerolactone, dimethoxymethane, 1,2-dimethoxyethane, tetrahydrofuran, 2-methyltetrahydrofuran, 1,3-dioxane, 4-methyl-1,3 - dioxolane, methyl formate, methyl acetate, methyl propionate, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, sulfolane, 3- methylsulfolane, dimethylsulfoxide, N,N-dimethylformamide, N-methyl oxazolidinone, acetonitrile, valeronit
  • said solvent is selected from ethylene carbonate, propylene carbonate, butylene carbonate, tetrahydrofuran, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, isopropyl acetate and n-butyl acetate. Even more preferably, said solvent is selected from dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, isopropyl acetate and n-butyl acetate. Still more preferably, said solvent is selected from ethyl methyl carbonate and n-butyl acetate.
  • step (b) comprises: (b1) introducing the crude NH4FSI in the vessel; (b2) pressurizing the vessel to a pressure (p); (b3) heating the vessel to a temperature (T); (b4) introducing the at least one supercritical fluid in the vessel.
  • step (b2) may be performed before step (b3), or step (b3) may be performed before step (b2), or step (b2) and step (b3) may be performed concomitantly.
  • step (b2) is performed at a pressure of at least 74 bars (7.4 MPa).
  • step (b3) is performed at a temperature of at least 30°C.
  • the flow rate for introducing the supercritical fluid in the vessel under step (b4) is not particularly limited.
  • the flow rate can be selected based on the apparatus used and the amount and purity of the crude NH4FSI.
  • Step (b4) can be performed in batch, continuously or semi-continuously.
  • the supercritical fluid used in step (b) comprises supercritical carbon dioxide (sCO2).
  • sCO2 is a fluid state of carbon dioxide that is held at or above its critical temperature (31.0 oC) and critical pressure (7.3773 MPa).
  • the supercritical fluid used in step (b) may consist essentially in sCO 2 , or it may consist in sCO 2 .
  • the sCO2 is mixed with up to 10 wt.% of ethanol, for example with 0.1 to 8 wt.% of ethanol, the wt.% being based on the total weight of the supercritical fluid and the ethanol.
  • the weight ratio of the supercritical fluid to the crude NH4FSI used in the process of the present invention may vary between 1/1 and 400/1.
  • the weight ratio of the supercritical fluid to the crude NH 4 FSI preferably varies between 5/1 and 350/1, for example between 20/1 and 300/1, between 30/1 and 250/1 or between 40/1 and 200/1.
  • the process of the present invention may be carried out in a batch mode, in a continuous or semi-continuous mode.
  • the process is carried out in a continuous or semi-continuous manner.
  • the process of the present invention comprises a step of continuously or semi-continuously withdrawing the purified salt of NH4FSI from the vessel.
  • the injection of the crude NH 4 FSI in the vessel is performed in a continuous or semi-continuous manner.
  • the crude NH4FSI is continuously injected in the vessel or alternatively the crude NH 4 FSI is semi- continuously injected in the vessel.
  • the crude NH 4 FSI may be injected in the vessel for a certain time (as an example between 30 and 120 sec, for example 60 sec) and then the injection is stopped for another period of time, which can be equal to, shorter or longer than the injection time.
  • the supercritical fluid can be introduced in the vessel in a continuous or semi-continuous manner.
  • the process of the present invention may comprise a step of continuously or semi-continuously withdrawing the salt of NH 4 FSI from the vessel.
  • the purified NH 4 FSI which is recovered in step (c) is preferably in solid form.
  • the purified NH 4 FSI is preferably recovered in the solid form, regardless if 17 SPOP 2023/006 the starting crude NH4FSI is in solid form, in the form of a slurry or a liquid. Even more preferably, said purified NH4FSI is in the form of a powder.
  • step (c) the NH 4 FSI in solid form can be recovered once step (b) is finished or while step b) is proceeding.
  • step (c) the purified NH4FSI flows into a separator with the supercritical fluid. The pressure is released and the supercritical fluid becomes a gas. Such gas is preferably recycled, as detailed below.
  • the process of the present invention may further comprise additional steps, such as preferably at least one step consisting in recycling the supercritical fluid.
  • the supercritical fluid may be reinjected in the process of the present invention as such or after additional step(s) of purification.
  • the recycling of the supercritical fluid may be performed in several ways.
  • the supercritical fluid may be recycled in a continuous way during the process. Preferably, it is recycled using a supercritical fluid pipe under pressure.
  • the supercritical fluid may be recovered as a liquid phase by releasing the pressure in the vessel, and then repressurizing it in its gas form, for example by means of a compressor, in order to recycle it as a supercritical fluid which can be rejected in the vessel.
  • the process of the present invention may be carried out in an equipment comprising: - a vessel, which withstands the pressure and temperature used, for example a pressure (p) of at least 73 bars (7.3 MPa) and a temperature (T) above 30oC; - a solvent trap; 18 SPOP 2023/006 - a gas tank and a supercritical gas generator; - at least one injector/entry valve mounted on the vessel; and - optionally a separator.
  • the vessel may preferably be made of sapphire, SS316L, glass or graphite filled PTFE.
  • the equipment may include a separator. Different separators may be used in the process of the present invention.
  • the separation may be carried out through traditional filtration (also referred to as "dead end filtration") or cross filtration, which is also called tangential filtration, as disclosed for example in US 2007/0021570 (in the name of Solvay SA.).
  • cyclonic separators may be used, for example those which operate as gas/solid separators.
  • the cyclonic separators are advantageous as solids which could plug the filter media are recovered.
  • the solid NH 4 FSI is recovered at the end of the process via a frit filter.
  • said frit filter can be made of stainless steel.
  • said frit filter has at least one of the following characteristics: pore size between 1 and 6 ⁇ m, preferably from 2 to 4 ⁇ m; diameter between 1 and 20 mm, preferably between 5 and 15 mm, more preferably about 10 mm; and/or a thickness from 0.1 to 5 mm, preferably between 0.7 and 3.5 mm, more preferably between 1.5 and 2.5 mm.
  • the filter(s) may notably be positioned at the bottom or at the top of the vessel.
  • composition (COMP) as defined above is obtained at the end of step (c) of the method according to the present invention.
  • Another object of the present invention relates to the use of ammonium salt of bis(fluorosulfonyl)imide (NH4FSI) in the solid form according to the present invention, as an intermediate in the manufacture of LiFSI, a battery electrolyte salt.
  • Another object of the present invention is the use of supercritical fluid extraction for purifying a crude ammonium salt of bis(fluorosulfonyl)imide (NH 4 FSI) comprising NH 4 FSI and at least one impurity.
  • Example 1 – Preparation of high purity NH4FSI in powder form starting from crude NH4FSI [00118] The equipment setup of Figure 1 was used and the experiment was performed with the following procedure. [00119] 10.668 g of crude NH4FSI was introduced into a vessel. The vessel was pressurized with sCO 2 (Temperature 45oC; Pressure 200 bars; CO 2 /NH 4 FSI solution ratio varying between 30 and 400 along the process).

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  • Manufacturing & Machinery (AREA)
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Abstract

La présente invention concerne un sel d'ammonium de haute pureté de bis(fluorosulfonyl)imide (NH4FSI), un procédé pour sa fabrication et son utilisation en tant qu'intermédiaire pour produire du bis(fluorosulfonyl)imide de lithium de haute pureté (LiFSI).
PCT/EP2024/072107 2023-08-07 2024-08-05 Bis(fluorosulfonyl)imide d'ammonium de haute pureté et son procédé de fabrication Pending WO2025032030A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP23306342 2023-08-07
EP23306342.9 2023-08-07

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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070021570A1 (en) 2005-07-15 2007-01-25 Solvay (Societe Anonyme) Process for preparing a halogenated polymer and device for its implementation
US7410620B2 (en) 1999-11-12 2008-08-12 North Carolina State University Apparatus for continuous production of polymers in carbon dioxide
US20130331609A1 (en) 2011-03-03 2013-12-12 Nippon Soda Co., Ltd. Production process for fluorosulfonylimide ammonium salt
EP2674395A1 (fr) 2011-02-10 2013-12-18 Nippon Soda Co., Ltd. Procédé pour la production de sel d'ammonium de fluorosulfonylimide
WO2016093399A1 (fr) 2014-12-11 2016-06-16 Chun Bo Ltd Sel sulfonyl imide de lithium contenant du fluor et procédé de purification pour ce dernier
JP2016124735A (ja) 2014-12-26 2016-07-11 株式会社日本触媒 フルオロスルホニルイミド化合物の製造方法
JP2016145147A (ja) 2015-02-03 2016-08-12 株式会社日本触媒 フルオロスルホニルイミド化合物の製造方法
EP3381923A1 (fr) 2015-11-26 2018-10-03 CLS Inc. Nouveau procédé de préparation de bis(fluorosulfonyl)imide delithium
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