Classifications

• • 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
  • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
  • C01D15/00—Lithium compounds
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/80—Compositional purity
  • C01P2006/82—Compositional purity water content
• • Y—GENERAL 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
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
  • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
  • Y02E60/10—Energy storage using batteries

Definitions

• the present disclosure relates to an aqueous alkali metal bis (fluorosulfonyl) imide solution, a container containing the aqueous solution, and a method for storing or transporting the aqueous solution.
• Alkali metal bis (fluorosulfonyl) imides such as lithium bis (fluorosulfonyl) imide are useful as intermediates for compounds having two N (SO 2 F) groups. It is also useful in various applications such as being used as an additive to an electrolyte, a battery or a capacitor in an electrolytic solution, a selective electrophoretic fluorinating agent, a photoacid generator, a thermoacid generator, a near-infrared absorbing dye, and the like. It is a compound (Patent Document 1).
• an aqueous solution as a form of an alkali metal bis (fluorosulfonyl) imide product.
• the product is stored and transported in an aqueous solution.
• the alkali metal bis (fluorosulfonyl) imide is susceptible to hydrolysis, and there is a need to further enhance the stability of the alkali metal bis (fluorosulfonyl) imide in an aqueous solution. It turned out to be.
• the present disclosure has been made in view of the above circumstances, and provides an aqueous alkali metal bis (fluorosulfonyl) imide solution having higher storage stability, a container containing the aqueous solution, and a method for storing or transporting the aqueous solution.
• the purpose is to do.
• the aqueous solution of the present disclosure is an aqueous solution containing an alkali metal bis (fluorosulfonyl) imide, and the total content of the alkali metal bis (fluorosulfonyl) imide and water is 98% by mass or more with respect to the total amount of the aqueous solution.
• the aqueous solution of the present disclosure preferably contains 10000 mass ppm or less of fluoride ions with respect to the total amount of the aqueous solution.
• the aqueous solution of the present disclosure preferably contains 10000 mass ppm or less of sulfate ions with respect to the total amount of the aqueous solution.
• the aqueous solution of the present disclosure preferably contains 1 to 10000 mass ppm of amidosulfate ion with respect to the total amount of the aqueous solution.
• the aqueous solution of the present disclosure preferably contains 1 to 90% by mass of alkali metal bis (fluorosulfonyl) imide with respect to the total amount of the aqueous solution.
• the container containing an aqueous solution of the present disclosure includes a container and an aqueous solution contained in the container, and the aqueous solution is the above-mentioned aqueous solution.
• the container contains at least one of the materials selected from the group consisting of resin, glass, and metal.
• the method for storing or transporting an aqueous solution containing an alkali metal bis (fluorosulfonyl) imide of the present disclosure is for storing or transporting the above aqueous solution.
• an alkali metal bis (fluorosulfonyl) imide aqueous solution having higher storage stability a container containing the aqueous solution, and a method for storing or transporting the aqueous solution.
• the alkali metal bis (fluorosulfonyl) imide aqueous solution of the present disclosure has a total content of alkali metal bis (fluorosulfonyl) imide and water of 98% by mass or more and a pH of 10 or less with respect to the total amount of the aqueous solution. is there. Since the aqueous solution of the present disclosure has excellent storage stability, it is suitable for storing or transporting an alkali metal bis (fluorosulfonyl) imide in an aqueous solution state.
• the alkali metal bis (fluorosulfonyl) imide aqueous solution is also simply referred to as an MFSI aqueous solution.
• the alkali metal bis (fluorosulfonyl) imide is an alkali metal salt of bis (fluorosulfonyl) imide and is a compound represented by the general formula: MN (SO 2 F) 2 (M is an alkali metal).
• M include Li, Na, K, Rb, and Cs. Li, Na, or K is preferable, and Li is more preferable.
• the alkali metal bis (fluorosulfonyl) imide is also simply referred to as MFSI, and when the alkali metal bis (fluorosulfonyl) imide containing a specific alkali metal is referred to, M is replaced with the alkali metal.
• fluorosulfonic acid amide When MFSI is hydrolyzed, fluorosulfonic acid amide is produced.
• the presence of fluorosulfonic acid amide is not preferable because even a small amount of fluorosulfonic acid amide adversely affects battery performance and the like.
• Fluorosulfuric acid amide is produced by reacting with water contained in air or an organic solvent even in a solid of MFSI (powder or the like) or a solution in which MFSI is dissolved in an organic solvent.
• the fluorosulfonic acid amide is immediately hydrolyzed and disappears in an aqueous solution.
• the MFSI is stored as a solid (powder or the like) or a solution dissolved in an organic solvent
• the content of the fluorosulfonic acid amide can be suppressed to a low level.
• the MFSI contained in the MFSI aqueous solution may contain two or more kinds of alkali metals, but it is preferable to contain only one kind of alkali metals.
• the inclusion of only one kind of alkali metal means that the total amount of alkali metals other than the kind of alkali metal in the MFSI aqueous solution is at the impurity level.
• the alkali metal contained in the MFSI aqueous solution is preferably 1 mol% or less, more preferably 0.5 mol% or less, and more preferably 0.1 mol% or less, based on the total amount of ions. More preferred.
• the total content of MFSI and water in the MFSI aqueous solution is preferably 98.5% by mass or more, and more preferably 99% by mass or more.
• the pH of the MFSI aqueous solution is preferably less than 7, more preferably 6 or less, and even more preferably 5 or less, from the viewpoint of further enhancing the storage stability of the MFSI aqueous solution. Further, the pH of the MFSI aqueous solution is preferably -3 or more, more preferably 1 or more, and 2 or more from the viewpoint of handleability such as suppressing the generation of impurities when extracting MFSI with an organic solvent. It is more preferable to have it, and it is particularly preferable to have 4 or more.
• the pH of the MFSI aqueous solution is preferably -3 to 10, more preferably -3 or more and less than 7, and -3 to 6. It is more preferable, and 0 to 6 is particularly preferable.
• the pH of the MFSI aqueous solution can be measured with a pH meter, pH test paper, or the like.
• the content of MFSI in the MFSI aqueous solution is not particularly limited as long as it is equal to or less than the saturation concentration of MFSI, and may be 1 to 90% by mass or 5 to 85% by mass with respect to the total amount of the MFSI aqueous solution. Good.
• the content of MFSI in the MFSI aqueous solution is preferably 5 to 90% by mass, more preferably 7 to 85% by mass, and 10 to 80% by mass with respect to the total amount of the MFSI aqueous solution.
• the content of MFSI in the MFSI aqueous solution may be 30% by mass or more, 32% by mass or more, or 35% by mass or more with respect to the total amount of the MFSI aqueous solution (upper limit). May be the saturated concentration of MFSI).
• the MFSI aqueous solution of the present disclosure may contain fluoride ions (F ⁇ ).
• the content of fluoride ions in the MFSI aqueous solution is preferably 10,000 mass ppm or less, more preferably 1 to 1000 mass ppm, still more preferably 1 to 500 mass ppm, based on the total amount of the MFSI aqueous solution. It is particularly preferably 2 to 100 mass ppm, and even more preferably 3 to 50 mass ppm.
• the fluoride ion may not be contained in the MFSI aqueous solution, and the content of the fluoride ion may be substantially 0 mass ppm.
• the content of fluoride ions in the MFSI aqueous solution may be 1000 mass ppm or less with respect to the total amount of the MFSI aqueous solution.
• the pH can be adjusted to a preferable range by adding an acid containing fluoride ions to the MFSI aqueous solution of the present disclosure.
• the acid used here include hydrofluoric acid, acidic ammonium fluoride and the like. As a result of pH adjustment, the above fluoride ions may be contained.
• MFSI solution of the present disclosure may include a sulfate ion (SO 4 2-).
• the content of sulfate ions in the MFSI aqueous solution is preferably 10,000 mass ppm or less, more preferably 2 to 1000 mass ppm, and further preferably 3 to 500 mass ppm, based on the total amount of the MFSI aqueous solution. It is particularly preferably about 100 mass ppm, and even more preferably 10 to 50 mass ppm.
• the sulfate ion may not be contained in the MFSI aqueous solution, and its content may be substantially 0 mass ppm.
• the sulfate ion may not be contained in the MFSI aqueous solution, and the content of the sulfate ion may be substantially 0 mass ppm.
• the pH can be adjusted to a preferable range by adding an acid containing sulfate ions to the MFSI aqueous solution of the present disclosure.
• the acid used here include sulfuric acid, ammonium sulfate, ammonium hydrogen sulfate, lithium hydrogen sulfate, sodium hydrogen sulfate, potassium hydrogen sulfate and the like.
• the above sulfate ion may be contained.
• the content of sulfate ions in the MFSI aqueous solution can be 10,000 mass ppm or less, or 100 to 5000 mass ppm, based on the total amount of the MFSI aqueous solution. It can be 500 to 3000 mass ppm.
• fluorosulfonic acid ion (FSO 3 -) may be contained.
• the content of fluorosulfate ion in the MFSI aqueous solution is preferably 10,000 mass ppm or less with respect to the total amount of the MFSI aqueous solution from the viewpoint of purification efficiency when separating MFSI from the MFSI aqueous solution with an organic solvent, and is preferably 2 to 1000 mass ppm. It is more preferably mass ppm, further preferably 3 to 500 mass ppm, particularly preferably 5 to 100 mass ppm, and even more preferably 10 to 50 mass ppm.
• the fluorosulfate ion may not be contained in the MFSI aqueous solution, and the content of the fluorosulfate ion may be substantially 0 mass ppm.
• the MFSI aqueous solution of the present disclosure may contain amidosulfate ions.
• amidosulfate ions neutralizes the excess base, making it difficult for the pH of the MFSI aqueous solution to exceed 10.
• amidosulfate ions are gradually hydrolyzed in an MFSI aqueous solution during storage to produce ammonium hydrogensulfate. Since the pH of the MFSI aqueous solution is less likely to fluctuate due to the buffering action of the generated ammonium hydrogen sulfate, it is easy to maintain the pH of the MFSI aqueous solution in an appropriate range.
• the content of amide sulfate ion is preferably 1 to 10000 mass ppm, more preferably 10 to 5000 mass ppm, still more preferably 100 to 4000 mass ppm, and 500 to 10000 mass ppm with respect to the total amount of the MFSI aqueous solution. It is particularly preferable to be 3000 mass ppm. Further, the content of amidosulfate ion may be 1500 mass ppm or less, 1 to 1000 mass ppm, or 1 to 500 mass ppm from the viewpoint of reducing the purification load of MFSI. Good. The concentration of amidosulfate ion may be adjusted by adding amidosulfate or a salt thereof (for example, an alkali metal salt of amidosulfate) to the MFSI aqueous solution.
• the MFSI aqueous solution of the present disclosure may contain ammonia or an ammonium salt as impurities.
• the content of ammonia or ammonium salt in the MFSI aqueous solution is preferably 10,000 mass ppm or less, preferably 1000 mass ppm or less, based on the total amount of the MFSI aqueous solution from the viewpoint of separability when separating MFSI from the MFSI aqueous solution with an organic solvent. It is more preferably ppm or less, and further preferably 1 to 500 mass ppm.
• the ammonia or ammonium salt may not be contained in the MFSI aqueous solution, and the content of the ammonia or ammonium salt may be substantially 0 mass ppm.
• the MFSI aqueous solution of the present disclosure may contain impurities derived from raw materials. Such impurities, bis (fluorosulfonyl) imide (H (SO 2 F) 2 N, hereinafter also referred to as HFSI.) And the like.
• the content of HFSI in the MFSI aqueous solution is preferably 7 mol parts or less, more preferably 5 mol parts or less, further preferably 3 mol parts or less, and 2 mol parts or less with respect to 100 mol parts of MFSI. Is particularly preferable, and even more preferably 1 mol part or less.
• the HFSI may not be contained in the MFSI aqueous solution, and the content of the HFSI may be substantially 0 mol part with respect to 100 mol parts of the MFSI.
• the MFSI aqueous solution of the present disclosure preferably does not contain a transition metal compound.
• the content of the transition metal compound in the MFSI aqueous solution is preferably 100 mass ppm or less, preferably 50 mass ppm or less, further preferably 10 mass ppm or less, and 5 mass ppm or less, based on the total amount of the MFSI aqueous solution. Is particularly preferable.
• the transition metal compound include bismuth compounds (bismuth fluoride (BF 3 ), bismuth halides such as bismuth chloride (Bizl 3 ), bismuth oxide and the like) and the like.
• the content of the bismuth compound in the MFSI aqueous solution is preferably 100 mass ppm or less, preferably 50 mass ppm or less, further preferably 10 mass ppm or less, and 5 mass ppm or less, based on the total amount of the MFSI aqueous solution. It is particularly preferable to have it, and even more preferably it is substantially 0 mass ppm.
• the method for preparing the MFSI aqueous solution of the present disclosure is not particularly limited, and examples thereof include the following methods 1) to 3). 1) Dissolve MFSI solid (powder) in water 2) Extract from MFSI organic solvent solution with water 3) Neutralization reaction between HFSI and alkali metal compound in water
• the MFSI solid (powder) used in 1) may be obtained by a conventionally known method. Such a method may be, for example, the one obtained by the methods 2) and 3), and the by-product is removed from the one obtained by the following method 4) or 5). You may.
• examples of the onium ions include ammonium ions, oxonium ions, phosphonium ions, sulfonium ions, and examples of the ammonium ion, NH 4 +, tetramethylammonium, tetrabutylammonium, tripropylamine en Moi bromide etc. Can be mentioned.
• examples of the bis (fluorosulfonyl) imide salt include alkali metal salts, alkaline earth metal salts, ammonium salts, and alkylammonium salts.
• examples of the organic solvent include ether solvents, ester solvents, nitrile solvents, halogen solvents, aromatic solvents, carbonate solvents and the like.
• the alkali metal compound preferably reacts with HFSI to produce a gas that can be easily removed such as water or carbon dioxide as a by-product, and alkali metal hydroxides, alkali metal carbonates and the like are preferable. Can be mentioned.
• almost equimolar HFSI and an alkali metal compound are used so that the unreacted product does not remain in the aqueous solution, and the insoluble unreacted product can be removed by filtration or the like.
• the by-product may be separated from the MFSI by applying the method 2) to the MFSI solution obtained by extracting the MFSI from the aqueous solution of the MFSI produced by the method 3) or 4) with an organic solvent. ..
• the pH can be adjusted by adding an acid or a base.
• the acid is not particularly limited, and examples thereof include hydrofluoric acid, hydrochloric acid, sulfuric acid, sodium hydrogensulfate, potassium hydrogensulfate, and lithium hydrogensulfate.
• bases alkali metal hydroxides (lithium hydroxide, sodium hydroxide, potassium hydroxide, etc.), alkali metal carbonates (lithium carbonate, sodium carbonate, potassium carbonate, etc., lithium hydrogen carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, etc.) ) And so on.
• the container containing the aqueous solution of the present disclosure contains the above-mentioned MFSI aqueous solution in the container. That is, the container containing the aqueous solution of the present disclosure includes a container and the MFSI aqueous solution of the present disclosure contained in the container.
• Aqueous solution refers to a state in which the aqueous solution is already contained in the container.
• the material of the container there are no particular restrictions on the material of the container, and any material such as resin, glass, or metal can be used.
• the resin include polypropylene, polyethylene, vinyl chloride, PET, PTFE, PFA and the like.
• the glass include soda-lime glass, borosilicate glass, quartz glass and the like.
• the metal include iron, SUS, copper, nickel alloy, cobalt alloy, titanium alloy and the like.
• the container may be a bottle, a bag, or a resin bag such as polypropylene.
• the container may be made of one or more materials, and for example, a material in which a plurality of resins are laminated, a material in which a metal foil is laminated on resin or glass, or the like may be used.
• MFSI aqueous solution MFSI gradually decomposes to become a strong acid and tends to corrode metals. In addition, a small amount of hydrofluoric acid is also generated, which may erode the glass. Therefore, when storing for a long period of time, it is preferable to store in a resin container.
• the container contains two or more kinds of materials, it is preferable that the surface on the side in contact with the MFSI aqueous solution is made of resin.
• the MFSI aqueous solution of the present disclosure is excellent in storage stability, it can be stored as it is.
• the MFSI aqueous solution may be stored as the above-mentioned container containing the aqueous solution.
• the storage temperature is preferably ⁇ 20 ° C. to 60 ° C., more preferably ⁇ 10 ° C. to 45 ° C., and even more preferably 0 ° C. to 40 ° C.
• the MFSI aqueous solution may once solidify and then decompose when the solidified MFSI aqueous solution is remelted.
• the storage temperature is ⁇ 20 ° C. or higher, the decomposition of MFSI during remelting tends to be suppressed.
• the storage period of the MFSI aqueous solution may be at least 1 day, at least 3 days, or at least 1 week.
• the MFSI aqueous solution is preferably stored in a sealed container in order to avoid a decrease in water content during storage.
• the MFSI aqueous solution of the present disclosure is excellent in storage stability, it can be transported as it is.
• the MFSI aqueous solution may be transported as the above-mentioned container containing the aqueous solution.
• Examples of the transportation method include transportation by a transportation vehicle, and examples thereof include a method of transporting the vehicle on a loading platform of the transportation vehicle.
• the MFSI aqueous solution of the present disclosure may be used as it is as an aqueous solution, but water may be removed by heating, depressurizing, spray-drying, or a combination thereof to obtain MFSI powder.
• the MFSI may be extracted with an organic solvent to obtain an organic solvent solution of MFSI.
• the organic solvent is not particularly limited, but an ether solvent, a nitrile solvent, an ester solvent, a carbonate solvent and the like can be used.
• Amidosulfate ions, fluorine ions, sulfate ions, and ammonia or ammonium salts can be selectively separated and removed into the aqueous layer by an extraction operation in the form of salts or molecules.
• the MFSI extracted with an organic solvent can be isolated and purified by further concentration, crystallization, recrystallization and the like.
• the obtained MFSI powder or solution can be used as an additive to an electrolytic solution of a battery or a capacitor, a selective electrophoretic fluorinating agent, a photoacid generator, a thermoacid generator, a near-infrared absorbing dye, and the like. ..
• aqueous solution was obtained by dissolving 10.0 g of lithium bis (fluorosulfonyl) imide powder in 10.0 g of water. It was found that the pH of the aqueous solution obtained by the pH meter was 2.9. By ion chromatography, it was found that the aqueous solution contained 30 mass ppm of fluoride ion, 20 mass ppm of sulfate ion, and 25 mass ppm of amidosulfate ion.
• the obtained aqueous solution contained 6 mass ppm of fluoride ion, 28 mass ppm of sulfate ion, 1930 mass ppm of amidosulfate ion, and 6 mass ppm of ammonium ion. .. It was also found that the pH of the aqueous solution obtained from the pH test paper was 5.
• Example 1 The aqueous solution obtained in Production Example 1 was stored in a polypropylene container at 25 ° C. for 1 week. By 19 F NMR analysis, it was found that the aqueous solution after storage contained 49.9% by mass of LiFSI and 29% by mass of fluoride ions. In addition, ion chromatography revealed that sulfate ion was contained in an amount of 22 mass ppm and amidosulfate ion was contained in an amount of 25 mass ppm. The total amount of water and LiFSI in the aqueous solution after storage was 100.0% by mass.
• Example 2 The aqueous solution obtained in Production Example 2 was stored in a polypropylene container at 25 ° C. for 1 week, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 49.6% by mass and fluoride ions were contained in the aqueous solution. It was found that 40 mass ppm, 17 mass ppm of sulfate ion, and 22 mass ppm of amidosulfate ion were contained. The total amount of water and LiFSI in the aqueous solution after storage was 99.4% by mass.
• Example 3 The aqueous solution obtained in Production Example 3 was stored in a polypropylene container at 25 ° C. for 1 week, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 50.0% by mass and fluoride ions were contained in the aqueous solution. It was found that 39 mass ppm, sulfate ion was 3301 mass ppm, amidosulfate ion was 246 mass ppm, and ammonium ion was 1 mass ppm. The total amount of water and LiFSI in the aqueous solution after storage was 99.7% by mass.
• Example 4 The aqueous solution obtained in Production Example 4 was stored in a polypropylene container at 5 ° C. for 1 week, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 50.1% by mass and fluorosulfonic acid ion was contained in the aqueous solution. It was found that 64 mass ppm of fluoride ion, 6 mass ppm of fluoride ion, 21 mass ppm of sulfate ion, 1820 mass ppm of amidosulfate ion, and 7 mass ppm of ammonium ion were contained.
• Example 5 The aqueous solution obtained in Production Example 4 was stored in a polypropylene container at 25 ° C. for 1 week, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 50.1% by mass and fluorosulfonic acid ion was contained in the aqueous solution.
• LiFSI was 50.1% by mass and fluorosulfonic acid ion was contained in the aqueous solution.
• fluoride ion was 6 mass ppm
• sulfate ion was 27 mass ppm
• amidosulfate ion was 1839 mass ppm
• ammonium ion was 6 mass ppm.
• Example 6 The aqueous solution obtained in Production Example 4 was stored in a polypropylene container at 40 ° C. for 1 week, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 50.1% by mass and fluorosulfonate ion in the aqueous solution. It was found that 33 mass ppm of fluoride ion, 13 mass ppm of fluoride ion, 175 mass ppm of sulfate ion, 1950 mass ppm of amidosulfate ion, and 8 mass ppm of ammonium ion. The total amount of water and LiFSI in the aqueous solution after storage was 99.8% by mass.
• Example 7 The aqueous solution obtained in Production Example 6 was stored in a polypropylene container at 40 ° C. for 3 months and then analyzed in the same manner as in Example 1. As a result, LiFSI was 10.2% by mass and fluoride ions were contained in the aqueous solution. 8 mass ppm, sulfate ion 12 mass ppm, and amidosulfate ion 3 mass ppm. The total amount of water and LiFSI in the aqueous solution after storage was 100.0% by mass.
• Example 8 The aqueous solution obtained in Production Example 7 was stored in a polypropylene container at 40 ° C. for 3 months, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 30.8% by mass and fluoride ions were contained in the aqueous solution. Contained 17 mass ppm and sulfate ion 3 mass ppm. The total amount of water and LiFSI in the aqueous solution after storage was 100.0% by mass.
• Example 9 The aqueous solution obtained in Production Example 8 was stored in a polypropylene container at 40 ° C. for 1 month, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 40.8% by mass and fluoride ions were contained in the aqueous solution. Contained 25 mass ppm and sulfate ion 5 mass ppm. The total amount of water and LiFSI in the aqueous solution after storage was 100.0% by mass.
• Example 10 The aqueous solution obtained in Production Example 9 was stored in a polypropylene container at 25 ° C. for 2 weeks, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 71.1% by mass and fluoride ions were contained in the aqueous solution. It contained 53 mass ppm of sulfate ion, 52 mass ppm of sulfate ion, and 187 mass ppm of amidosulfate ion. The total amount of water and LiFSI in the aqueous solution after storage was 100.0% by mass.
• Example 11 The aqueous solution obtained in Production Example 10 was stored in a polypropylene container at 25 ° C. for 2 weeks, and then the same analysis as in Example 1 was performed. As a result, LiFSI was 80.8% by mass and fluoride ions were contained in the aqueous solution. It contained 130 mass ppm, 102 mass ppm of sulfate ion, and 375 mass ppm of amidosulfate ion. The total amount of water and LiFSI in the aqueous solution after storage was 99.9% by mass.
• Table 1 shows the storage conditions in Examples 1 to 11 and Comparative Examples, the concentration of each component before and after storage, and the like.

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• 2020
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