CN113247871B - Preparation method of lithium bis (fluorosulfonyl) imide - Google Patents
Preparation method of lithium bis (fluorosulfonyl) imide Download PDFInfo
- Publication number
- CN113247871B CN113247871B CN202110623551.3A CN202110623551A CN113247871B CN 113247871 B CN113247871 B CN 113247871B CN 202110623551 A CN202110623551 A CN 202110623551A CN 113247871 B CN113247871 B CN 113247871B
- Authority
- CN
- China
- Prior art keywords
- fluorosulfonyl
- imide
- bis
- lithium
- lithium bis
- 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
Links
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
-
- 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
-
- 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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
-
- 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
- C01P2006/40—Electric properties
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a preparation method of lithium bis (fluorosulfonyl) imide, which comprises the steps of dropwise adding bis (fluorosulfonyl) imide into anhydrous lithium halide under the condition of mixing and stirring with a non-polar solvent, and absorbing tail gas by using alkali liquor; after the dropwise addition is finished, continuously reacting at 0-60 ℃ for 1-12 hours, cooling to room temperature, dropwise adding an organic alkaline compound, and adjusting the pH of the reaction solution to 5-8; filtering, leaching the filter cake by adopting a nonpolar solvent to obtain a crude product of the lithium bis (fluorosulfonyl) imide. The invention has the advantages of mild reaction, simple process and low cost, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of preparation of electrolyte in lithium ion battery electrolyte, and particularly relates to a preparation method of lithium bis (fluorosulfonyl) imide.
Background
Lithium bis (fluorosulfonyl) imide (LiFSI) is an electrolyte lithium salt of a lithium ion battery, has the advantages of high and low temperature resistance, stable structure, difficult hydrolysis and the like, is superior to lithium hexafluorophosphate which is widely applied at present in application safety and stability, and is an ideal substitute product which is expected to replace lithium hexafluorophosphate as a main electrolyte lithium salt in the future. At present, the preparation technology of lithium bis (fluorosulfonyl) imide, which is publicly reported at home and abroad, mainly has two routes:
one is double decomposition reaction of potassium bifluoro sulfonyl imide salt and organic lithium salt of lithium tetrafluoroborate or lithium perchlorate in non-proton organic solvent to produce lithium bifluoro sulfonyl imide and potassium tetrafluoroborate or potassium perchlorate, filtering to separate, evaporating to concentrate and crystallizing to obtain the product. The defects are as follows: 1) the double decomposition reaction is difficult to complete, and the residual potassium ions in the product are high; 2) lithium tetrafluoroborate and lithium perchlorate which are used as reaction raw materials have higher solubility in a reaction organic solvent and are difficult to separate, and the obtained product often contains part of unreacted or excessive raw materials and has low purity; 3) the organic lithium salts such as lithium tetrafluoroborate or lithium perchlorate are high in price, which results in high manufacturing cost; lithium perchlorate is an explosive compound, brings certain safety risk and is not suitable for industrial production.
The other route is that the bifluoro-sulfonyl imide and basic lithium salt such as lithium hydroxide or lithium carbonate are subjected to acid-base neutralization reaction in a low-polarity organic solvent to generate the bifluoro-sulfonyl imide lithium and water. And then thionyl chloride is added to react with water to generate hydrogen chloride and sulfur dioxide gas so as to achieve the aim of removing water. Filtering, separating solid from liquid, and further purifying to obtain the final product. The main defects are as follows: 1) the bis-fluorosulfonyl imide is a strong proton acid, and reacts violently with alkali to generate a large amount of heat. The reaction process needs refrigeration and low-temperature control, and the energy consumption is high; 2) the reaction is essentially acid-base neutralization reaction, generates water with equal mole, adopts thionyl chloride to remove water, is difficult to completely react, has longer reaction time and more three wastes. Meanwhile, the dehydration reaction process easily causes partial hydrolysis of the product, so that the water in the product remains, chloride ions and sulfate ions exceed the standard, and a high-quality product is difficult to obtain.
Disclosure of Invention
In order to solve the problems of the preparation process of the lithium bis (fluorosulfonyl) imide in the prior art, the invention aims to provide the preparation method of the lithium bis (fluorosulfonyl) imide, which has the advantages of mild reaction, simple process and low cost and is suitable for industrial production.
In order to achieve the purpose and achieve the technical effect, the invention adopts the following process:
a preparation method of lithium bis (fluorosulfonyl) imide is characterized in that under the condition of mixing and stirring anhydrous lithium halide salt and a nonpolar solvent, bis (fluorosulfonyl) imide is dropwise added, and tail gas is absorbed by alkali liquor; after the dropwise addition is finished, continuously reacting at 0-60 ℃ for 1-12 hours, cooling to room temperature, dropwise adding an organic alkaline compound, and adjusting the pH of the reaction solution to 5-8; filtering, leaching the filter cake by adopting a nonpolar solvent to obtain a crude product of the lithium bis (fluorosulfonyl) imide.
Further, the preparation method of the lithium bis (fluorosulfonyl) imide further comprises the steps of dissolving a crude lithium bis (fluorosulfonyl) imide product in an aprotic polar organic solvent, filtering to remove insoluble substances, concentrating the filtrate under reduced pressure, and adding a poor solvent for crystallization; filtering, washing and drying to obtain the high-purity lithium bis (fluorosulfonyl) imide product, wherein the purity of the lithium bis (fluorosulfonyl) imide is more than or equal to 99.70%, the water content is less than or equal to 30ppm, the acidity (calculated by HF) is less than or equal to 50ppm, the free chlorine is less than or equal to 10ppm, and the content of impurity ions such as metal potassium, sodium and the like is less than or equal to 5 ppm.
Further, the anhydrous lithium halide salt is one of anhydrous lithium chloride, anhydrous lithium fluoride or anhydrous lithium bromide; from the economic and environmental protection points of view, anhydrous lithium chloride and anhydrous lithium fluoride are preferred; from the viewpoint of the progress of the reaction, anhydrous lithium chloride is more preferable.
Further, the molar ratio of the anhydrous lithium halide salt to the bis-fluorosulfonyl imide is (1-1.1) to 1; anhydrous lithium halide salt and difluoride sulfimide are used in equivalent amount or lithium salt is slightly excessive, so that the sufficient reaction of the difluoride sulfimide is ensured.
Further, the nonpolar solvent is halogenated alkane selected from one or more of dichloromethane, trichloromethane, carbon tetrachloride, dichloroethane, trichloroethane, tetrachloroethane, dichloropropane, trichloropropane and tetrachloropropane; preferably dichloromethane and dichloroethane which are relatively less toxic, and more preferably, when the nonpolar solvent is dichloromethane, the reaction temperature is controlled to be 60 ℃ at reflux temperature.
Further, the addition amount of the nonpolar solvent is 1-5 times of the mass times of the bis-fluorosulfonyl imide.
The organic alkaline compound is a nitrogen-containing organic weak base, and is selected from one or a combination of more than two of triethylamine, tripropylamine, n-propylamine, isopropylamine, dipropylamine, butylamine, isobutylamine, tert-butylamine, hexylamine, octylamine, aniline, cyclohexylamine, pyridine and piperidine.
Further, the water content of the aprotic polar organic solvent is less than 1000ppm, preferably less than 500ppm, more preferably less than 300ppm, the aprotic polar organic solvent is an ester compound, a ketone compound, a nitrile compound or an ether compound, and is selected from one or a mixture of two or more of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, propylene carbonate, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, acetone, methyl ethyl ketone, acetonitrile, propionitrile, diethyl ether, isopropyl ether, methyl tert-butyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, 1, 4-dioxane, tetrahydrofuran or 2-methyltetrahydrofuran.
Further, the addition amount of the aprotic polar organic solvent is 0.8-5 times of the mass multiple of the crude product of the lithium bis (fluorosulfonyl) imide; the addition amount of the aprotic polar organic solvent is preferably 1-3 times of the mass of the crude product of the bis (fluorosulfonyl) imide lithium in terms of energy consumption, smooth filtering operation and the like.
Further, the poor solvent is selected from one or more of benzene, toluene, xylene, chlorobenzene, hexane, cyclohexane, heptane, octane, dichloromethane, dichloroethane, trichloroethane, tetrachloroethane, and petroleum ether.
The principle of the invention is as follows: the method adopts the steps that the bis-fluorosulfonyl imide is fully reacted with lithium halide salt, and then a proper amount of organic alkaline compound is added for reaction assistance, so that high reaction conversion rate can be obtained, and free fluorine, chloride ions and other acidic impurities in a complex reaction system can be obtained. After the dropwise addition of the bis (fluorosulfonyl) imide, the reaction system is kept at 0-60 ℃ for reaction. The reaction temperature is too low, and the reaction is slow; the reaction temperature is higher than 60 ℃, and the generated product is easy to be partially decomposed in an acid system. When the nonpolar solvent is dichloromethane, the reaction temperature is controlled to be 60 ℃ of reflux temperature under the condition of heat preservation. After the heat preservation reaction is finished, in order to further accelerate the reaction process and the reaction conversion rate, an organic alkaline compound is dropwise added into the reaction system, and the pH value of the reaction solution is adjusted to 5-8. The organic alkaline compound can be used as an acid-binding agent to generate a complex with hydrogen chloride, hydrogen fluoride or hydrogen bromide generated by the reaction, and the complex neutralizes free acid in the reaction system to promote the forward progress of the reaction. Meanwhile, the organic alkaline compound and the complex have better solubility in the halogenated alkane nonpolar solvent provided by the technical scheme, and the product lithium bis (fluorosulfonyl) imide is almost insoluble in the solvent, so that a better separation effect can be achieved by simple filtration. The chemical reaction in the technical scheme is an anhydrous system, so that the hydrolysis problems of reaction raw materials and target products under the conditions of temperature rise and acidity are fundamentally avoided. The organic alkali complex has higher solubility in the nonpolar halogenated alkane solvent provided by the technical scheme, the target product lithium bifluorosulfonyl imide is almost insoluble, and the removal is more thorough through solid-liquid separation and leaching after the reaction is finished.
The invention has the beneficial effects that: the preparation method of the lithium bis (fluorosulfonyl) imide provided by the invention has the advantages of mild reaction conditions, easiness in operation, less three wastes generation, environmental friendliness, capability of simply and conveniently obtaining a high-purity lithium bis (fluorosulfonyl) imide product with high technical indexes, capability of controlling residual moisture, free acid, fluoride ions, chloride ions, other impurities and the like in the lithium bis (fluorosulfonyl) imide product at a lower level, and higher reaction conversion rate and yield.
Detailed Description
The present invention will be described in further detail with reference to specific examples, so that the advantages of the present invention will be more apparent. It should be understood that the description is intended for purposes of illustration only and is not intended to limit the scope of the present disclosure. The experimental procedures, in which specific conditions are not specified, in the following examples are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
Example 1
42g (1 mol) of anhydrous lithium chloride was charged into a dry three-necked flask with stirring and condensing reflux apparatus under nitrogen atmosphere, 360g of methylene chloride was then added thereto, and stirring was turned on. 181g (1 mol) of bis (fluorosulfonyl) imide is added into a dry constant-pressure dropping funnel under a nitrogen atmosphere, the mixture is dropped into a flask at room temperature, acid tail gas escapes in the dropping process, and tail gas of a condensation reflux pipe is connected to an alkali liquor absorption device. After 1 hour, the dropwise addition is finished, the temperature is raised to about 40 ℃ for reflux, the reaction is stopped after 1 hour of continuous reaction, and the temperature is reduced to room temperature. And (3) measuring the pH value of the reaction liquid to be 1, slowly dropwise adding triethylamine into the reaction liquid while stirring, continuously detecting the pH value of the reaction liquid in the process, stopping dropwise adding until the pH value is 6-7, and continuously stirring for about 10 minutes. And filtering under the protection of nitrogen, and leaching a filter cake twice by using dichloromethane to obtain 178g of a solid crude product.
The crude product was added to 180g of dimethyl carbonate containing 95ppm of water under nitrogen, and dissolved with stirring. Filtering with 0.1 μm PTFE filter membrane to room temperature, concentrating the filtrate at 50 deg.C under reduced pressure for 5 hr, adding toluene 250g, stirring, cooling, crystallizing for 12 hr, filtering, and drying the filter cake under reduced pressure to obtain 173g of lithium bis (fluorosulfonyl) imide product with yield of 92.5%.
The detection shows that the purity of the product is 99.85 percent, the water content is 12ppm, the acidity (calculated by HF) is 15ppm, the free chlorine is 1.23ppm, and the impurity ions such as metal potassium, sodium and the like are less than 3 ppm.
Example 2
To a dry three-necked flask with stirring and condensing reflux apparatus was added 28.6g (1.1 mol) of anhydrous lithium fluoride under nitrogen atmosphere, and then 181g of dichloroethane was added thereto, and the stirring was turned on. 181g (1 mol) of bis (fluorosulfonyl) imide is added into a dry constant-pressure dropping funnel under a nitrogen atmosphere, the mixture is dropped into a flask at room temperature, and tail gas of a condensation reflux pipe is connected to an alkali liquor absorption device. After 1 hour, the dropwise addition is finished, the temperature is raised to 55-60 ℃, the reaction is continued for 12 hours, and the temperature is stopped to be reduced to the room temperature. And (3) measuring the pH value of the reaction liquid to be 1, slowly dropwise adding dipropylamine into the reaction liquid while stirring, continuously detecting the pH value of the reaction liquid in the process, stopping dropwise adding until the pH value is 5-6, and continuously stirring for about 10 minutes. Filtering under the protection of nitrogen, and leaching the filter cake twice with dichloroethane to obtain 166g of a solid crude product.
Under nitrogen atmosphere, the crude product was added to a mixed solvent of 160g of diethyl ether and 160g of ethylene glycol diethyl ether, the water content of the mixed solvent was 126ppm, and the mixture was dissolved with stirring. Filtering with 0.1 μm PTFE filter membrane to room temperature, concentrating the filtrate at 60 deg.C under reduced pressure for 6 hr, adding 300g dichloroethane, stirring, cooling, crystallizing for 12 hr, filtering, and drying the filter cake under reduced pressure to obtain 158g of lithium bis (fluorosulfonyl) imide product with yield of 84.5%.
The detection shows that the purity of the product is 99.76%, the water content is 18ppm, the acidity (calculated by HF) is 21ppm, the free chlorine is 0.69ppm, and the impurity ions such as metal potassium, sodium and the like are less than 2 ppm.
Example 3
To a dry three-necked flask with stirring and condensing reflux apparatus, 46g (1.1 mol) of anhydrous lithium chloride was charged under nitrogen atmosphere, and 540g of dichloroethane was subsequently added thereto, and stirring was turned on. 181g (1 mol) of bis (fluorosulfonyl) imide is added into a dry constant-pressure dropping funnel under a nitrogen atmosphere, the mixture is dropped into a flask at room temperature, acid tail gas escapes in the dropping process, and tail gas of a condensation reflux pipe is connected to an alkali liquor absorption device. After 1 hour, the dropwise addition is finished, the reaction is carried out at the temperature of 0-8 ℃ for 12 hours, and the pH of the reaction solution is measured to be 1. Slowly dropwise adding pyridine into the reaction solution under stirring, continuously detecting the pH value of the reaction solution in the process, stopping dropwise adding until the pH value is 7-8, and continuously stirring for about 30 minutes. Filtering under the protection of nitrogen, and leaching the filter cake twice with dichloroethane to obtain 173g of a solid crude product.
The above crude product was added to 340g of acetonitrile containing 280ppm of acetonitrile in water under nitrogen atmosphere, and dissolved with stirring. And (3) filtering the solution to room temperature by using a 0.1-micron PTFE filter membrane, concentrating the filtrate at 45-50 ℃ under reduced pressure for 4 hours, adding 350g of heptane into the concentrated solution, stirring the solution, cooling the solution for crystallization for 12 hours, filtering the solution, and drying a filter cake under reduced pressure to obtain 171g of lithium bis (fluorosulfonyl) imide product with the yield of 91.4%.
The detection proves that the purity of the product is 99.92 percent, the water content is 28ppm, the acidity (calculated by HF) is 23ppm, the free chlorine is 0.72ppm, and the impurity ions such as metal potassium, sodium and the like are less than 3 ppm.
Comparative examples
The same materials weight, proportion and operation conditions as those in example 1, after the completion of the heat preservation reaction of the bis (fluorosulfonyl) imide, triethylamine was not added dropwise thereto, and the crude product (155 g) was obtained by direct filtration and elution.
The operation conditions of the purification steps are completely the same, and 131g of lithium bis (fluorosulfonyl) imide product is obtained after concentration, crystallization, filtration and drying, and the yield is 70%.
The detection shows that the product has the purity of 99.81 percent, the water content of 16ppm, the acidity (calculated by HF) of 56ppm, the free chlorine of 18ppm, and the impurity ions such as metal potassium, sodium and the like which are less than 5 ppm.
It will be appreciated that various alterations and modifications of the invention will occur to those skilled in the art upon reading the above teachings, and that such equivalents are intended to fall within the scope of the invention as defined by the appended claims.
Claims (5)
1. A preparation method of lithium bis (fluorosulfonyl) imide is characterized by comprising the following steps: dropwise adding difluoride sulfimide under the condition of mixing and stirring anhydrous lithium halide salt and a non-polar solvent, and absorbing tail gas by adopting alkali liquor; after the dropwise addition is finished, continuously reacting at 0-60 ℃ for 1-12 hours, cooling to room temperature, dropwise adding an organic alkaline compound, and adjusting the pH of the reaction solution to 5-8; filtering, leaching a filter cake by using a non-polar solvent to obtain a crude product of the lithium bis (fluorosulfonyl) imide; the molar ratio of the anhydrous lithium halide salt to the bis (fluorosulfonyl) imide is (1-1.1) to 1; the nonpolar solvent is halogenated alkane selected from one or more of dichloromethane, trichloromethane, carbon tetrachloride, dichloroethane, trichloroethane, tetrachloroethane, dichloropropane, trichloropropane and tetrachloropropane; the addition amount of the nonpolar solvent is 1-5 times of the mass multiple of the bis (fluorosulfonyl) imide; the organic alkaline compound is nitrogen-containing organic weak base selected from one or a combination of more than two of triethylamine, tripropylamine, n-propylamine, isopropylamine, dipropylamine, butylamine, isobutylamine, tert-butylamine, hexylamine, octylamine, aniline, cyclohexylamine, pyridine and piperidine.
2. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 1, wherein: the preparation method of the lithium bis (fluorosulfonyl) imide further comprises the steps of dissolving a crude lithium bis (fluorosulfonyl) imide product in an aprotic polar organic solvent, filtering to remove insoluble substances, concentrating the filtrate under reduced pressure, and adding a poor solvent for crystallization; and filtering, washing and drying to obtain the high-purity lithium bis (fluorosulfonyl) imide product.
3. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 1 or 2, wherein: the anhydrous lithium halide salt is one of anhydrous lithium chloride, anhydrous lithium fluoride or anhydrous lithium bromide.
4. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 2, wherein: the water content of the aprotic polar organic solvent is less than 1000ppm, the aprotic polar organic solvent is an ester compound, a ketone compound, a nitrile compound or an ether compound, and is selected from one or a mixture of more than two of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, propylene carbonate, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, acetone, methyl ethyl ketone, butanone, acetonitrile, propionitrile, diethyl ether, isopropyl ether, methyl tert-butyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, 1, 4-dioxane, tetrahydrofuran or 2-methyltetrahydrofuran; the addition amount of the aprotic polar organic solvent is 0.8-5 times of the mass multiple of the crude product of the bis (fluorosulfonyl) imide.
5. The method for preparing lithium bis (fluorosulfonyl) imide according to claim 2, wherein: the poor solvent is one or more selected from benzene, toluene, xylene, chlorobenzene, hexane, cyclohexane, heptane, octane, dichloromethane, dichloroethane, trichloroethane, tetrachloroethane or petroleum ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110623551.3A CN113247871B (en) | 2021-06-04 | 2021-06-04 | Preparation method of lithium bis (fluorosulfonyl) imide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110623551.3A CN113247871B (en) | 2021-06-04 | 2021-06-04 | Preparation method of lithium bis (fluorosulfonyl) imide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113247871A CN113247871A (en) | 2021-08-13 |
| CN113247871B true CN113247871B (en) | 2021-09-24 |
Family
ID=77186434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110623551.3A Active CN113247871B (en) | 2021-06-04 | 2021-06-04 | Preparation method of lithium bis (fluorosulfonyl) imide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113247871B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603069A (en) * | 2021-10-08 | 2021-11-05 | 江苏华盛锂电材料股份有限公司 | Method for removing trace impurities in lithium bis (fluorosulfonyl) imide |
| CN114368733A (en) * | 2022-01-29 | 2022-04-19 | 宁德时代新能源科技股份有限公司 | Lithium bis (fluorosulfonyl) imide, preparation method thereof, electrolyte and secondary battery |
| CN114560452B (en) * | 2022-03-29 | 2023-06-23 | 多氟多新材料股份有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| CN114655939B (en) * | 2022-04-13 | 2023-09-08 | 多氟多新材料股份有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| CN115535995A (en) * | 2022-11-03 | 2022-12-30 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium difluorophosphate |
| CN116462165A (en) * | 2023-04-28 | 2023-07-21 | 湖北兴发化工集团股份有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524387A (en) * | 2013-10-25 | 2014-01-22 | 中国海洋石油总公司 | Preparation method of imidodisulfuryl fluoride lithium salt |
| CN104477861A (en) * | 2014-11-24 | 2015-04-01 | 中国船舶重工集团公司第七一八研究所 | Preparation method of difluoro-sulfonyl imine salt |
| CN106276829A (en) * | 2016-08-23 | 2017-01-04 | 荣成青木高新材料股份有限公司 | A kind of synthetic method of pair of fluorine sulfimide lithium |
| CN108946686A (en) * | 2018-07-31 | 2018-12-07 | 九江天赐高新材料有限公司 | A kind of preparation method of double fluorine sulfimide lithiums |
| CN110668411A (en) * | 2019-11-18 | 2020-01-10 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium bis (fluorosulfonyl) imide |
-
2021
- 2021-06-04 CN CN202110623551.3A patent/CN113247871B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524387A (en) * | 2013-10-25 | 2014-01-22 | 中国海洋石油总公司 | Preparation method of imidodisulfuryl fluoride lithium salt |
| CN104477861A (en) * | 2014-11-24 | 2015-04-01 | 中国船舶重工集团公司第七一八研究所 | Preparation method of difluoro-sulfonyl imine salt |
| CN106276829A (en) * | 2016-08-23 | 2017-01-04 | 荣成青木高新材料股份有限公司 | A kind of synthetic method of pair of fluorine sulfimide lithium |
| CN108946686A (en) * | 2018-07-31 | 2018-12-07 | 九江天赐高新材料有限公司 | A kind of preparation method of double fluorine sulfimide lithiums |
| CN110668411A (en) * | 2019-11-18 | 2020-01-10 | 江苏华盛锂电材料股份有限公司 | Purification method of lithium bis (fluorosulfonyl) imide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113247871A (en) | 2021-08-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113247871B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN109941982B (en) | Purification method of lithium difluorophosphate | |
| CN108368132B (en) | Novel method for producing lithium bis (fluorosulfonyl) imide | |
| CN111498819B (en) | Preparation of imides containing fluorosulfonyl groups | |
| CN109941978B (en) | Method for preparing ammonium bifluorosulfonamide and alkali metal salt of bifluorosulfonamide | |
| WO2018201711A1 (en) | Method for preparing lithium bis (fluorosulfonyl) imide | |
| CN108373142B (en) | Preparation method of high-purity lithium bis (fluorosulfonyl) imide | |
| CN106276829B (en) | A kind of synthetic method of double fluorine sulfimide lithiums | |
| CN104495767A (en) | Preparation method of lithium bis(fluorosulfonyl)amide | |
| CN101959874B (en) | Method for producing fluorinated 1,3-dioxolan-2-one | |
| CN113800485B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| US20240297345A1 (en) | Preparation of lithium bis(fluorosulfonyl)imide, and application thereof | |
| CN101723346B (en) | Preparation method of lithium hexafluorophosphate | |
| CN107416782A (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| CN112174101A (en) | Preparation method of high-purity lithium bis (fluorosulfonyl) imide | |
| KR20200049164A (en) | Very efficient Method for preparing lithium bis(fluorosulfonyl)imide | |
| CN112300111A (en) | Method for treating fluoroethylene carbonate solid slag | |
| CN115285965B (en) | Synthesis method of sodium hexafluorophosphate | |
| CN110921640A (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN114014280B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN113929711A (en) | Preparation method of lithium difluoroborate | |
| CN115676855B (en) | Preparation method of sodium ion battery electrolyte sodium salt | |
| CN110540176B (en) | Method for improving purity of lithium bis (fluorosulfonyl) imide | |
| CN116750733A (en) | Method for preparing lithium bis (fluorosulfonyl) imide by utilizing sulfuryl fluoride | |
| CN114890402B (en) | Preparation method of hexafluorophosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |