CN111533094A - Method for simply preparing high-purity lithium bis (fluorosulfonyl) imide - Google Patents
Method for simply preparing high-purity lithium bis (fluorosulfonyl) imide Download PDFInfo
- Publication number
- CN111533094A CN111533094A CN202010338462.XA CN202010338462A CN111533094A CN 111533094 A CN111533094 A CN 111533094A CN 202010338462 A CN202010338462 A CN 202010338462A CN 111533094 A CN111533094 A CN 111533094A
- 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.)
- Pending
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
- C01P2006/80—Compositional purity
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
-
- 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)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a method for simply preparing high-purity lithium bis (fluorosulfonyl) imide, which comprises the following steps: s1, slowly dropping the difluoride sulfimide into a special lithium salt dissolved in a low-polarity organic solvent at a low temperature under the protection of inert gas to perform an exchange reaction to generate difluoride sulfimide lithium and gas HX, S2, filtering the product, adding a poor solvent to wash for multiple times, and performing vacuum drying to obtain the high-purity difluoride sulfimide lithium. The method is simple to operate, does not produce byproducts which need filtration or distillation, and does not need complicated processes of water removal and impurity removal, and can directly obtain the high-purity lithium bis (fluorosulfonyl) imide.
Description
Technical Field
The invention belongs to the technical field of lithium battery electrolytes in fluorine chemical industry, and particularly relates to a method for simply preparing high-purity lithium bis (fluorosulfonyl) imide.
Background
The research of lithium ion batteries has been rapidly developed in the last decades of the increasing shortage of energy. The most used at present is lithium hexafluorophosphate (LiPF)6) And lithium bistrifluoromethanesulfonylimide (LiTFSI), but both of them are poor in thermal stability and chemical stability, so that lithium bistrifluoromethanesulfonylimide (LiFSI) is produced at the same time, and has high thermal stability, does not decompose at 200 ℃ or below, and also has good chemical stability. Therefore, LiFSI is the newest and hottest direction for lithium battery electrolyte research.
In the prior art, the following reports mainly exist for the preparation of lithium bis (fluorosulfonyl) imide:
chinese patent (CN 105523970A) also reports that bis (fluorosulfonyl) imide metal salt with purity more than or equal to 99.9% is used as a raw material to react with lithium tetrafluoroborate or lithium perchlorate, and then the high-purity bis (fluorosulfonyl) imide lithium is obtained through purification and crystallization. But firstly, the cost of lithium tetrafluoroborate and lithium perchlorate is high, secondly, the lithium perchlorate is dangerous, so that the safety of the reaction can not be ensured, and most importantly, because the lithium tetrafluoroborate and the lithium perchlorate have very high solubility in a solvent, the residual lithium tetrafluoroborate and the lithium perchlorate in the bis (fluorosulfonyl) imide lithium are difficult to separate, so that metal ions except lithium are easy to exceed the standard, and the purification is difficult.
Aiming at the preparation of lithium bis (fluorosulfonyl) imide, it is reported at home and abroad that lithium bis (fluorosulfonyl) imide (CN 201510261089, CN 201610288440, CN103664712A, EP 2415757, EP 2439173, US 20120020867) is obtained mainly by reacting the lithium bis (fluorosulfonyl) imide with alkaline lithium salt at low temperature. The method has harsh operating conditions, and the acid-base neutralization can release heat violently, so the reaction needs to be carried out at low temperature, even at-78 ℃, and the operation has potential safety hazards and is more energy-consuming.
Chinese patent (CN 106241757A) reports that bis (fluorosulfonyl) imide and LiX are subjected to a displacement reaction, wherein X is selected from Cl, Br or I, the reaction is firstly carried out in the presence of an organic solvent, and then a poor solvent is added for treatment, which seems to be simple, but LiX has low reaction activity, long reaction time and incomplete reaction, Cl ions, Br ions or I ions in the bis (fluorosulfonyl) imide obtained after the reaction are extremely easy to exceed the standard and are difficult to remove, so that the obtaining of high-purity bis (fluorosulfonyl) imide lithium is difficult.
Chinese patent (CN 107055493 a) mainly discloses a method of obtaining lithium bis (fluorosulfonyl) imide and carboxylic acid by reacting lithium bis (fluorosulfonyl) imide with lithium carboxylate in the corresponding carboxylic acid, wherein first lithium bis (fluorosulfonyl) imide will dissolve in carboxylic acid and cannot be separated by filtration; secondly, if the solvent is removed by distillation under reduced pressure, the boiling point of the carboxylic acid is high due to the presence of hydrogen bonds, so that the removal of the solvent requires much energy, and thus industrialization is difficult to achieve.
Chinese patent (CN 107416782 a) reports that bis (fluorosulfonyl) imide reacts with RLi in the absence of solvent or in the presence of solvent to produce lithium bis (fluorosulfonyl) imide and an organic HR, so that after the reaction is finished, the reaction solvent needs to be treated, and the organic byproduct HR produced by the reaction needs to be treated.
Disclosure of Invention
Aiming at the defects, the method selects the exchange reaction of the difluoride sulfimide and the special lithium salt in the organic solvent at low temperature, only produces the difluoride sulfimide lithium and gas HX, does not have byproducts which need filtration or distillation, and does not need to undergo the complicated processes of water removal and impurity removal, and can directly obtain the high-purity difluoride sulfimide lithium. The method has the advantages of simple reaction operation, simple post-treatment, less side reaction, high yield, high product purity, good quality, simple process and easy realization of industrial preparation.
Aiming at the defects in the prior art, the invention discovers a new process after intensive research, and adopts the top-speed scheme as follows:
s1 dropping the bis-fluorosulfonylimide slowly into special lithium salt dissolved in low-polarity organic solvent under inert gas protection at low temperature for exchange reaction to generate lithium bis-fluorosulfonylimide and gas HX (X = C)nH2n，CnHnN is 0. ltoreq.n.ltoreq.4, and when n =0, X = H).
And S2, filtering the crude product of the lithium bis (fluorosulfonyl) imide, adding a poor solvent, washing for multiple times, and performing vacuum drying to obtain the high-purity lithium bis (fluorosulfonyl) imide.
According to the technical scheme, by-products do not need to be filtered or distilled, and complicated processes of water removal and impurity removal are not needed, so that the high-purity lithium bis (fluorosulfonyl) imide can be directly obtained.
On one hand, the reaction product of the special lithium salt and the difluoride sulfimide selected by the invention only comprises the difluoride sulfimide lithium and gas HX, and in the reaction, a reaction by-product HX can leave a reaction system, so that the forward reaction can be promoted, and on the other hand, impurities and ions can not be left in the reaction system, so that after the reaction is finished, the complicated processes of water removal and impurity removal are not needed, and the high-purity difluoride sulfimide lithium can be directly obtained.
On the other hand, the solvent selected for the reaction is a low-polarity organic solvent, and the lithium bis (fluorosulfonyl) imide generated by the reaction can be directly precipitated in a form of precipitation, so that possible impurity ions can be left in the solvent to a certain extent, recrystallization is not needed after solid is obtained, after the reaction is finished, only a poor solvent is needed to be used for washing for several times, solid-liquid separation is directly carried out, and then vacuum pumping is carried out to obtain the high-purity lithium bis (fluorosulfonyl) imide.
The method has the advantages of simple reaction operation, simple post-treatment, less side reaction, high yield, high product purity, good quality, simple process and easy realization of industrial preparation.
Preferred specific lithium salts are selected from one or a combination of more of methyllithium, ethyllithium, propyllithium, butyllithium, ethynyllithium, propynyllithium, butynthium, lithium carbide, lithium hydride.
Comprises the following steps;
s1, slowly dropping the bis (fluorosulfonyl) imide into a special lithium salt dissolved in a low-polarity organic solvent at a low temperature under the protection of inert gas to perform an exchange reaction to generate a crude bis (fluorosulfonyl) imide lithium and a gas HX (X = CnH2n, CnHn, n is more than or equal to 0 and less than or equal to 4, and when n =0, X = H);
and S2, filtering the crude product of the lithium bis (fluorosulfonyl) imide, adding a poor solvent, washing for multiple times, and performing vacuum drying to obtain the high-purity lithium bis (fluorosulfonyl) imide.
Preferably, the inert gas in S1 is preferably nitrogen.
Preferably, the molar ratio of the bis-fluorosulfonyl imide used in the reaction in the step S1 to the special lithium salt is 1:1 to 5: 1.
Preferably, the low-polarity organic solvent in step S1 and the poor solvent in step S2 are both one or more selected from saturated hydrocarbons, halogenated hydrocarbons, and aromatic hydrocarbons.
Preferably, the saturated hydrocarbon is one or more of n-hexane, cyclohexane and petroleum ether, the halogenated hydrocarbon is one or more of dichloromethane, 1, 2-dichloroethane, chloroform and carbon tetrachloride, and the aromatic hydrocarbon is one or more of benzene and toluene.
Preferably, in the step S1, the molar ratio of the low-polar organic solvent to the reactant is 1:1 to 5: 1.
Preferably, the molar ratio of the poor solvent to the reactant in the step S2 is 1:1 to 5: 1.
Preferably, the low temperature required by the reaction in the step S1 is-78-0 ℃, preferably-78-20 ℃, and the time required by the reaction is 0.5-5 hours, preferably 1-3 hours.
Preferably, the vacuum degree of the vacuum pumping in the step S2 is 3 to 10 torr, preferably 4 to 8 torr, the temperature is 0 to 50 ℃, and the temperature is preferably 20 to 40 ℃.
The invention has the following advantages:
1. the special lithium salt selected by the reaction and the bis-fluorosulfonyl imide react quickly and thoroughly, so that the reaction time is greatly shortened, the atom utilization rate is improved, and the environment friendliness is better realized;
2. the reaction of the special lithium salt selected by the reaction and the bis-fluorosulfonyl imide does not produce a byproduct which is difficult to remove, only produces gas, and is easy to separate from the system, so that the post-treatment is simple and does not need to go through complicated processes of water removal and impurity removal;
3. the solvent selected in the reaction is a low-polarity organic solvent, on one hand, the selection range is wide, on the other hand, the solid of the bis-fluorosulfonyl imide lithium can be directly obtained, the solid-liquid separation is directly carried out, and then the high-purity bis-fluorosulfonyl imide lithium can be obtained by vacuum drying.
Therefore, the invention provides the high-purity lithium bis (fluorosulfonyl) imide which can be prepared efficiently with high quality and low cost, and is suitable for industrial production.
Detailed Description
The following examples are intended to illustrate several specific embodiments of the present invention, but do not limit the invention to these specific embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Example 1
Adding 1mol/L methyl lithium toluene solution (100 mL) into a 250 mL reaction bottle under the protection of nitrogen, slowly dropwise adding toluene solution (50 mL) of bis (fluorosulfonyl) imide (18.1 g) at-40 ℃, after dropwise adding, naturally heating to room temperature, stirring for 1 h at room temperature, filtering under nitrogen protection, washing solid with dry toluene (15 mL x 3) for three times, and vacuum drying under the vacuum degree of 5torr to obtain white high-purity lithium bis (fluorosulfonyl) imide (18.5 g), wherein the yield is 98.9%, and the content is not less than 99.9%. (detection result: Na)+（≤1ppm）、K+（≤1ppm）、Cl-（≤5ppm）、F-（≤1ppm），H2O（≤20ppm），19F NMR（400MHz，D2O）：51.9ppm）。
Example 2
Adding 1mol/L ethyl lithium n-hexane solution (100 mL) into a 250 mL reaction bottle under the protection of nitrogen, slowly dropwise adding the n-hexane solution (50 mL) of bis (fluorosulfonyl) imide (18.3 g) in an environment of-50 ℃, naturally heating to room temperature after dropwise adding, stirring for 1 h at room temperature, filtering under the protection of nitrogen, washing the solid with dry n-hexane (10 mL × 3) for three times, and drying in vacuum under the condition of a vacuum degree of 4 torr to obtain white high-purity lithium bis (fluorosulfonyl) imide (18.3 g), wherein the yield is 97.6%, and the content is not less than 99.9%. (detection result: Na)+（≤1ppm）、K+（≤1ppm）、Cl-（≤5ppm）、F-（≤1ppm），H2O（≤20ppm），19F NMR（400MHz，D2O）：51.9ppm）。
Example 3
Adding 1mol/L propyllithium cyclohexane (100 mL) into a 250 mL reaction bottle under the protection of nitrogen, slowly dropwise adding a cyclohexane solution (50 mL) of bis (fluorosulfonyl) imide (18.2 g) at-78 ℃, naturally raising the temperature to room temperature after the dropwise adding is finished, stirring for 0.5 h at room temperature, filtering under the protection of nitrogen, washing the solid with dry cyclohexane (12 mL x 3) for three times, and performing vacuum drying under the condition of a vacuum degree of 5torr to obtain white high-purity lithium bis (fluorosulfonyl) imide (18 g), wherein the yield is 96.3%, and the content is not less than 99.9%. (detection result: Na)+（≤1ppm）、K+（≤1ppm）、Cl-（≤5ppm）、F-（≤1ppm），H2O（≤20ppm），19F NMR（400MHz，D2O）：51.9ppm）。
Example 4
Adding lithium hydride (1.2 g) into a 250 mL reaction bottle under the protection of nitrogen, adding cyclohexane (80 mL), slowly dropwise adding a cyclohexane solution (80 mL) of bis (fluorosulfonyl) imide (27.5 g) at 0 ℃, naturally raising the temperature to room temperature after dropwise adding, stirring for 1 h at room temperature, filtering under nitrogen protection, washing the solid with dried dichloromethane (15 mL x 3) for three times, and drying in vacuum under the vacuum degree of 6 torr to obtain white high-purity bis (fluorosulfonyl) imideLithium (27.9 g), yield 99.5%, content ≥ 99.9%. (detection result: Na)+（≤1ppm）、K+（≤1ppm）、Cl-（≤5ppm）、F-（≤1ppm），H2O（≤20ppm），19F NMR（400MHz，D2O）：51.9ppm）。
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for simply preparing high-purity lithium bis (fluorosulfonyl) imide is characterized by comprising the following steps;
s1, slowly dropping the bis (fluorosulfonyl) imide into a special lithium salt dissolved in a low-polarity organic solvent at a low temperature under the protection of inert gas to perform an exchange reaction to generate a crude bis (fluorosulfonyl) imide lithium and a gas HX (X = CnH2n, CnHn, n is more than or equal to 0 and less than or equal to 4, and when n =0, X = H);
and S2, filtering the crude product of the lithium bis (fluorosulfonyl) imide, adding a poor solvent, washing for multiple times, and performing vacuum drying to obtain the high-purity lithium bis (fluorosulfonyl) imide.
2. The method for simply preparing the high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein the specific lithium salt in S1 is selected from one or more of methyllithium, ethyllithium, propyllithium, butyllithium, ethynlithium, propynlithium, butynlithium, lithium carbide, lithium, and lithium hydride.
3. The method for simply preparing the high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein said inert gas in S1 is preferably nitrogen.
4. The method for simply preparing high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein the molar ratio of the bis (fluorosulfonyl) imide used in the reaction in step S1 to the specific lithium salt is 1: 1-5: 1.
5. The method for simply preparing high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein said low-polarity organic solvent in step S1 and said poor solvent in step S2 are selected from one or more of saturated hydrocarbons, halogenated hydrocarbons, and aromatic hydrocarbons.
6. The method for simply preparing the high-purity lithium bis (fluorosulfonyl) imide according to claim 5, wherein said saturated hydrocarbon is preferably one or more of n-hexane, cyclohexane and petroleum ether, said halogenated hydrocarbon is preferably one or more of dichloromethane, 1, 2-dichloroethane, chloroform and carbon tetrachloride, and said aromatic hydrocarbon is preferably one or more of benzene and toluene.
7. The method for simply preparing high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein the molar ratio of the low-polar organic solvent to the reactant in step S1 is 1:1 to 5: 1.
8. The method for simply preparing high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein the molar ratio of the poor solvent to the reactant in step S2 is 1:1 to 5: 1.
9. The method for simply preparing high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein the low temperature required for the reaction in step S1 is-78 to 0 ℃, and the time required for the reaction is 0.5 to 5 hours.
10. The method for simply preparing high-purity lithium bis (fluorosulfonyl) imide according to claim 1, wherein the vacuum degree of vacuum pumping in step S2 is 3-10 torr, and the temperature is 0-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010338462.XA CN111533094A (en) | 2020-04-26 | 2020-04-26 | Method for simply preparing high-purity lithium bis (fluorosulfonyl) imide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010338462.XA CN111533094A (en) | 2020-04-26 | 2020-04-26 | Method for simply preparing high-purity lithium bis (fluorosulfonyl) imide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111533094A true CN111533094A (en) | 2020-08-14 |
Family
ID=71975412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010338462.XA Pending CN111533094A (en) | 2020-04-26 | 2020-04-26 | Method for simply preparing high-purity lithium bis (fluorosulfonyl) imide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111533094A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022053002A1 (en) * | 2020-09-10 | 2022-03-17 | Solvay Sa | Purification of bis (fluorosulfonyl) imide salt |
| CN114655939A (en) * | 2022-04-13 | 2022-06-24 | 多氟多新材料股份有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| WO2023102417A1 (en) * | 2021-12-02 | 2023-06-08 | Honeywell International Inc. | Processes for producing lithium bis(fluorosulfonyl) imide |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044728A (en) * | 2016-05-27 | 2016-10-26 | 上海康鹏科技有限公司 | Preparation method of imidodisulfuryl fluoride lithium salt |
| CN106365132A (en) * | 2016-08-31 | 2017-02-01 | 中国船舶重工集团公司第七八研究所 | Preparation method of difluoro-sulfimide and lithium difluoro-sulfimide |
| CN108503670A (en) * | 2018-04-11 | 2018-09-07 | 惠州市大道新材料科技有限公司 | A kind of preparation method of fluorine phosphorimide and its alkali metal salt |
| CN109311669A (en) * | 2016-05-26 | 2019-02-05 | 森田化学工业株式会社 | The manufacturing method of double fluorine sulfimide alkali metal salts and double fluorine sulfimide alkali metal salt compositions |
| WO2019188200A1 (en) * | 2018-03-27 | 2019-10-03 | ダイキン工業株式会社 | Production method for lithium sulfamate, and novel lithium sulfamate |
| CN110980669A (en) * | 2019-11-29 | 2020-04-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Preparation method of bis (fluorosulfonyl) imide alkali metal salt |
-
2020
- 2020-04-26 CN CN202010338462.XA patent/CN111533094A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109311669A (en) * | 2016-05-26 | 2019-02-05 | 森田化学工业株式会社 | The manufacturing method of double fluorine sulfimide alkali metal salts and double fluorine sulfimide alkali metal salt compositions |
| CN106044728A (en) * | 2016-05-27 | 2016-10-26 | 上海康鹏科技有限公司 | Preparation method of imidodisulfuryl fluoride lithium salt |
| CN106365132A (en) * | 2016-08-31 | 2017-02-01 | 中国船舶重工集团公司第七八研究所 | Preparation method of difluoro-sulfimide and lithium difluoro-sulfimide |
| WO2019188200A1 (en) * | 2018-03-27 | 2019-10-03 | ダイキン工業株式会社 | Production method for lithium sulfamate, and novel lithium sulfamate |
| CN108503670A (en) * | 2018-04-11 | 2018-09-07 | 惠州市大道新材料科技有限公司 | A kind of preparation method of fluorine phosphorimide and its alkali metal salt |
| CN110980669A (en) * | 2019-11-29 | 2020-04-10 | 中船重工（邯郸）派瑞特种气体有限公司 | Preparation method of bis (fluorosulfonyl) imide alkali metal salt |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022053002A1 (en) * | 2020-09-10 | 2022-03-17 | Solvay Sa | Purification of bis (fluorosulfonyl) imide salt |
| WO2023102417A1 (en) * | 2021-12-02 | 2023-06-08 | Honeywell International Inc. | Processes for producing lithium bis(fluorosulfonyl) imide |
| CN114655939A (en) * | 2022-04-13 | 2022-06-24 | 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111533094A (en) | Method for simply preparing high-purity lithium bis (fluorosulfonyl) imide | |
| CN109941978B (en) | Method for preparing ammonium bifluorosulfonamide and alkali metal salt of bifluorosulfonamide | |
| CN108373142B (en) | Preparation method of high-purity lithium bis (fluorosulfonyl) imide | |
| CN113800485B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN110105393B (en) | Process method for synthesizing lithium difluorooxalate phosphate | |
| WO2020024430A1 (en) | Preparation method for hydrogen bis(fluorosulfonyl)imide and lithium salt thereof | |
| CN111224164B (en) | Preparation method of lithium difluorophosphate | |
| CN108275666B (en) | Preparation method of bis (fluorosulfonyl) imide alkali metal salt | |
| CN102180457A (en) | Process for preparing lithium hexafluorophosphate by organic solvent method | |
| CN112320772A (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN114031056A (en) | Method for preparing phosphorus pentafluoride by polymerizing phosphate | |
| CN110684042A (en) | Preparation method of lithium bis (oxalato) borate | |
| CN113912028B (en) | Method for purifying difluoro sulfimide | |
| CN115893337A (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN113929711A (en) | Preparation method of lithium difluoroborate | |
| CN108912156B (en) | Preparation method of lithium bis (oxalato) borate | |
| CN116143088A (en) | Preparation method of difluoro-sulfonyl imide and difluoro-sulfonyl imide lithium | |
| CN115259112A (en) | Production method of bis-fluorosulfonyl imide and lithium salt thereof | |
| CN108190858B (en) | Preparation method of graphite fluoride | |
| CN112645294B (en) | Preparation method of high-purity lithium bis (fluorosulfonyl) imide | |
| CN110589776B (en) | Method for synthesizing magnesium sulfide by mechanical ball milling | |
| CN114560452B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN116282084A (en) | Method for preparing sodium hexafluorophosphate in perhalogen organic compound | |
| CN115819358A (en) | Method for continuously synthesizing 3-methyl-1-phenyl-1, 2, 4-triazole-5-ketone metal salt | |
| CN117326930A (en) | Process for producing pyromellitic acid |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200814 |
|
| RJ01 | Rejection of invention patent application after publication |