CN107416782A - A kind of preparation method of imidodisulfuryl fluoride lithium salt - Google Patents
A kind of preparation method of imidodisulfuryl fluoride lithium salt Download PDFInfo
- Publication number
- CN107416782A CN107416782A CN201710680013.1A CN201710680013A CN107416782A CN 107416782 A CN107416782 A CN 107416782A CN 201710680013 A CN201710680013 A CN 201710680013A CN 107416782 A CN107416782 A CN 107416782A
- Authority
- CN
- China
- Prior art keywords
- lithium salt
- preparation
- organic
- solvent
- imidodisulfuryl fluoride
- 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
-
- 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
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
-
- 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)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation method of imidodisulfuryl fluoride lithium salt, it is characterized in that, comprise the following steps：S01：Double fluorine sulfimides and organic lithium salt LiR are swapped into reaction in solvent-free or organic solvent; produce double fluorine sulphonyl imonium lithium salts and organic matter HR; the PKa of the organic matter HR is 0 ~ 50, and the exchange reaction is carried out under the conditions of gas shield, and reaction temperature is 0~60 DEG C；S02：Reactant under condition of no solvent in S01 is added into bad reagent crystallization, separation of solid and liquid produces imidodisulfuryl fluoride lithium salt；S03：By the reactant separation of solid and liquid in S01 under the conditions of organic solvent, liquid phase is concentrated, adds bad reagent crystallization, separation of solid and liquid produces imidodisulfuryl fluoride lithium salt.Preparation method provided by the invention has the characteristics of step is simple, high income, purity are high, stability is good and impurity content is low.
Description
Technical field
The present invention relates to a kind of preparation method of imidodisulfuryl fluoride lithium salt, belong to chemosynthesis technical field.
Background technology
Double fluorine sulfimide lithium abbreviation LiFSI, be one can be with wide variety of lithium salt electrolyte material, it is in electrolyte
In the electrochemical stability that has and heat-staple speciality, will not produce the corrosive gas such as hydrofluoric acid using process, can improve
The high/low temperature resistance of electrode interface SEI layers at low temperature, lithium battery capacitance loss in placement process is reduced, so as to improve battery
Performance.Patent US7709175 is directed to LiFSI electrical speciality research, it is found that its characteristic is much better than current commercialized hexafluoro phosphorus
Sour lithium (LiPF6), LiBF4 (LiBF4) and bis trifluoromethyl sulfimide lithium (LiTFSI), therefore industry is combined to
Double fluorine sulfimide lithiums of high-purity will have greatest help for lifting lithium battery technique.
Patent US2013331609, US2012041233 is first prepared among double fluorine sulfimide salts of metal or organic base
Body, then carry out cation exchange reaction with LiOH or Li2CO3 and double fluorine sulfonamides are made, the disadvantage is that, exchange reaction reaches one
It is difficult to continue after individual balance, conversion ratio is relatively low；And (M refers to metal cation to the intermediate MSFI that unreacted is complete, organic base
Cation is similar to LiFSI properties, it is difficult to be kept completely separate, causes LiFSI qualities not high, can not directly apply to battery electrolysis
Matter.
Ion is carried out in a solvent using sylvite (KFSI) and lithium perchlorate (LiClO4) or LiBF4 (LiBF4)
Exchange reaction obtains double fluorine sulfimides, and it is exceeded that this reaction is easily caused potassium ion in product, and LiClO4 and reaction produce
Potassium hyperchlorate (KClO4), be explosive compound；And LiBF4 has very big solubility in a solvent, therefore
Product is caused not to be easily purified.
CN103910346 then proposes with sylvite (KFSI) to enter with indissoluble lithium salts such as di-oxalate lithium borate and difluoro lithium borate
Row metathesis exchange reaction, although improving the problem of above-mentioned, still have the presence that KFSI residuals cause potassium ion.
United States Patent (USP) US2004097757 is directly reacted using HClSI with LiF prepares LiFSI, and salt exchanges and halogen exchange
Reaction is carried out simultaneously, although avoiding the residual of potassium ion, course of reaction can discharge a large amount of cyanogen fluoric acids, and the more matter of accessory substance
Measure purity difference.
Patent CN106241757A is then added dropwise to the dimethyl carbonate solution reaction containing LiCl using HFSI and prepares LiFSI,
Course of reaction can discharge a large amount of hydrochloric acid and slowly, also easily cause Chloride residue.
Patent CN103391896A reports utilize the butyl acetate solution of double fluorine sulfimide ammoniums (HFSI), with lithium hydroxide
Reactant aqueous solution obtains LiFSI butyl acetate solution.By concentration, LiFSI is obtained after filtration drying.The side of the patent report
The problem of method is present is that product purity and yield are too low, and consumption of raw materials and discarded object produce too much, and manufacturing cost is too high.
From above-mentioned LiFSI analysis of Production Technology, using MSFI with lithium salts exchange reaction mode is inevasible has friendship
The problem of reaching balance is changed, causes difficulty and the pollution of other impurity metal ions of purification.Being for starting material using HFSI can
To avoid the pollution of other impurity metal ions, solid-liquid biphasic reaction process discharges a large amount of hydrochloric acid and slowly, easily cause chlorine from
Son residual；Two aqueous liquid phase reactors cause product yield low, moisture in product, can not be effectively controlled, cause product matter
Amount is poor, and these disadvantages also make LiFSI mass be difficult to meet to require, and it can not be made to be applied to the application of industrial lithium battery.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of preparation method is simple, high income, purity are high, stability
The preparation method of good and low impurity content imidodisulfuryl fluoride lithium salt.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of imidodisulfuryl fluoride lithium salt, comprises the following steps：
S01：Double fluorine sulfimides and organic lithium salt LiR are swapped into reaction in solvent-free or organic solvent, produce double fluorine
Sulphonyl imonium lithium salts and organic matter HR, the organic matter HR PKa are 0 ~ 50, and the exchange reaction is under the conditions of gas shield
Carry out, the protective gas typically refers to be not easy and main component (such as double fluorine sulfimides, the organic lithium salt in reaction system
Deng) gaseous material that chemically reacts, can be such as nitrogen, helium, neon, argon gas, Krypton, xenon in one kind or
A variety of combinations, reaction temperature are 0~60 DEG C, preferably 15~40 DEG C, can be by the way of water-bath temperature control, art technology
Personnel can adjust the reaction time of above-mentioned reaction according to reaction process, such as can be judged instead by monitoring the response situation of raw material
Process is answered, in some embodiments of the invention, the reaction time of above-mentioned reaction can be 1~4 hour；
S02：Reactant under condition of no solvent in S01 is added into bad reagent crystallization, separation of solid and liquid produces double fluorine sulfimides
Lithium salts；
S03：By the reactant separation of solid and liquid in S01 under the conditions of organic solvent, liquid phase is concentrated, adds bad reagent crystallization, Gu
Liquid, which separates, produces imidodisulfuryl fluoride lithium salt.
Double fluorine sulfimides described in S01 and the organic lithium salt LiR mol ratio are 0.90 ~ 1.1, preferably 0 .95
~1.05.
Organic solvent described in S01 is one or more combinations in ketone, esters or ether solvent, and the ketone is molten
Agent may be selected from one in 1-METHYLPYRROLIDONE, acetone, methyl ethyl ketone, butanone, methyl tertbutyl ketone or 4-methyl-2 pentanone
Kind or a variety of combinations；The esters solvent may be selected from dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, ethylene carbonate,
Propene carbonate, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate or acetic acid second
One or more combinations in alkene ester；The ether solvent may be selected from ether, propyl ether, isopropyl ether, butyl ether, isobutyl ether, tetrahydrochysene
It is one or more in furans, methyltetrahydrofuran, cyclopentyl methyl ether, dioxane, dioxolane or glycol dimethyl ether
Combination, those skilled in the art can adjust the dosage of reaction dissolvent according to specific reaction system and the species of reaction dissolvent, have
The dosage of solvent can be 1~6 times of HFSI weight, preferably 1 .5~3 times of HFSI weight.
Organic matter HR described in S01 is trifluoracetic acid, trichloroacetic acid, formic acid, acetic acid, propionic acid, oxalic acid, citric acid, benzene first
Sour or other organic matters with acid group.
Organic matter HR described in S01 is acetylacetone,2,4-pentanedione, trifluoroacetylacetone (TFA), hexafluoroacetylacetone or other has diketone base
Organic matter.
Organic matter HR described in S01 is methanol, ethanol, isopropanol, isobutanol, phenol or other organic with alcohol radical
Thing.
Organic matter HR described in S01 is diisopropylamine, double -3 methyl silicon amine or other organic matters with two level ammonium.
Organic matter HR described in S01 is pyrovinic acid, 9 fluorine butyl sulfonic acids or other organic matters with sulfonate radical.
Organic matter HR described in S01 is methyl acetate, ethyl acetate, dimethyl malenate, diethyl malonate or other
Organic matter with esters.
Bad reagent described in bad reagent and S03 described in S02 is selected from saturated hydrocarbons, halogenated hydrocarbon, arene
Or one or more combinations in Polyhalogenated aromatic hydrocarbons low polar solvent, it may be selected from n-hexane, hexamethylene, dichloromethane, two
One or more combinations in chloroethanes, toluene, dimethylbenzene, chlorobenzene or dichloro-benzenes, the dosage of the bad reagent can be
1 .5~8 times of HFSI weight, preferably 2~4 times, the number of crystallization can be at least once.
Thickening temperature described in S03 is 10~80 DEG C, preferably 25 ~ 60 DEG C, can be by the way of being concentrated under reduced pressure.
Double fluorine sulfimides can be prepared by the preparation method of double fluorine sulfimides in CN104925765A.
The beneficial effect that the present invention is reached：The present invention is prepared double using double fluorine sulfimides with organic lithium salt synthetic reaction
Fluorine sulfimide lithium salts, reaction postprocessing method is simple, and product yield is high, and purity is high, steady quality, moreover it is possible to effectively reduce product
The impurity contents such as middle potassium ion, sodium ion, chlorion, sulfate ion and moisture, operating procedure of the present invention is simple, production cost
Rationally, it is safe, and it is more suitable for industrialized production.
Embodiment
The invention will be further described below.Following examples are only used for the technical side for clearly illustrating the present invention
Case, and can not be limited the scope of the invention with this.
Embodiment 1
In 250mL reaction bulbs, phenol lithium salts 24.2g is placed, control temperature stirs lower dropwise addition 45g HFSI to 10~30 DEG C.Stir
Mix 3 hours, add 200g dichloromethane stirring reactions, white solid product separates out, and obtains product 42.3g after filtered, dry, receives
Rate 88%.(testing result：AAS(ppm)：Na+(4ppm), K+(4ppm), Fe2+＜ 1ppm, Ca2+<1ppm ；IC：Cl-
(7ppm), SO4 2-(<1ppm )。
Embodiment 2
In 250mL reaction bulbs, acetic acid lithium salts 15.75g is placed, control temperature stirs lower dropwise addition 45g HFSI to 10~30 DEG C.Stir
To mix 2 hours, add 200g dichloromethane stirring reactions, white solid product is separated out, and product 47.04g is obtained after filtered, dry,
Yield 98%.(testing result：AAS( ppm )：Na+(4 ppm), K+(4ppm), Fe2+＜ 1ppm, Ca2+<1ppm ；IC：
Cl-(7ppm), SO4 2- (<1ppm)。
Embodiment 3：
In 500mL reaction bulbs, dimethyl carbonate 120g, pyrovinic acid lithium salts 24.75g, control temperature to 10~30 are separately added into
DEG C, lower dropwise addition 45g HFSI are stirred, are stirred 4 hours, filtrate decompression removes solvent, thick concentrate is obtained, into concentrate
200g toluene stirring reactions are added, white solid product is separated out, and product 39.2g, yield 81.2% are obtained after filtered, dry.(inspection
Survey result：AAS( ppm )：Na+(4ppm), K+(4ppm), Fe2+＜ 1ppm, Ca2+<1ppm ；IC：Cl-(4ppm),
SO4 2- (<1ppm)。
Embodiment 4
In 500mL reaction bulbs, tetrahydrofuran 150g, diethyl malonate lithium salts 40.7g, control temperature to 10~30 are separately added into
DEG C, lower dropwise addition 45g HFSI are stirred, are stirred 2 hours, filtrate decompression removes solvent, thick concentrate is obtained, into concentrate
200g n-hexane stirring reactions are added, white solid product is separated out, and product 43.2g, yield 89.5% are obtained after filtered, dry.
(testing result：AAS( ppm )：Na+(4ppm), K+(4ppm), Fe2+＜ 1ppm, Ca2+<1ppm ；IC：Cl-(5ppm
), SO4 2- ( <1ppm )。
The preparation of double fluorine sulfimides：In 1000mL tetrafluoro reaction bulbs, HClSI 500g, SbCl5 1g are added, are warming up to
100~105 DEG C, HF gases about 110g is slowly passed through under stirring, reaction is cooled to room temperature after 15 hours, advertises nitrogen, obtains thick
Product about 420g, short steaming obtain product 380g.Product is colourless liquid, and fusing point is 17 DEG C or so.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvement and deformation can also be made, these are improved and deformation
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of imidodisulfuryl fluoride lithium salt, it is characterized in that, comprise the following steps：
S01：Double fluorine sulfimides and organic lithium salt LiR are swapped into reaction in solvent-free or organic solvent, produce double fluorine
Sulphonyl imonium lithium salts and organic matter HR, the organic matter HR PKa are 0 ~ 50, and the exchange reaction is under the conditions of gas shield
Carry out, reaction temperature is 0~60 DEG C；
S02：Reactant under condition of no solvent in S01 is added into bad reagent crystallization, separation of solid and liquid produces double fluorine sulfimides
Lithium salts；
S03：By the reactant separation of solid and liquid in S01 under the conditions of organic solvent, liquid phase is concentrated, adds bad reagent crystallization, Gu
Liquid, which separates, produces imidodisulfuryl fluoride lithium salt.
2. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, it is double described in S01
Fluorine sulfimide and the organic lithium salt LiR mol ratio are 0.90 ~ 1.1.
3. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Solvent is one or more combinations in ketone, esters or ether solvent.
4. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Machine thing HR is trifluoracetic acid, trichloroacetic acid, formic acid, acetic acid, propionic acid, oxalic acid, citric acid, benzoic acid or other having with acid group
Machine thing.
5. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Machine thing HR is acetylacetone,2,4-pentanedione, trifluoroacetylacetone (TFA), hexafluoroacetylacetone or other organic matters with diketone base.
6. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Machine thing HR is methanol, ethanol, isopropanol, isobutanol, phenol or other organic matters with alcohol radical.
7. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Machine thing HR is diisopropylamine, double -3 methyl silicon amine or other organic matters with two level ammonium.
8. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Machine thing HR is pyrovinic acid, 9 fluorine butyl sulfonic acids or other organic matters with sulfonate radical.
9. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, have described in S01
Machine thing HR is methyl acetate, ethyl acetate, dimethyl malenate, diethyl malonate or other organic matters with esters.
10. a kind of preparation method of imidodisulfuryl fluoride lithium salt according to claim 1, it is characterized in that, described in S02 not
Bad reagent described in good reagent and S03 be selected from saturated hydrocarbons, halogenated hydrocarbon, arene, Polyhalogenated aromatic hydrocarbons or other
One or more combinations in low polar solvent, and/or thickening temperature described in S03 are 10~80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710680013.1A CN107416782A (en) | 2017-08-10 | 2017-08-10 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710680013.1A CN107416782A (en) | 2017-08-10 | 2017-08-10 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107416782A true CN107416782A (en) | 2017-12-01 |
Family
ID=60437623
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710680013.1A Pending CN107416782A (en) | 2017-08-10 | 2017-08-10 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107416782A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373142A (en) * | 2018-01-25 | 2018-08-07 | 广州理文科技有限公司 | A kind of high-purity is double（Fluorine sulphonyl）The preparation method of imine lithium |
| CN109928371A (en) * | 2019-04-12 | 2019-06-25 | 广州理文科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| CN110697668A (en) * | 2019-11-20 | 2020-01-17 | 上海如鲲新材料有限公司 | Preparation method of high-purity bis (fluorosulfonyl) imide salt |
| KR20200005970A (en) * | 2018-07-09 | 2020-01-17 | 이피캠텍 주식회사 | method for preparing lithium bisfluorosulfonylimide |
| CN111320151A (en) * | 2020-02-18 | 2020-06-23 | 白银科奥夫化学科技有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| CN111573639A (en) * | 2020-05-12 | 2020-08-25 | 广州理文科技有限公司 | Method for preparing lithium bis (fluorosulfonyl) imide by using organic metal lithium reagent |
| CN111634894A (en) * | 2019-03-01 | 2020-09-08 | 麻省固能控股有限公司 | Lithium sulfonimide salt composition being liquid at room temperature and free of free solvent and application thereof in lithium ion battery |
| CN112236388A (en) * | 2018-06-01 | 2021-01-15 | 阿科玛法国公司 | Method for producing lithium bis (fluorosulfonyl) imide salt |
| CN114031053A (en) * | 2021-12-15 | 2022-02-11 | 江苏华盛锂电材料股份有限公司 | Preparation method of bis (fluorosulfonyl) imide salt |
| US11267707B2 (en) | 2019-04-16 | 2022-03-08 | Honeywell International Inc | Purification of bis(fluorosulfonyl) imide |
| CN114524422A (en) * | 2022-03-31 | 2022-05-24 | 河南省氟基新材料科技有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105916805A (en) * | 2013-12-05 | 2016-08-31 | 罗地亚经营管理公司 | Method for preparing bis(fluorosulfonyl)imide acid and salts thereof |
| 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 |
| KR101718292B1 (en) * | 2015-11-26 | 2017-03-21 | 임광민 | Novel method for preparing lithium bis(fluorosulfonyl)imide |
-
2017
- 2017-08-10 CN CN201710680013.1A patent/CN107416782A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105916805A (en) * | 2013-12-05 | 2016-08-31 | 罗地亚经营管理公司 | Method for preparing bis(fluorosulfonyl)imide acid and salts thereof |
| KR101718292B1 (en) * | 2015-11-26 | 2017-03-21 | 임광민 | Novel method for preparing lithium bis(fluorosulfonyl)imide |
| 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 |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373142A (en) * | 2018-01-25 | 2018-08-07 | 广州理文科技有限公司 | A kind of high-purity is double（Fluorine sulphonyl）The preparation method of imine lithium |
| CN112236388A (en) * | 2018-06-01 | 2021-01-15 | 阿科玛法国公司 | Method for producing lithium bis (fluorosulfonyl) imide salt |
| KR20200005970A (en) * | 2018-07-09 | 2020-01-17 | 이피캠텍 주식회사 | method for preparing lithium bisfluorosulfonylimide |
| KR102275418B1 (en) | 2018-07-09 | 2021-07-12 | 이피캠텍 주식회사 | method for preparing lithium bisfluorosulfonylimide |
| CN111634894B (en) * | 2019-03-01 | 2023-12-29 | 麻省固能控股有限公司 | Free solvent free lithium sulfonimide salt compositions that are liquid at room temperature and their use in lithium ion batteries |
| CN111634894A (en) * | 2019-03-01 | 2020-09-08 | 麻省固能控股有限公司 | Lithium sulfonimide salt composition being liquid at room temperature and free of free solvent and application thereof in lithium ion battery |
| CN109928371A (en) * | 2019-04-12 | 2019-06-25 | 广州理文科技有限公司 | A kind of preparation method of imidodisulfuryl fluoride lithium salt |
| US11267707B2 (en) | 2019-04-16 | 2022-03-08 | Honeywell International Inc | Purification of bis(fluorosulfonyl) imide |
| EP3825278A1 (en) * | 2019-11-20 | 2021-05-26 | Shanghai Rolechem Co., Ltd. | Method for preparing high-purity bisfluorosulfonylimide salt |
| CN110697668B (en) * | 2019-11-20 | 2021-08-06 | 上海如鲲新材料有限公司 | Preparation method of high-purity bis (fluorosulfonyl) imide salt |
| CN110697668A (en) * | 2019-11-20 | 2020-01-17 | 上海如鲲新材料有限公司 | Preparation method of high-purity bis (fluorosulfonyl) imide salt |
| CN111320151A (en) * | 2020-02-18 | 2020-06-23 | 白银科奥夫化学科技有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
| CN111573639A (en) * | 2020-05-12 | 2020-08-25 | 广州理文科技有限公司 | Method for preparing lithium bis (fluorosulfonyl) imide by using organic metal lithium reagent |
| CN114031053A (en) * | 2021-12-15 | 2022-02-11 | 江苏华盛锂电材料股份有限公司 | Preparation method of bis (fluorosulfonyl) imide salt |
| CN114031053B (en) * | 2021-12-15 | 2023-05-09 | 江苏华盛锂电材料股份有限公司 | Preparation method of difluoro sulfonyl imide salt |
| CN114524422A (en) * | 2022-03-31 | 2022-05-24 | 河南省氟基新材料科技有限公司 | Preparation method of lithium bis (fluorosulfonyl) imide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107416782A (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| CN110697668B (en) | Preparation method of high-purity bis (fluorosulfonyl) imide salt | |
| KR101668293B1 (en) | Method for preparing bis(fluorosulfonyl)imide | |
| CN106044728B (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| KR101338653B1 (en) | Process for producing perfluoroalkylsulfonic acid salt | |
| CN106241757B (en) | A kind of preparation method of imidodisulfuryl fluoride lithium salt | |
| CN113247871B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN106276829B (en) | A kind of synthetic method of double fluorine sulfimide lithiums | |
| CN103259040B (en) | Organotin fluoride is utilized to prepare the method for high-purity lithium difluorophosphate | |
| CN104744427A (en) | Method for preparing cyclic sulphate | |
| US10734664B1 (en) | Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude HFSI, and uses of purified HFSI products | |
| EP2289875B1 (en) | Process for producing perfluoroalkanesulfinic acid salt | |
| CN109678694A (en) | A kind of preparation method of tetrafluoro oxalic acid lithium phosphate | |
| WO2016072158A1 (en) | Method for purifying electrolyte solution and method for producing electrolyte solution | |
| WO2011027867A1 (en) | Method for producing bis(sulfonyl)imide ammonium salts, bis(sulfonyl)imide, and bis(sulfonyl)imide lithium salts | |
| KR101961779B1 (en) | Process for preparing a sulfonimide compound and its salts | |
| KR20140102248A (en) | Lipf6 solutions | |
| WO2011148971A1 (en) | Process for preparation of fluorine-containing sulfonyl imide compounds | |
| JP6023432B2 (en) | Perfluorobutanesulfonyl fluoride, perfluorobutanesulfonic acid potassium salt, and method for producing perfluorobutanesulfonyl fluoride | |
| US20120302787A1 (en) | Process for producing perfluorobutanesulfonic acid salt | |
| KR101609404B1 (en) | Aqueous methods for making fluorinated sulfonate esters | |
| WO2012039025A1 (en) | Process for producing perfluoroalkylsulfonamide | |
| JP2011037784A (en) | Method for producing perfluoroalkyl sulfonamide | |
| JP5811671B2 (en) | Method for producing fluoroalkanesulfonic acid | |
| CN116573618A (en) | Process for preparing alkali metal salt of bisfluorosulfonyl imide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171201 |