CN103864022A - Sulfuryl fluoride preparation method - Google Patents
Sulfuryl fluoride preparation method Download PDFInfo
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- CN103864022A CN103864022A CN201210540471.2A CN201210540471A CN103864022A CN 103864022 A CN103864022 A CN 103864022A CN 201210540471 A CN201210540471 A CN 201210540471A CN 103864022 A CN103864022 A CN 103864022A
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Abstract
The invention provides a sulfuryl fluoride preparation method using sulfuryl chloride as a raw material by two-stage fluorination reaction, the sulfuryl fluoride preparation method has the advantages of simple technology and equipment, easy enlarging production, high product purity and the like, and prepared sulfuryl fluoride can be used as a fumigant to replace methyl bromide.
Description
Technical field
The present invention relates to a kind of preparation method of sulfuryl fluoride, especially relate to a kind of method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material.
Background technology
Sulfuryl fluoride (Profume), under normal temperature, be colorless and odorless gas, there is desinsection wide spectrum, diffusion permeability is strong, toxicity is low, residual less, use temperature scope extensively, do not fire the features such as not quick-fried, non-corrosiveness, it is logistics remove the evil, the enter and leave the border relevant industries such as health quarantine and Plant Quarantine and agricultural, forestry, trade in commodities, traffic health, water conservancy, building use ideal fumigant both at home and abroad at present, be to substitute monobromomethane, do not destroy the good fumigant of environmental protection of atmospheric ozone layer.
The preparation method of the sulfuryl fluoride of report is as follows at present:
(1) taking sulphur trioxide as raw material
US3403144 has reported that employing barium fluoride or barium silicofluoride react the method for preparing sulfuryl fluoride with sulphur trioxide, and temperature of reaction is 500～600 DEG C, and barium fluoride is reacted preparation with hydrofluoric acid by barium sulphide.
Patent CN102351681 has reported the method for continuously synthetic trifluoroacetyl chloride and sulfuryl fluoride, pass into continuously by sulphur trioxide and Freon 113 the reactive distillation column middle and lower part that catalyzer and filler are housed, control 120～130 DEG C of tower reactor temperature, reflux ratio 2.5～3, from overhead collection trifluoroacetyl chloride, sulfuryl chloride in tower reactor and pyrosulfuryl chloride are after fractionation, by sulfuryl chloride and hydrogen fluoride, under the effect of Pd/C catalyzer, fluoridation generates sulfuryl fluoride.
(2) taking sulfurous gas as raw material
Muetterties has reported that silver fluoride reacts the method (Inorganic Syntheses, Volume VI, p158-161) of preparing sulfuryl fluoride with sulfurous gas.
US Patent No. 2772144, US3092458, US3320030, US4102987 etc. have reported taking sulfurous gas, chlorine, hydrogen fluoride as raw material, under the catalysis of Pd/C catalyzer, prepare sulfuryl fluoride, reaction produces difluoro sulfoxide, by product, separate with sulfuryl fluoride is more difficult, the easy inactivation of the method catalyzer, catalytic efficiency is low, and catalyzer cost is high.
(3) taking sulfuryl chloride as raw material
Patent CN1489560 has reported to adopt to have at least two nitrogen-atoms monocycle or the dicyclic compound of (wherein at least one nitrogen-atoms inserts in ring) uses as catalyzer or the fluorizating agent of fluorine chlorine replacement reaction, as sulfuryl chloride reacts the mixture that can obtain sulfuryl fluoride and sulfuryl fluoride chlorine with the hydrogen fluoride adducts of DBN or DBU.But the method still needs to use hydrofluoric acid, and conversion unit is had relatively high expectations.
Tullock etc. have reported (J.O.C 1965,25,2016-2019) use the anhydrous Sodium Fluoride of high dispersive to carry out permutoid reaction as fluorizating agent and muriate and prepare reacting of corresponding fluorochemical, when wherein sulfuryl chloride reacts with Sodium Fluoride, when mole proportioning of Sodium Fluoride and sulfuryl chloride is 4.96:1, when reaction solvent is acetonitrile, reaction product only obtains sulfuryl fluoride chlorine, in the time that reaction solvent changes DMF into, reaction product is the mixture of sulfuryl fluoride and sulfuryl fluoride chlorine, taking sulfuryl fluoride chlorine as main.
Padam etc. have reported taking potassium hydrogen fluoride or Potassium monofluoride as fluorination reagent and sulfuryl chloride carries out fluorine chlorine permutoid reaction, reaction product is the mixture of sulfuryl fluoride and sulfuryl fluoride chlorine, wherein sulfuryl fluoride chlorine is principal product, the yield of sulfuryl fluoride chlorine approximately 40%, the about 20%(Indian Journal of the yield of Chemistry 1981 of sulfuryl fluoride, Vol 20A, p777-779).
Summary of the invention
The object of the present invention is to provide a kind of processing method of preparing sulfuryl fluoride, there is Processes and apparatus simple, be easy to amplify and produce, and the advantages such as high purity product that are easy to get.
For reaching goal of the invention the technical solution used in the present invention be:
Prepare a processing method for sulfuryl fluoride taking sulfuryl chloride as raw material, it is characterized in that adopting two-stage fluoridation,
(1) first step fluoridation: add polar non-proton organic solvent, organic amine catalyzer and anhydrous potassium fluoride in the first reactor, under whipped state, add sulfuryl chloride, controlling charge temperature is 40～90 DEG C, after having fed in raw material, be warming up to 50～150 DEG C, reaction pressure control is 1～10atm, sulfuryl chloride and anhydrous potassium fluoride carry out fluorine chlorine permutoid reaction, generate the SO that contains of gaseous state
2f
2and SO
2the reacting product stream of ClF;
(2) second stage fluoridation: contain polar non-proton organic solvent and anhydrous potassium fluoride in the second reactor, what first step fluoridation generated contains SO
2f
2and SO
2the reacting product stream of ClF adds from the second reactor bottom in gas sparging mode, further reacts rear generation be essentially SO with anhydrous potassium fluoride
2f
2reacting product stream, after condensation, obtain SO
2f
2, controlling temperature of reaction is 40～90 DEG C, reaction pressure is 1～5atm.
Reaction equation of the present invention is as follows:
SO
2Cl
2+KF→SO
2F
2+SO
2ClF (1)
SO
2ClF+KF→SO
2F
2 (2)
In first step fluoridation, in the first reactor, organic solvent and catalyzer are liquid, and anhydrous potassium fluoride in organic solvent, carries out fluorine chlorine permutoid reaction with the sulfuryl chloride of liquid with solid particulate form suspended dispersed under whipped state, generate the SO that contains of gaseous state
2f
2and SO
2the reacting product stream of ClF, this reacting product stream is with SO
2f
2be main, account for 70～90% of reaction product current mass, contain in addition a small amount of SO
2clF.The object of second stage fluoridation is to make SO
2clF further reacts and generates SO with anhydrous potassium fluoride
2f
2, for being conducive to raw material contact, promoting reaction, gaseous state containing SO
2f
2and SO
2the reacting product stream of ClF adds from the second reactor bottom in gas sparging mode, fully contacts with the anhydrous potassium fluoride being suspended in organic solvent, and further reaction generates and is essentially SO
2f
2reacting product stream.
The fluorination reagent that the present invention uses is anhydrous potassium fluoride, and its moisture content is preferably 20～4000ppm, and more preferably 20～2000ppm, is particularly preferably 20～1000ppm.
The polar non-proton organic solvent that the present invention uses is the one in acetonitrile, dimethyl formamide, N,N-DIMETHYLACETAMIDE, Nitromethane 99Min., ethyl acetate, butylacetate, methylcarbonate, methylene dichloride and hexanaphthene, more than two or three combination preferably; The further preferably one in acetonitrile, ethyl acetate, Nitromethane 99Min. and methylene dichloride, more than two or three combination.
The organic amine catalyzer that the present invention uses is the one in Trimethylamine 99, triethylamine, tripropyl amine, Tributylamine, triethanolamine, methyl piperidine, lupetidine and lupetazin, more than two or three combination preferably; More preferably triethylamine and/or Tributylamine.Mole proportion optimization of organic amine catalyzer and sulfuryl chloride is 0.001:1～0.05:1.
In the present invention, mole proportion optimization of raw material sulfuryl chloride and anhydrous potassium fluoride is 1:2～1:25, more preferably 1:2.5～1:15.
In reaction of the present invention, when first step fluoridation, temperature of reaction is too low, and speed of response is slower, and temperature of reaction is too high, and energy consumption is larger, therefore first step fluorination reaction temperature is preferably 50～100 DEG C; When second stage fluoridation, reactant is gaseous state, and being increases the retention time of reaction substrate in reaction system, and ensures speed of response, and second stage fluorination reaction temperature is preferably 40～90 DEG C, more preferably 50～80 DEG C.First step fluoridation is preferably carried out under 1～10atm pressure, particularly preferably in carrying out under normal pressure; Second stage fluoridation is preferably carried out under 1～5atm pressure, particularly preferably in carrying out under normal pressure.
When first step fluoridation, the heat release of reacting while dripping sulfuryl chloride for the ease of controlling, raw material sulfuryl chloride can use reaction solvent to dilute.In first step fluoridation, the time for adding of sulfuryl chloride is preferably 0.1～4h, contains SO in the fluoridation of the second stage
2f
2and SO
2the feed rate of the reacting product stream of ClF is preferably 0.01～0.5L/min.
Compared with prior art, tool of the present invention has the following advantages: Processes and apparatus is simple, and corrodibility is little, is easy to amplify produce, and is easy to get and arrives high purity product etc.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, but does not limit the invention to these embodiments.One skilled in the art would recognize that the present invention contained all alternativess, improvement project and the equivalents that within the scope of claims, may comprise.
Embodiment 1
First step fluoridation:
Is furnished with thermometer, in the 250mL there-necked flask of prolong, add acetonitrile 100mL, triethylamine 9.03mg, anhydrous potassium fluoride 40.00g(0.69mol, moisture content 300ppm), under stirring, in condenser, condensate temperature is-12 DEG C, after reaction system vacuumizes, be heated to 60 DEG C, drip sulfuryl chloride (18.6g, acetonitrile (30mL) solution 0.135mol), this solution is faint yellow, significant reaction heat release in dropping process, control sulfuryl chloride rate of addition, that temperature of reaction maintains 60-65 DEG C, time for adding is 2h, after dropping finishes, being warming up to temperature of reaction is 70 DEG C, continue reaction 2h, reaction solution is oyster white, yellow disappearance, gaseous product 14g is collected in reaction altogether.The gas that reaction produces carries out GC, GC-MS qualitative, quantitative characterizes, and reaction liquid after filtering, carries out GC, GC-MS.Through qualitative and quantitative analysis, the transformation efficiency of sulfuryl chloride is 99.8%, and gaseous product is sulfuryl fluoride (SO
2f
2), sulfuryl fluoride chlorine (SO
2clF), and trace solvent and air, sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) selectivity is respectively 83.1%, 16.3%, and other are 0.6% years old.
Second stage fluoridation:
Be furnished with in the 100mL there-necked flask of thermometer, prolong and magnetic stirrer, add acetonitrile 40mL, anhydrous potassium fluoride 15.00g(0.26mol, moisture content 300ppm), the gas autoreaction bottle bottom of collecting through one-level fluoridation passes into, gas feed speed is 0.1L/min, and temperature of reaction is 50 DEG C, and condenser temperature is-19 DEG C, collect reactant gases, after secondary fluoridation, sulfuryl fluoride chlorine is further fluoridized, after testing sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) content is respectively 99.1%, 0.45%, and other are 0.45% years old.
Embodiment 2
First step fluoridation:
Is furnished with thermometer, in the 250mL there-necked flask of prolong, add DMF50mL, Tributylamine 7.58mg, anhydrous potassium fluoride 20.01g(0.34mol, moisture content 250ppm), under stirring, in condenser, condensate temperature is-12 DEG C, after reaction system vacuumizes, be heated to 80 DEG C, drip sulfuryl chloride (5.5g, 0.041) DMF(15mL) solution, this solution is faint yellow, significant reaction heat release in dropping process, control sulfuryl chloride rate of addition, that temperature of reaction maintains 80～85 DEG C, time for adding is 50min, after finishing, dropping is warming up to 95 DEG C, continue reaction 1h, reaction solution is oyster white, yellow disappearance, gaseous product 4.25g is collected in reaction altogether.The gas that reaction produces carries out GC, GC-MS qualitative, quantitative characterizes, and reaction liquid after filtering, carries out GC, GCMS.Through qualitative and quantitative analysis, the transformation efficiency of sulfuryl chloride is 99.9%, and gaseous product is sulfuryl fluoride (SO
2f
2), sulfuryl fluoride chlorine (SO
2clF), sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) selectivity is respectively 86.4%, 13.3%, and other are 0.3% years old.
Second stage fluoridation:
Be furnished with in the 100mL there-necked flask of thermometer, prolong and magnetic stirrer, add DMF35mL, anhydrous potassium fluoride 11.20g(0.19mol, moisture content 250ppm), the gas autoreaction bottle bottom of collecting through one-level fluoridation passes into, gas feed speed is 0.05L/min, and temperature of reaction is 80 DEG C, and condenser temperature is-22 DEG C, collect reactant gases, after secondary fluoridation, sulfuryl fluoride chlorine is further fluoridized, after testing sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) content is respectively 98.8%, 0.61%, and other are 0.59% years old.
Embodiment 3
First step fluoridation:
Is furnished with thermometer, in the 250mL there-necked flask of prolong, add ethyl acetate 50mL, Trimethylamine 99 3.56mg, anhydrous potassium fluoride 15.00g(0.26mol, moisture content 560ppm), under stirring, in condenser, condensate temperature is-6 DEG C, reaction system vacuumizes after processing, be heated to 50 DEG C, drip sulfuryl chloride (4.86g, ethyl acetate (15mL) solution 0.036mol), this solution is faint yellow, significant reaction heat release in dropping process, control sulfuryl chloride rate of addition, that temperature of reaction maintains 50～55 DEG C, time for adding is 30min, after finishing, dropping is warming up to 60 DEG C, continue reaction 1h, reaction solution is oyster white, yellow disappearance, gaseous product 3.88g is collected in reaction altogether.The gas that reaction produces carries out GC, GC-MS qualitative, quantitative characterizes, and reaction liquid after filtering, carries out GC, GC-MS.Through qualitative and quantitative analysis, the transformation efficiency of sulfuryl chloride is 99.5%, and gaseous product is sulfuryl fluoride (SO
2f
2), sulfuryl fluoride chlorine (SO
2clF), sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) selectivity is respectively 73.4%, 26.2%, and other are 0.4% years old.
Second stage fluoridation:
Be furnished with in the 100mL there-necked flask of thermometer, prolong and magnetic stirrer, add ethyl acetate 40mL, anhydrous potassium fluoride 5.36g(0.09mol, moisture content 560ppm), the gas autoreaction bottle bottom of collecting through one-level fluoridation passes into, gas feed speed is 0.02L/min, and temperature of reaction is 55 DEG C, and condenser temperature is-19 DEG C, collect reactant gases, after secondary fluoridation, sulfuryl fluoride chlorine is further fluoridized, after testing sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) content is respectively 97.3%, 2.18%, and other are 0.52% years old.
Embodiment 4
First step fluoridation:
Is furnished with thermometer, in the 1000mL there-necked flask of prolong, add acetonitrile 500mL, anhydrous potassium fluoride 253.00g(4.36mol, moisture content 310ppm), triethylamine 3.26g, under stirring, in condenser, condensate temperature is-2 DEG C, reaction system vacuumizes after processing, be heated to 70 DEG C, drip sulfuryl chloride (151.00g, acetonitrile (80mL) solution 1.12mol), this solution is faint yellow, significant reaction heat release in dropping process, control sulfuryl chloride rate of addition, that temperature of reaction maintains 70～75 DEG C, time for adding is 2.5h, after dropping finishes, being warming up to reaction soln refluxes, continue reaction 2h, after finishing, reaction finds through analyzing, sulfuryl chloride is complete reaction substantially, transformation efficiency is 99.8%, the gas that reaction produces directly enters secondary fluorination reactor, in reaction process, gas sampling GC analyzes, sulfuryl fluoride (SO
2f
2), sulfuryl fluoride chlorine (SO
2clF) selectivity is respectively 83.1%, 16.7%, and other are 0.2% years old.
Second stage fluoridation:
Be furnished with in the 250mL there-necked flask of thermometer, prolong and magnetic stirrer, add acetonitrile 100mL, anhydrous potassium fluoride 35.00g(0.60mol, moisture content 310ppm), the gas autoreaction bottle bottom that one-level fluoridation produces passes into, the speed that gas passes into is 0.1L/min, and temperature of reaction is 60 DEG C, and condenser temperature is-19 DEG C, collect reactant gases, after secondary fluoridation, sulfuryl fluoride chlorine is further fluoridized, after testing sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) content is respectively 99.0%, 0.5%, and other are 0.5% years old.
Embodiment 5
First step fluoridation:
Is furnished with thermometer, in the 1000mL there-necked flask of prolong, add ethyl acetate 500mL, Tributylamine 6.31g, anhydrous potassium fluoride 253.00g(4.36mol, moisture content 360ppm), under magnetic agitation, in condenser, condensate temperature is 9 DEG C, be heated to 65 DEG C, drip sulfuryl chloride (130.00g, ethyl acetate (80mL) solution 0.96mol), this solution is faint yellow, significant reaction heat release in dropping process, control rate of addition, make temperature of reaction maintain 65-70 DEG C, time for adding is 2.5h, after dropping finishes, being warming up to reaction soln refluxes, continue reaction 2h, the gas that reaction produces is collected with the steel cylinder of processing that vacuumizes of the refrigerator-freezer that is placed in-80 DEG C, reaction liquid is found by analysis, sulfuryl chloride primitive reaction is complete, transformation efficiency 99.7%, in reaction process, gas sampling GC analyzes, sulfuryl fluoride (SO
2f
2), sulfuryl fluoride chlorine (SO
2clF) selectivity is respectively 86.7%, 13.0%, and other are 0.3% years old.
Second stage fluoridation:
Be furnished with in the 250mL there-necked flask of thermometer, prolong and magnetic stirrer, add ethyl acetate 130mL, anhydrous potassium fluoride 58.00g(1mol, moisture content 360ppm), the gas autoreaction bottle bottom that one-level fluoridation is collected passes into certain speed, the speed that gas passes into is 0.08L/min, and temperature of reaction is 70 DEG C, and condenser temperature is-29 DEG C, collect reactant gases, after secondary fluoridation, sulfuryl fluoride chlorine is further fluoridized, after testing sulfuryl fluoride (SO
2f
2) and sulfuryl fluoride chlorine (SO
2clF) content is respectively 98.7%, 0.9%, and other are 0.4% years old.
Through two-stage fluoridation, the gaseous reaction product obtaining can obtain the sulfuryl fluoride that purity is greater than 99.8% after simple aftertreatment.Two-stage flaorination process provided by the invention, compared with one-level fluoridation, selectivity and the yield of sulfuryl fluoride are all greatly improved, and are easy to purify.
Meanwhile, the present invention, by using anhydrous potassium fluoride, has avoided using the corrosion of hydrofluoric acid to conversion unit, is beneficial to industry and amplifies.
Claims (10)
1. a processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material, is characterized in that adopting two-stage fluoridation,
(1) first step fluoridation: add polar non-proton organic solvent, organic amine catalyzer and anhydrous potassium fluoride in the first reactor, under whipped state, add sulfuryl chloride, controlling charge temperature is 40～90 DEG C, mole proportioning of sulfuryl chloride and anhydrous potassium fluoride is 1:2～1:25, mole proportioning of catalyzer and sulfuryl chloride is 0.001:1～0.05:1, after having fed in raw material, be warming up to 50～150 DEG C, reaction pressure control is 1～10atm, sulfuryl chloride and anhydrous potassium fluoride carry out fluorine chlorine permutoid reaction, generate the SO that contains of gaseous state
2f
2and SO
2the reacting product stream of ClF;
(2) second stage fluoridation: contain polar non-proton organic solvent and anhydrous potassium fluoride in the second reactor, what first step fluoridation generated contains SO
2f
2and SO
2the reacting product stream of ClF adds from the second reactor bottom in gas sparging mode, further reacts rear generation be essentially SO with anhydrous potassium fluoride
2f
2reacting product stream, after condensation, obtain SO
2f
2, controlling temperature of reaction is 40～90 DEG C, reaction pressure is 1～5atm.
2. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 1, it is characterized in that described first step fluorination reaction temperature is 50～100 DEG C, reaction pressure is normal pressure, and second stage fluorination reaction temperature is 40～90 DEG C, and reaction pressure is normal pressure.
3. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 1, it is characterized in that polar non-proton organic solvent is selected from one, more than two or three combination in acetonitrile, dimethyl formamide, N,N-DIMETHYLACETAMIDE, Nitromethane 99Min., ethyl acetate, butylacetate, methylcarbonate, methylene dichloride and hexanaphthene.
4. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 3, it is characterized in that described polar non-proton organic solvent is selected from one, more than two or three combination in acetonitrile, ethyl acetate, Nitromethane 99Min. and methylene dichloride.
5. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 1, it is characterized in that described organic amine catalyzer is selected from one, more than two or three combination in Trimethylamine 99, triethylamine, tripropyl amine, Tributylamine, triethanolamine, methyl piperidine, lupetidine and lupetazin.
6. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 5, it is characterized in that described organic amine catalyzer is selected from triethylamine and/or Tributylamine.
7. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 7, mole proportioning that it is characterized in that described sulfuryl chloride and anhydrous potassium fluoride is 1:2.5～1:15.
8. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 1, the moisture content that it is characterized in that described anhydrous potassium fluoride is 20～4000ppm.
9. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 1, the time for adding that it is characterized in that sulfuryl chloride in described first step fluoridation is 0.1～4h, contains SO in the fluoridation of the second stage
2f
2and SO
2the feed rate of the reacting product stream of ClF is 0.01～0.5L/min.
10. according to the processing method of preparing sulfuryl fluoride taking sulfuryl chloride as raw material claimed in claim 1, it is characterized in that the SO that contains of described first step fluoridation generation
2f
2and SO
2in the reacting product stream of ClF, SO
2the mass content of ClF is 70～90%.
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| CN105107531A (en) * | 2015-08-19 | 2015-12-02 | 杭州茂宇电子化学有限公司 | Catalyst for synthesizing sulfuryl fluoride and preparation method therefor |
| CN114477100A (en) * | 2022-01-29 | 2022-05-13 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by sulfuryl chloride fluorination method |
| CN115259112A (en) * | 2022-07-04 | 2022-11-01 | 浙江中欣氟材股份有限公司 | Production method of bis-fluorosulfonyl imide and lithium salt thereof |
| CN115557471A (en) * | 2022-01-29 | 2023-01-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride and sulfuryl fluoride |
| WO2023142031A1 (en) * | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by using fluorination method for sulfuryl chloride |
| WO2023142027A1 (en) * | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105107531A (en) * | 2015-08-19 | 2015-12-02 | 杭州茂宇电子化学有限公司 | Catalyst for synthesizing sulfuryl fluoride and preparation method therefor |
| CN114477100A (en) * | 2022-01-29 | 2022-05-13 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by sulfuryl chloride fluorination method |
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| WO2023142031A1 (en) * | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | Method for preparing sulfuryl fluoride by using fluorination method for sulfuryl chloride |
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| CN115259112A (en) * | 2022-07-04 | 2022-11-01 | 浙江中欣氟材股份有限公司 | Production method of bis-fluorosulfonyl imide and lithium salt thereof |
| CN115259112B (en) * | 2022-07-04 | 2023-08-25 | 浙江中欣氟材股份有限公司 | Difluorosulfonyl imide and method for producing lithium salt thereof |
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