73 results about "Sulfonyl fluoride" patented technology

The invention relates to the technical field of chemical synthesis, and discloses a preparation method of anhydrous N, N-dimethyl amino sulfuryl fluoride, which comprises the following steps: (1) introducing sulfuryl fluoride gas into a dimethylamine organic solution to carry out nucleophilic substitution reaction, and then adding triethylamine to obtain a mixed solution containing N, N-dimethyl amino sulfuryl fluoride; and (2) sequentially carrying out normal-pressure rectification and reduced-pressure rectification on the mixed solution containing the N, N-dimethyl amino sulfonyl fluoride to obtain the N, N-dimethyl amino sulfonyl fluoride. According to the method, water is not introduced in the whole process, the risk of water residue is avoided, and the prepared product is high in yield and purity.

The invention provides perfluorosulfonic acid resin and a polymerization method. The polymerization method comprises the following steps: mixing perfluoromethyl vinyl ether, perfluorosulfonyl fluoride vinyl ether and a fluorine-containing solvent to obtain a mixed solution; and adding an initiator into the mixed solution, introducing a tetrafluoroethylene monomer, carrying out a copolymerization reaction, carrying out solid-liquid separation, and carrying out transformation and drying to obtain the perfluorinated sulfonic acid resin. The perfluoromethyl vinyl ether monomer is introduced into a copolymerization system, so that the rigidity of a polymer main chain is effectively reduced, and the flexibility and low-temperature mechanical strength of the resin are enhanced; the crystallinity is effectively reduced, the Tg is adjusted, and the catalyst is suitable for low-temperature proton exchange membrane fuel cells and other application scenes; the introduction of perfluoromethyl vinyl ether improves the compatibility between the main chain and the sulfonyl fluoride-containing side chain, and is beneficial to the formation of a clearer and more continuous hydrophilic / hydrophobic microphase separation structure. A stable proton conduction network is facilitated, and the electrochemical performance of the resin under harsh working conditions is remarkably improved.

The application belongs to the field of fine chemical industry and environmental protection, and particularly relates to a method for preparing metal triflate by using high gravity reaction. The method comprises the following steps: 1, using trifluoromethylsulfonyl chloride and anhydrous HF gas as raw materials to generate trifluoromethylsulfonyl fluoride gas; 2, performing gas-liquid contact reaction of the trifluoromethylsulfonyl fluoride gas with an alkali metal solution to obtain a mixed solution; 3, performing solid-liquid separation on the mixed solution by using a filter press, and the liquid phase is a triflate salt solution; 4, drying the triflate salt solution by using a spray dryer to obtain a solid-phase product triflate salt. The method uses trifluoromethylsulfonyl chloride and anhydrous HF as raw materials to replace triflic acid in the traditional method, and utilizes high gravity reaction, so that the production cost is greatly reduced. The process is simple, the obtained product triflate metal salt has low impurity content, is superior to the industry standard, the process is zero emission, and has good economic value and social value.

The application discloses a preparation method of a nitrogen-containing heterocyclic compound and an alkali metal salt of the nitrogen-containing heterocyclic compound, and steps of the preparation method of the nitrogen-containing heterocyclic compound comprise: (1) uniformly mixing trithiocyanic acid with a first solvent, introducing sulfuryl fluoride gas or adding an alkenyl sulfonyl fluoride to perform a reaction, and obtaining a crude product through a crude treatment after the reaction is finished; (2) purifying the crude product to obtain the nitrogen-containing heterocyclic compound shown in a structural formula 1; wherein R1, R2 and R3 are each independently selected from -H, -SO2F or -CH2-(CH2) n -SO2F, n is an integer selected from 1-10, and R1, R2 and R3 are not H at the same time. The preparation method of the nitrogen-containing heterocyclic compound and the alkali metal salt of the nitrogen-containing heterocyclic compound can be applied to a large amount of trithiocyanic acid in a lithium battery electrolyte, raw materials are easy to obtain, operation is simple, the yield is high, the condition is mild, the requirement for equipment is low, and the method is suitable for industrial production.

This application relates to the field of synthesis technology of lithium-ion battery electrolyte additives, specifically to a synthesis process of 1,3-propanedisulfonyl fluoride. The synthesis process includes the following steps: S1. Adding 1,3-propanedisulfonyl chloride and potassium fluoride to a reaction vessel; S2. Adding distilled water as a reaction solvent to the reaction vessel and refluxing under stirring; S3. After the reaction solution has settled and separated into layers, separating and collecting the oil phase, adding toluene and activated carbon to the oil phase, and refluxing for decolorization; S4. Performing a first crystallization treatment on the decolorized solution, followed by filtration, and washing the filter cake obtained from the filtration; S5. Collecting the filtrate obtained after the first washing and performing a second crystallization treatment, followed by filtration again; S6. Vacuum drying the filter cake obtained in steps S4 and S5 to obtain 1,3-propanedisulfonyl fluoride. This application features mild reaction conditions, simple operation, low cost, and environmental friendliness.

The invention discloses a diaminomaleonitrile derivative, a non-aqueous electrolyte thereof and a sodium ion battery. The structural formula of the diaminomaleonitrile derivative disclosed by the invention is shown as a formula I, and R1, R2, R3 and R4 are respectively and independently selected from one of-SO2F and-CH2CH2SO2F. The diaminomaleonitrile derivative has cyano (-CN), sulfonyl fluoride (-SO2F) and carbon-carbon double-bond functional groups, the functional groups have a synergistic effect, a stable CEI film can be formed on a positive electrode, the contained sulfonyl fluoride group can adjust charge distribution while enhancing the oxidation resistance of molecules, the functions of optimizing an ion transmission path and the like are achieved, and the service life of the battery is prolonged. Therefore, the high-voltage resistance of the battery is improved. Formula 1.

The invention provides a synthesis method of a negative charge highly delocalized sulfonyl imide alkali metal salt {[(R3SO2) (R2 (R1SO2N) SO) N] M), M = Li, Na, K, Rb or Cs}. The synthesis method comprises the following steps: carrying out oxidation and fluorination reaction on alkyl (S-alkyl sulfonyl imide) potassium sulfinate (or rubidium or cesium) and an N-fluorine electrophilic reagent to synthesize alkyl (S-alkyl sulfonyl imide) sulfonyl fluoride with the yield of 70-90%; the obtained alkyl (S-alkyl sulfimide) sulfonyl fluoride and sulfamide containing substituent R3 or alkali metal salt thereof are subjected to nucleophilic substitution reaction, the product is purified to obtain the high-purity negative-charge highly-delocalized sulfimide alkali metal salt, and the method has the characteristics that the operation is simple, the raw materials are low in price, the product is easy to separate and purify, the method is suitable for industrial mass production, and the like; and the prepared negative charge highly delocalized sulfimide alkali metal salt is high in chemical stability and good in solubility, and is a preferable electrolyte material for realizing high-specific-energy power and energy storage batteries.

The invention discloses a preparation method of an N-hydroxyurea compound, which specifically comprises the following steps: step 1, sequentially carrying out Lossen rearrangement and nucleophilic reaction under the action of alkali by taking Boc NHOH as shown in a formula 1 as an initial reactant, SO2F2 gas as an acylating agent and an amine compound RR 'NH as a nucleophilic reagent to obtain a tert-butoxyurea compound as shown in a formula 2; and 2, removing the tert-butoxy group from the tert-butoxyurea compound to obtain the N-hydroxyurea compound as shown in a formula 3. The innovation point of the invention is that commercialized easily available gas sulfonyl fluoride promotes Lossen rearrangement of tert-butylhydroxylamine to generate a key intermediate tert-butoxy isocyanate, the key intermediate tert-butoxy isocyanate and a substrate amine compound are subjected to a one-pot reaction to obtain the N-hydroxyurea compound, the reaction conditions are simple, the operation is convenient, the compatibility of substrate functional groups is strong, and the application prospect is good.

This application provides a perfluoro-4-butoxy-1-butylsulfonyl fluoride, its preparation method, and its application, relating to the field of chemical synthesis technology. The preparation method of the perfluoro-4-butoxy-1-butylsulfonyl fluoride according to this application includes the following steps: adding butoxybutylsulfonyl fluoride and functional additives to an electrolytic cell containing anhydrous hydrogen fluoride for an electrolytic reaction. The functional additives include alkali metal fluorides, thiols, and perfluorobutylsulfonyl fluoride, wherein the carbon chain length of the thiols is C2~C6. The preparation method of perfluoro-4-butoxy-1-butylsulfonyl fluoride can improve the yield of the target product.

The invention relates to an internal sulfonamide compound and a preparation method thereof. The invention relates to a preparation method of a sulfamide compound, which comprises the following steps: mixing an aminomalonic acid diethyl ester compound or an N-benzyl malonic acid monomethyl ester monoamide compound, a beta-aryl vinyl sulfonyl fluoride compound and MS, adding a solvent and a base catalyst, reacting at room temperature for 12-24 hours, separating and purifying to obtain the amide compound. The sulfamide compound and the preparation method thereof have the advantages of being simple in method, free of transition metal catalysis, wide in substrate range, mild in reaction condition, good in universality and the like.

The present invention addresses the problem of providing an electrolyte solution for a lithium metal secondary battery, which, when using 1, 2-dimethoxyethane (DME) as a solvent, is capable of simultaneously suppressing an increase in the resistance of the lithium metal secondary battery, suppressing the generation of gas, and suppressing an increase in the thickness of the negative electrode. The present invention is an electrolyte solution for a lithium metal secondary battery, the electrolyte solution comprising an electrolyte salt, an organic solvent, and a first additive, the electrolyte salt comprising lithium bis (fluorosulfonyl) imide (LiFSI), the organic solvent comprising 1, 2-dimethoxyethane (DME), the first additive being N, N-dimethyltrifluoromethanesulfonamide (DMTMSA), or N, N-dimethylformamide (DMTMSA), and the electrolyte solution comprising lithium bis (fluorosulfonyl) imide (LiFSI), the organic solvent comprising 1, 2-dimethoxyethane (DME), and the second additive comprising N, N-dimethyltrifluoromethanesulfonamide (DMTMSA), or N, N-dimethyltrifluoromethanesulfonamide (DMTMSA). The electrolyte solution for a lithium metal secondary battery contains at least one of N, N-dimethylaminosulfonyl fluoride (DMSF), and the first additive is contained in an amount of 0.2 parts by mass or more when the total mass of the electrolyte salt and the organic solvent is taken as 100 parts by mass.

This invention relates to an alkyl sulfonyl fluoride resin, its preparation method, and its applications. The structural formula of the alkyl sulfonyl fluoride resin is shown below: where n1 is 1~10000; n2 = 0~2. The preparation method includes: mixing compound 1 as shown in Formula I with a nitrite reagent and boron trifluoride diethyl ether and performing a diazotization reaction to obtain compound 2 as shown in Formula II; and then performing a fluorination reaction of compound 2 with a sulfur source, a fluorine source or a fluorosulfonylating reagent and an acid under the action of a catalyst to obtain the resin. Compared with the prior art, the preparation method of this invention is simple, the raw materials are readily available, and the prepared sulfonyl fluoride resin has high reactivity and good stability, and can be used as a high-efficiency matrix resin for the preparation of novel functional resins.

The invention discloses a preparation method of a benzylsulfonyl fluoride compound, which comprises the following steps: taking benzylthiocyanate as a substrate, in a solvent, taking benzylthiocyanate shown as a formula (1) as a substrate, reacting under the action of an additive, an F source and a gas atmosphere, and obtaining the benzylsulfonyl fluoride compound shown as a formula (2) after the reaction is finished, in the formulas (1) and (2), R is selected from one or more of H, alkyl, aryl, halogen, cyano, nitryl, alkoxy, acyl and amido. According to the method disclosed by the invention, the target product can be synthesized by only 4-8 hours, so that the target product can be obtained with relatively high yield, and the method is relatively rapid and efficient. According to the synthesis method disclosed by the invention, the benzyl sulfuryl fluoride compound is synthesized from simple and easily available benzyl thiocyanate under relatively simple conditions, and the fluorine-containing building block compound which is widely applied to the fields of medicines, pesticides and petrochemical engineering is realized.

The invention relates to a preparation method of trifluoromethanesulfonamide, which comprises the following steps: S1, introducing a refrigerant into a reactor to reduce the temperature of the reactor to 0 DEG C or below, introducing raw material ammonia water and a phase transfer catalyst into the reactor, introducing trifluoromethanesulfonyl fluoride into the ammonia water, and carrying out phase transfer reaction to obtain trifluoromethanesulfonamide; reacting trifluoromethanesulfonyl fluoride with excessive ammonia water to generate trifluoromethanesulfonamide ammonium salt and ammonium fluoride by-products; s2, raising the temperature to room temperature, discharging excessive ammonia gas, and adding acid into the reaction liquid to adjust the pH value to 2-3; and S3, extracting the reaction liquid by using an extracting agent, and combining and concentrating organic phases to obtain a trifluoromethanesulfonamide crude product. The method has the characteristics that the process is environment-friendly and simple, three wastes are easy to separate and recover, raw materials are cheap and easy to obtain, the reaction process is simple, no waste gas pollution is generated even if nitrogen protection is needed, the operation is easy, and the method is suitable for industrial production.

The invention belongs to the field of organic synthesis, and particularly relates to a synthesis method of terminal alkyne. The method comprises the following steps: mixing a 2-methylpyridine compound as shown in a formula 1 and N, N-dimethylformamide as shown in a formula 2 with an organic solvent (cyclopentyl methyl ether or tetrahydrofuran) in the presence of lithium bis (trimethylsilyl) amide, cesium fluoride, perfluorobutyl sulfonyl fluoride and 1, 8-diazabicyclo [5.4. 0] undec-7-ene, and reacting to synthesize the terminal alkyne as shown in a formula 3. The raw materials adopted by the invention are common chemicals in the market. The method is wide in application range, common terminal alkyne compounds can be synthesized, reaction substrates can be adjusted according to needs, and a series of terminal alkyne derivatives can be synthesized. Certain support is provided for research in the fields of medicine, material science and the like. The invention provides biological activity of an iso-terminal alkyne compound on oomycetes plant pathogens and a determination method of the iso-terminal alkyne compound.

The invention discloses a perfluorosulfonyl imide type proton exchange resin with a coupled multi-active center, which is obtained by grafting phosphonated polyhedral oligomeric silsesquioxane (POSS) on perfluorosulfonamide, and the specific preparation process is as follows: perfluorosulfonyl fluoride and ammonia gas react to generate perfluorosulfonamide; carrying out substitution reaction on the phosphonated POSS and triethyl phosphite to obtain an intermediate product; and carrying out Michael addition reaction on the intermediate product and perfluorosulfonylamino, and acidifying to obtain the target product. According to the perfluorosulfonyl imide type proton exchange resin with the coupled multi-element active center, the glass-transition temperature of a proton exchange membrane can be increased; meanwhile, the sulfonyl imide and the phosphonic acid group cooperatively construct a multiple proton transmission path and have rapid proton conduction capability, so that the proton exchange membrane can ensure rapid proton transmission even at a high temperature, the conductivity of the proton exchange membrane is improved, and the problem that a perfluorosulfonic acid proton exchange membrane in the prior art is relatively poor in performance under a high-temperature working condition is solved.

The application relates to the field of secondary batteries, and provides a battery monomer, a preparation method of the battery monomer, a battery device and an energy storage device. In the battery monomer, an electrolyte comprises a cyanopyridine additive, a sulfonyl fluoride additive and an amine additive, at least the initial efficiency of the battery monomer can be improved, and the capacity attenuation and internal resistance increase of the battery monomer can be well inhibited, so that the use performance of the battery monomer is improved.

The invention provides chiral spiral polyisocyanide with a sulfonamide structure as well as a preparation method and application of the chiral spiral polyisocyanide, and belongs to the technical field of high polymer materials. The preparation method comprises the following steps: carrying out nucleophilic fluorine exchange reaction on chiral alpha-phenylethylamine and sulfonyl fluoride isocyanide to prepare a sulfonamide modified isocyanide monomer, and initiating the activity of the monomer by adopting a nickel / palladium catalyst to carry out polymerization reaction, thereby preparing the chiral spiral polyisocyanide with a sulfonamide structure. The chiral spiral polyisocyanide with the sulfonamide structure has excellent stability and anti-interference capability, has high specificity to fluorine anions, generates macroscopic color change under visible light, disappears circular dichroism spectrum signals, and has wide application prospects in the field of fluorine ion recognition and detection.

The utility model relates to the technical field of chemical synthesis devices, in particular to a continuous production device for fluorination reaction. Comprising a catalyst conveying assembly, a hydrogen fluoride conveying assembly, a sulfonyl fluoride synthesis assembly and a sulfonyl chloride conveying assembly, the sulfonyl fluoride synthesis assembly comprises a reactor, a circulating pump, a static mixer, a post-treatment system and a filtering assembly, and the reactor is provided with a first inlet, a second inlet, a first outlet and a second outlet; the hydrogen fluoride conveying assembly communicates with the first inlet through a pipeline, the catalyst conveying assembly communicates with the second inlet through a pipeline, the first outlet communicates with the circulating pump through a pipeline, the end, away from the reactor, of the circulating pump communicates with the static mixer through a pipeline, and the end, away from the circulating pump, of the static mixer is connected to the first inlet through a pipeline. The second outlet is communicated with the post-treatment system through a pipeline, and the sulfonyl chloride conveying assembly is communicated with the static mixer through a pipeline; according to the utility model, the production efficiency is improved, and the energy consumption is reduced.

Described herein is a method including (I) forming a first mixture including: an ionomer including at least one pendant -SO3M group, where M is selected from H, alkali metals, alkaline-earth metals, and combinations thereof; a chlorination reagent; and a chlorination solvent; (II) reacting the first mixture to produce an at least partially chlorinated ionomer including at least one pendant -SO2Cl group; (III) forming a second mixture including: the at least partially chlorinated ionomer including at least one pendant -SO2Cl group; a fluorination reagent; and optionally a fluorination solvent; and (IV) reacting the second mixture to produce a sulfonyl fluoride-containing polymer including at least one pendant -SO2F group. The method is useful for recycling ionomers.

The invention relates to a preparation method of bis (fluorosulfonyl) imine salt. The method comprises the following steps: adding anhydrous ammonium fluoride and cation source fluoride into an organic solvent, and then dropwise adding a sulfonyl chloride solution; and after dropwise adding, continuously stirring, and carrying out reflux reaction for 5-20 hours to obtain the bis (fluorosulfonyl) imine salt. According to the method, hydrogen fluoride and sulfonyl fluoride are not adopted, meanwhile, the adverse effect of water of water-containing metal hydroxide or metal carbonate in the bis (fluorosulfonyl) imide salification reaction process on product purification is avoided, and efficient, low-cost and large-scale preparation of the bis (fluorosulfonyl) imide salt is achieved.

The present application relates to a method for preparing sulfuryl fluoride, the method comprising: (1) providing a reaction stream comprising an organic base-hydrogen fluoride complex; (2) introducing sulfur dioxide and chlorine into the reaction stream comprising the organic base-hydrogen fluoride complex, and reacting to form a product stream comprising sulfuryl fluoride. The method described in the present application has mild reaction conditions, high product yield and purity, material recycling, less waste, etc., and is suitable for industrial production.

The invention provides a preparation method of an anti-dehumidification fluorine-containing polymer filter membrane aiming at the problem that the existing fluorine-containing polymer filter membrane is easy to dehumidify, and belongs to the technical field of membrane separation. The method comprises the following steps: (1) directly infiltrating a fluorine-containing polymer filter membrane by using a monomer (such as perfluoro (4-methyl-3, 6-dioxa-7-octene) sulfonyl fluoride or dodecafluoro-6-heptylene-1-sulfonyl fluoride) of which one end of a molecular chain contains a reactive perfluoroalkyl group and the other end contains a hydrophilic group without alcohol pre-wetting; (2) irradiating the infiltrated filter membrane with ultraviolet light (such as a mercury lamp, excimer laser, an LED or a microwave electrodeless lamp); (3) soaking the treated filter membrane in a perfluoro solvent and an alcohol solvent in sequence; and (4) sequentially soaking the treated membrane in an alkaline liquid, an acidic liquid and deionized water for 1-60 minutes respectively. The prepared filter membrane has excellent anti-dehumidification performance and can be widely applied to the fields of gas separation, liquid filtration and the like.

A method for preparing cyano sulfonyl fluoride compounds is provided. Oxime ether compounds are used as free radical precursors, and under the condition of photocatalyst regulation, and in combination with the strategy of free radical sulfur dioxide insertion, the process involves photocatalytic oxidation, C—C bond cleavage rings, free radical SO2 insertion and fluorination to achieve cyano / fluorosulfonyl reaction of oxime ether, yielding cyano sulfonyl fluoride products.

The application relates to a lithium ion battery. The lithium ion battery comprises an electrolyte, a negative electrode sheet and a positive electrode sheet, the electrolyte comprises a first additive and a second additive, the first additive is fluoroethylene carbonate, the second additive is a sulfonyl fluoride compound, and A+lambda*B >= alpha / P+beta is met; A represents the mass percentage of fluoroethylene carbonate in the electrolyte, the unit is %, B represents the mass percentage of the second additive in the electrolyte, the unit is %, P represents the porosity of the negative electrode sheet, the unit is %, and the value range is 25-40; lambda represents a replacement equivalent coefficient, the value range is 0.1-0.5; alpha represents a porosity requirement coefficient of the negative electrode sheet, the value range is 80-120; and beta represents a reference film forming requirement coefficient, the value range is 3-7. In the scheme provided by the application, a stable and dense composite SEI film can be constructed, the cycle stability of the battery is improved, gas production is inhibited, and the long cycle life and high-temperature storage performance of the lithium ion battery are improved.

The application discloses a synthesis method of a beta-fluorosulfonyl sulfone compound and application thereof, and belongs to the technical field of chemical synthesis and medicinal chemistry. The method comprises the following steps: under a protective atmosphere, potassium trifluoroborate compound, a photocatalyst, a sulfur dioxide source, a hydrogen source and ethylenesulfonyl fluoride are mixed in an organic solvent, and reaction is carried out under light irradiation to obtain the beta-fluorosulfonyl sulfone compound. The application can realize preparation of a series of beta-fluorosulfonyl sulfone compounds, provides a new synthesis method for synthesis of the beta-fluorosulfonyl sulfone compound, and sulfone groups and sulfonyl fluoride groups are part of the structures of various drug molecules, so that the application is expected to be widely applied in the fields of organic synthesis, drug development and polymer materials.

The invention discloses a cyanophenyl sulfate compound and a preparation method and application thereof, and belongs to the technical field of battery electrolyte additives, the compound has a structure as shown in a formula I. The preparation method comprises the following steps: S1, mixing a compound as shown in a formula 2, a first acid-binding agent and a reaction solvent at 20-50 DEG C, introducing sulfonyl fluoride gas, and reacting for 6-24 hours; s2, adding a second acid-binding agent, and continuously reacting for 6-24 hours; s3, stopping introducing the sulfonyl fluoride gas, adding the compound as shown in the formula 2 again, reacting for 6-24 hours, and separating out a large amount of solid, namely the cyanophenyl sulfate compound; the invention provides a high-performance electrolyte additive, through molecular structure design, the technical problems of limited functional density and insufficient high-temperature stability of sulfate additives are solved, and an important material basis is provided for developing a new generation of lithium ion batteries with high energy density, long service life and high safety.

The invention provides a method for preparing 1, 3-perfluoropropane disulfonyl fluoride through electrolysis, which comprises the following steps: step 1, sequentially adding anhydrous HF (hydrogen fluoride), raw materials and a fluorinating agent into an electrolytic bath to form electrolyte; step 2, carrying out low-current water removal; and 3, electrolysis is conducted after water removal is completed, a final electrolysis product is obtained through electrolysis, the electrolysis product and the electrolyte are layered up and down, and liquid obtained in the lower layer contains the electrolysis product 1, 3-perfluoropropane disulfonyl fluoride. The method is simple in reaction condition, simple in device, high in yield and suitable for large-scale application.

The invention discloses a high-voltage lithium ion battery electrolyte additive, an electrolyte and a battery, and relates to the technical field of lithium ion battery electrolytes. The electrolyte additive comprises benzenesulfonyl fluoride and a bis-phosphorous acid propane derivative; the structural formula of the bis-phosphorous acid propane derivative is shown in the specification. According to the invention, the bis-phosphorous acid propane compound and the benzenesulfonyl fluoride have a synergistic effect, a compact and stable CEI film is formed on the surface of the positive electrode, effective passivation of the surface of the positive electrode is realized, and guarantee is provided for improving the interface stability of the electrolyte and the long cycle performance of the battery under high voltage.