23 results about "Difluoroacetic acid" patented technology

A method for producing an aromatic heterocycle-substituted difluoroacetic acid derivative having a partial structure represented by the formula (III), by reacting an N-oxido aromatic heterocyclic compound having a partial structure represented by the formula (I) with tetrafluoroethylene in the presence of a compound represented by the formula (II): R—YH, in a solvent selected from an aromatic hydrocarbon solvent, an ester solvent and an ether solvent:

The invention relates to the technical field of batteries, and provides a battery. The battery comprises a positive plate, a negative plate and electrolyte, the negative plate comprises a negative current collector and a negative active material layer arranged on at least one side surface of the negative current collector, and a plurality of concave parts are arranged on the surface of one side, far away from the negative current collector, of the negative active material layer; the negative active material layer comprises a silicon-based material and a carbon-based fiber material, and the length-diameter ratio of the carbon-based fiber material is 10-500; the electrolyte comprises a first solvent, and the first solvent comprises ethyl difluoroacetate; based on the total mass of the electrolyte, the mass ratio of the first solvent is 20.2%-75.1%. According to the battery, the cycling stability under high-voltage and high-temperature working conditions can be improved while the quick charging performance is ensured.

A lithium-ion battery includes an electrolyte, a negative electrode plate and a positive electrode plate. The electrolyte includes a fluorinated solvent, the fluorinated solvent comprises a difluoroethyl acetate; and with a content of the difluoroethyl acetate being f wt % based on a total weight of the electrolyte, and a ratio of a width of the negative electrode plate to a width of the positive electrode plate being g, the lithium-ion battery satisfies a following relation: 2≤f / g≤30.

The embodiment of the invention provides a bromo-ethyl difluoroacetate-mediated novel amide dehydration cyaniding method, which comprises the following steps of: heating and reacting 0.2 mmol and 1.0 equivalent weight of amide compound and 0.6 mmol and 3.0 equivalent weight of bromo-ethyl difluoroacetate for 24 hours under an oil bath condition of 90 DEG C to generate an experimental reactant; concentrating the experimental reactant under reduced pressure to obtain a residue; and purifying the residue by silica gel rapid column chromatography to obtain the target product nitrile compound. According to the scheme, the process reaction conditions are mild, a strict anhydrous and anaerobic environment is not needed, the harsh requirements on equipment and operation are greatly reduced, and the production safety and practicability are improved. Acetone is used as a solvent, so that high-efficiency reaction can be realized, the solvent after reaction is convenient to recycle and recycle, the production cost and the environmental burden are remarkably reduced, and the remarkable green chemical engineering characteristic is embodied.

The invention provides a preparation method and application of an all-solid-state lithium ion battery, the all-solid-state lithium ion battery comprises a positive electrode, a negative electrode and a solid electrolyte, and the preparation method comprises the following steps: adding an interface modifier into raw materials of the positive electrode and / or the solid electrolyte, the fluoro anhydride is selected from at least one of difluoroacetic anhydride, trifluoroacetic anhydride, pentafluoropropionic anhydride or heptafluorobutyric anhydride. According to the preparation method and application of the all-solid-state lithium ion battery provided by the invention, the interfacial compatibility of the solid electrolyte with the positive electrode and the negative electrode can be remarkably improved, and the cycle performance of the high-voltage all-solid-state lithium ion battery is improved.

The invention relates to the field of macromolecules, and discloses a method for refining polyetherketoneketone and a polyetherketoneketone refined product. The method comprises the following steps: (1) treating a polyetherketoneketone complex by adopting a pretreatment agent; (2) the polyether ketone ketone crude product and a mixed chain supporting solution are mixed and washed, a first product is obtained, the mixed chain supporting solution comprises a main chain supporting agent and a cosolvent, the main chain supporting agent comprises one or more selected from parachlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid, the cosolvent comprises one or more selected from N, N-dimethylformamide and dimethyl sulfoxide, and the main chain supporting agent comprises one or more selected from dichlorophenol, trifluoroacetic acid, difluoroacetic acid, dichloroacetic acid and chloroacetic acid. The solvent is one or more of water, N-methyl pyrrolidone and N-methyl formamide; (3) adding a mixed aqueous solution into the first product to remove at least part of metal ions to obtain a second product; and (4) washing the second product for multiple times by using an organic solvent, and washing and drying to obtain the refined polyether ketone ketone. The content of aluminum ions in the polyetherketoneketone prepared by the method is low.

The invention discloses a fluorine-containing medical intermediate ethyl difluoroacetate and a preparation method thereof, and belongs to the technical field of synthesis of organic fluorine compounds. The method comprises the following steps: firstly, taking tetrafluoroethylene and ethanol as raw materials, and reacting under the action of a basic catalyst to prepare an intermediate 1, 1, 2, 2-tetrafluoroethyl ether with stable properties; and then gasifying the intermediate, and performing catalytic cracking through a modified gamma-aluminum oxide catalyst bed layer subjected to specific high-temperature pre-fluorination treatment under the mild condition of 160-190 DEG C to generate high-activity difluoroacetyl fluoride in situ, and finally, directly introducing the cracking gas containing difluoroacetyl fluoride into a low-temperature reaction solution containing ethanol and an acid-binding agent without separation, and carrying out esterification reaction. According to the method, a brand-new synthesis route and a special catalyst are adopted, reaction conditions are mild, the cracking step selectivity is high, the production efficiency and the total yield are remarkably improved through integrated process design, and the technological process is simple, safe and reliable.

An electrolyte, a secondary battery, and an electronic device. The electrolyte comprises ethyl 2,2-difluoroacetate, 1,2,3-tris(2-cyanoethoxy)propane, and 1,3-propane sultone. Based on 100 parts by mass of the electrolyte, ethyl 2,2-difluoroacetate accounts for 1.5 to 6 parts by mass, 1,2,3-tris(2-cyanoethoxy)propane accounts for 0.5 to 4 parts by mass, and 1,3-propane sultone accounts for 1 to 5.5 parts by mass. The overcurrent and overtemperature safety of secondary batteries are improved.

The invention relates to the technical field of batteries, and provides a battery, which comprises a pole piece and an electrolyte, the electrolyte comprises ethyl difluoroacetate, lithium bis (trifluoromethylsulfonyl) imide and lithium hexafluorophosphate; the mass ratios of the ethyl difluoroacetate and the lithium bis (trifluoromethylsulfonyl) imide in the electrolyte are respectively recorded as a% and b%; 20.2 < = a < = 75.1; 0.5 < = b < = 12; the pole piece comprises a current collector, a first layer and a second layer, the second layer is located between the current collector and the first layer, and the thickness of the first layer is 1-15 nm; the second layer is an active material layer; the pole pieces comprise a positive pole piece and a negative pole piece; the second layer of the negative plate comprises a silicon-based material; the first layer of the negative plate comprises elements N and P, the content ratio of the elements N to P is c, and c is more than or equal to 0.015 and less than or equal to 60; the first layer of the positive plate comprises elements F and S, the content ratio of the elements F to S is d, d is larger than or equal to 5 and smaller than or equal to 80, and the needling safety performance and the cycle performance of the battery can be improved.

The invention discloses a method for preparing triphenyl sulfonium salt containing a ketal structure and purifying an isomer of the triphenyl sulfonium salt, which comprises the following steps: S1, carrying out condensation reaction on sodium difluoroacetate sulfonate and keto-containing alcohol to obtain keto-containing sodium difluorosulfonate acetate; s2, enabling the keto-containing sodium difluorosulfonate acetate to react with triphenyl sulfur chloride, so as to obtain keto-containing triphenyl sulfonium salt; s3, the keto-containing triphenyl sulfonium salt and D-ketonic acid lactone are subjected to a reaction, and a mixed product containing a ketal structure triphenyl sulfonium salt isomer is obtained; s4, dissolving the mixed product in C1-C4 fatty alcohol, cooling, crystallizing, filtering and drying to obtain a purified product; the content of the cis-triphenylsulfonium salt containing the ketal structure in the purified product is 95% or above. The obtained triphenyl sulfonium salt containing the ketal structure is stable in structure and good in solubility, the purity of the product is improved through C1-C4 fatty alcohol and a cooling crystallization method, and the problem of insufficient purity caused by poor batch stability in a synthesis process is effectively solved.

An electrolyte. The electrolyte comprises a fluorine-containing ester additive. The ratio of the fluorine-containing ester additive in the electrolyte is 2-9% by mass percentages. The fluorine-containing ester additive comprises 2,2-difluoroethyl acetate, difluoroethylene carbonate and trifluoroethyl methyl carbonate.

This invention provides a battery and an electrical device, including a positive electrode sheet comprising a positive electrode active material, the positive electrode active material being doped with and / or coated with aluminum; a negative electrode sheet comprising a negative electrode active material, the negative electrode active material comprising silicon particles; an electrolyte comprising a first solvent, a second solvent, a first additive, a second additive, and a third additive; the first solvent comprising ethyl 2,2-difluoroacetate, the second solvent comprising propylene carbonate, the first additive comprising 1,3-propanesulfonate lactone, the second additive comprising vinyl sulfate, and the third additive comprising succinate; this invention, through the synergistic design of a full battery system of "aluminum-modified positive electrode + silicon-based negative electrode + multifunctional composite electrolyte," achieves excellent low-temperature discharge performance, ultra-long cycle life, high interface stability, and outstanding thermal safety characteristics while maintaining high energy density.

This invention provides a battery and an electrical device, comprising a positive electrode sheet including a positive active material, the positive active material being doped with and / or coated with aluminum; a negative electrode sheet including a negative active material, the negative active material including silicon particles; and an electrolyte including a first solvent, a second solvent, a first additive, and a second additive; the first solvent including ethyl 2,2-difluoroacetate, the second solvent including a chain-like fluorosulfonamide compound, the first additive including mannitol carbonate sulfate, and the second additive including fluoroethylene carbonate. This invention, through the introduction of aluminum into the positive active material, the use of silicon particles in the negative active material, and the synergistic design with the multi-component solvent and additives in the electrolyte, achieves a comprehensive improvement in the battery's cycle performance, interface stability, and safety, making it particularly suitable for high-energy-density lithium-ion battery applications.

The invention belongs to the technical field of electrolytes, and particularly discloses a flame-retardant low-temperature-resistant high-voltage high-entropy electrolyte for a lithium metal battery, a preparation method of the electrolyte and the battery. Solvents of the electrolyte comprise fluoroethylene carbonate, methyl trifluoroethyl carbonate, ethyl difluoroacetate, methyl trifluoroacetate and ethoxypentafluorocyclotriphosphazene; the volume ratio of the fluoroethylene carbonate to the methyl trifluoroethyl carbonate to the ethyl difluoroacetate to the methyl trifluoroacetate to the ethoxypentafluorocyclotriphosphazene is (1-5): (2-6): (2-6): (2-6): (0.5-1.5), and the concentration of the lithium hexafluorophosphate is 0.5-1.5 mol / L. The electrolyte has good high voltage tolerance, allows a ternary positive electrode (NCM 811) to operate at a high cut-off voltage of 4.8 V, has good low temperature tolerance, and allows a commercially feasible lithium metal battery to show good cyclicity at-20 DEG C.

The invention relates to the technical field of batteries, and discloses a battery, which comprises a battery cell, a shell and an electrolyte, the battery cell comprises a negative electrode plate, the negative electrode plate comprises a negative electrode current collector and a negative electrode active material layer, and the negative electrode active material layer comprises a silicon-based material; the shell comprises a first side wall, the first side wall comprises a first part and a second part, the second part is connected to the first part, the second part is located at least one end of the extension direction of the first side wall, and the first part is sunken towards one side close to the battery cell relative to the second part; the electrolyte comprises a fluorine-containing compound, and the fluorine-containing compound comprises at least one of ethyl difluoroacetate and fluoroethylene carbonate; the concave distance T of the first part relative to the second part is greater than or equal to 0.1 mm and less than or equal to 0.8 mm; the mass ratio c of the silicon element in the negative electrode active material layer is 1.5%-50%; and based on the total mass of the electrolyte, the mass ratio A of the fluorine-containing compound is 8-70%. The invention has the effects of preventing shell corner breakage and prolonging the cycle life of the battery.

The invention discloses a preparation method of 1-(3, 5-difluoro-2-hydroxybenzene) ethyl-1-ketone, which comprises the following steps: (1) taking a compound (III) 2, 4-difluorophenol as an initial raw material, and carrying out substitution reaction on the compound (III) 2, 4-difluorophenol and acetyl chloride to generate a compound (II) 2, 4-phenyl difluoroacetate; and (2) carrying out an intramolecular Friedel-Crafts reaction on the compound (II) 2, 4-phenyl difluoroacetate to prepare a compound (I), namely the 1-(3, 5-difluoro-2-hydroxybenzene) ethyl-1-ketone. Compared with a traditional method, the preparation method disclosed by the invention has the following advantages: firstly, reaction conditions are mild, and dangerous chemical reactions are not involved; 2, the operation is simple, complicated purification modes such as column chromatography are avoided, and kilogram-level preparation is facilitated; 3, the raw materials are cheap and easy to obtain, the cost is lower, the steps and atom economy are better, and efficient synthesis economics is met; and 4, the total yield is high, and the method has great economic value.

This application relates to a battery and an electrical device. The battery includes a positive electrode, a negative electrode, a separator, and an electrolyte; the positive electrode active material layer includes aluminum; the separator includes an oxide solid electrolyte coating; the electrolyte includes a solvent, an additive, and a lithium salt; the solvent includes a first solvent and a second solvent; the additive includes a first additive and a second additive; the first solvent includes propylene carbonate and / or ethylene carbonate, and the second solvent includes ethyl 2,2-difluoroacetate and / or trifluoroethyl methyl carbonate; the first additive includes mannitol sulfate, and the second additive includes ethylene sulfate; 0.08≤(A+C+D)×10000 / X≤0.77; 0.05≤(C+D)×100 / (B+W)≤2.77; 3.23≤(C+H) / B≤63.97. The solution provided in this application results in a battery exhibiting excellent thermal shock safety and high and low temperature cycling performance.

The invention discloses a characterization method for post-translational modification of a GLP-1 drug containing an Fc fragment, belongs to the field of biological medicines, and is used for separating post-translational modification variants of drugs such as dulatide and Esupaglutide alpha. The method relates to reversed-phase liquid chromatography-tandem mass spectrometry in which a certain proportion of difluoroacetic acid is added into a mobile phase, and key quality evaluation indexes or identification indexes comprise 62181 Da (-380 Da) (corresponding to DesHGEG shearing) in a mass spectrum of a back peak 1 of dulatide, 59464 Da (-3125 Da) in a mass spectrum of a front peak 1 of Esupaglutide alpha, 58012 Da (-4577 Da) in a mass spectrum of a front peak 2 of Esupaglutide alpha, and the like, wherein the 52181 Da (-380 Da) and the 58012 Da (-4577 Da) respectively correspond to K28 / K46 truncation. The method has the advantages of high sensitivity, high resolution, wide applicability and the like, and enables the previous unanalyzed dulatide and Esupaglutide alpha post-translational modification to be clearly characterized.

The utility model relates to the technical field of chemical equipment, in particular to a rectification device for 2-(1-acetyl-6-fluoro-1H-indazole-5-yl)-2, 2-ethyl difluoroacetate, which comprises a rectification tower and the like. A heating device is arranged at the bottom end of the rectifying tower, a rectifying pipe is connected to the top end of the rectifying tower, a condenser is connected to the other end of the rectifying pipe, a water inlet pipe is connected to the upper end of the condenser, a return pipe is connected to the lower end of the condenser, and a condensing pipe is mounted in the condenser. According to the utility model, the consumption of water resources is greatly reduced by recycling the cooling water, and the contact area between the condensation pipe and the cooling water is increased by combining with the spiral condensation pipe, so that the heat exchange efficiency is enhanced.

The invention discloses a preparation method of an alkynyl bicyclo [3.1. 1] heptane difluoroacetate compound in the technical field of organic synthesis, which comprises the following steps: by taking terminal alkyne, [3.1. 1] propeller alkane and gem-difluorobromoacetate as initial raw materials, under the condition that the stoichiometric copper acetylacetonate and 1, 8-diazabicyclo [5.4. 0] undec-7-ene (DBU) are taken as alkalis and acetonitrile is taken as a solvent, carrying out a reaction on the initial raw materials to prepare the alkynyl bicyclo [3.1. 1] heptane difluoroacetate compound. The reaction is carried out through a one-pot method. The process comprises the following key steps: firstly, generating high-activity gem-difluoroacetate free radicals from gem-difluorobromoacetate; the free radical and high-tension [3.1. 1] propeller alkane are subjected to ring-opening addition, ring tension is released, and a new carbon center free radical intermediate is generated; the intermediate is then captured by alkynyl copper species generated in situ, and finally a target product is obtained through reduction elimination. The method is mild in reaction condition and wide in substrate universality, the problems of tedious synthesis steps and low efficiency in the prior art are solved, and a novel and efficient way is provided for preparation of the important molecules.

The invention discloses a synthesis method of a photoacid generator intermediate, which comprises the following steps: adding ethyl brominated difluoroacetate into a mixed solution of Na2S2O4 and triethylamine, stirring for reaction, and performing dot-plate central control reaction; adding hydrogen peroxide, stirring for reaction, and performing point-plate central control reaction; after sodium hydroxide is added for stirring reaction, concentrated sulfuric acid is added for stirring reaction, and 2, 2-difluoro-2-sulfonyl acetic acid is obtained. According to the invention, ethyl brominated difluoroacetate is used as a reaction substrate, so that the price is low; the synthesis route is simple, and the risk of highly toxic by-products is avoided; the reaction can be centrally controlled and thoroughly carried out, the yield is high, purification is convenient, the product purity is high, and large-scale production can be realized; the problems that in the prior art, a synthetic route has highly toxic by-products, the yield is low, the route is complex, and the cost is high are solved.

The application discloses a method for preparing difluoromethyl compounds by using a photocatalytic LMCT strategy and belongs to the technical field of catalytic synthesis, in particular to a method for preparing difluoromethyl compounds by using a photocatalytic LMCT strategy. The application solves the problems of the existing synthesis method, such as being too complicated, needing pre-activation and a stoichiometric oxidant. The method comprises the following steps: adding olefin compounds, difluoroacetic acid, 2,4,6-triisopropylbenzenethiol and Fe(acac)3 into a solvent to obtain a reaction mixed solution, irradiating the reaction mixed solution by using an LED light source under room temperature and in an inert gas atmosphere, and obtaining difluoromethyl compounds. The application embodies the green reaction and the mild reaction. The method is very simple to operate, various raw materials are commercially available, olefins are easy to prepare, and the reaction can be efficiently realized by using a catalytic amount of a cheap metal catalyst through a one-pot method, so that the method has potential industrial application value. The application can be applied to the field of organic synthesis.

This invention relates to the field of organic synthesis, specifically to a method for the preparation of difluoroenones and their in-situ reaction with amines, alcohols, etc., to convert them into the corresponding difluoroacetamides and difluoroacetic acid esters. The invention involves sequentially adding potassium fluoride, an amine or alcohol, and a difluorobromoacrylsilyl compound to a reaction solvent under a nitrogen atmosphere to obtain a mixture. This mixture is stirred at 25°C until the reaction is complete, filtered, and purified to obtain the difluoroacetamide or difluoroacetic acid ester compound. The preparation method of this invention is simple to operate (highly reactive difluoroenones are generated in situ and participate in the reaction), achieving efficient synthesis of difluoroacetamide / difluoroacetic acid esters and avoiding the use of highly volatile difluoroacetyl chloride. The difluorobromoacrylsilyl used in this invention can be conveniently prepared on a large scale and can be purified by distillation. The reaction conditions involved in the preparation method of this invention have good substrate tolerance and can be applied to aliphatic amines, aromatic amines, and various primary and secondary alcohols.