30results about "Nitrosyl chloride" patented technology

A method for purifying a sulfimine aqueous solution includes a heating step in which a sulfimine aqueous solution containing a sulfimine compound represented by general formula (1) is subjected to a heating treatment. In a method for producing a nonaqueous electrolyte, an electrolyte solvent is added to the sulfimine aqueous solution purified by the purification method and subjected to dehydration. A method for producing an electrolyte composition includes a step of removing an electrolyte solvent from a nonaqueous electrolyte obtained by the production method by distillation. LiN(RSO2)(FSO2) (R represents a fluorine atom, an alkyl group having 1 to 6 carbon atoms, or a fluoroalkyl group having 1 to 6 carbon atoms.)(1).

This application relates to lithium bis(fluorosulfonyl)imide and a method for purifying lithium bis(fluorosulfonyl)imide. The method includes: providing a mixture containing lithium bis(fluorosulfonyl)imide; adding an organic ammonium salt to the mixture and reacting it to obtain an intermediate mixture; and reacting the intermediate mixture with lithium ions under alkaline conditions to obtain lithium bis(fluorosulfonyl)imide. The method described in this application can improve the purity of lithium bis(fluorosulfonyl)imide.

The present invention relates to a method for removing one or more target impurities, which are chlorides, from a crude bisfluorosulfonylimide mixture containing a hydrogen (bisfluorosulfonyl)imide compound, and to forming a purified mixture by reacting the crude mixture in the molten phase with water or an aqueous solution of an inorganic acid to remove the one or more target impurities.

The application discloses a preparation method of high-stability lithium bisfluorosulfonimide liquid salt, and the method comprises the following steps: uniformly dispersing lithium carbonate in a methyl ethyl carbonate solvent, slowly and dropwise adding bisfluorosulfonimide acid at 10-30 DEG C, and obtaining initial lithium bisfluorosulfonimide liquid salt after the reaction is completed; and removing water from the initial liquid salt through rectification to obtain finished products with water content of less than or equal to 10 ppm. The application adopts lithium carbonate and bisfluorosulfonimide acid as raw materials, and methyl ethyl carbonate as a dispersion medium, and has the advantages of mild reaction conditions, safe and environment-friendly raw materials, no need for high temperature and high pressure, no hydrolysis of the prepared initial liquid salt under high water content conditions, excellent stability, short process, low energy consumption, low production cost, suitability for large-scale industrial production, and wide application of the prepared lithium bisfluorosulfonimide liquid salt in the field of lithium ion battery electrolyte.

This invention discloses an apparatus for the continuous production of bis(fluorosulfonyl)imide intermediates. The apparatus includes a feed mixer with liquid and gas feed ports. The outlet of the feed mixer is connected to the top of a coil reactor via a pipe and is also connected to the inlet of the coil inside the reactor. The outlet of the coil connects from the bottom of the reactor to the top of a separator. A cooling tank is provided outside the coil. The separator has a by-product outlet at the top and a product outlet at the bottom. A steam heater is also provided inside the separator. This apparatus can directly separate the product and by-product, thereby achieving the goal of continuous production of bis(fluorosulfonyl)imide intermediates, increasing production scale and capacity, and ensuring smooth production operation. Furthermore, this apparatus can recover and reuse unreacted raw materials and solvents during the production process, reducing production costs.

The application belongs to the technical field of secondary batteries, and particularly relates to a preparation method of a double-fluorosulfonylimide alkali liquid salt. First, crude double-fluorosulfonylimide acid is added into a low-temperature melting and crystallization device for purification, and the purified double-fluorosulfonylimide acid is obtained through crystallization, sweating and other processes; then the purified double-fluorosulfonylimide acid is reacted with an alkali metal chloride salt in a good solvent at low temperature, and a double-fluorosulfonylimide alkali liquid salt is prepared by using positive pressure filtration. The moisture content of the liquid salt is within 15 ppm, the acidity is within 20 ppm, the chloride ion content is within 2 ppm, the sulfate ion content is within 5 ppm, the sulfamate ion is within 50 ppm, the fluoride ion content is within 12 ppm, and the purity of the liquid salt is above 99.6%. The preparation method of the liquid salt in the application is simple, has low energy consumption and high purity, is suitable for large-scale production, and can be adjusted according to the solvent type of the electrolyte, and is simple and efficient.

A method for recovering raw and auxiliary materials in the production of lithium bis(fluorosulfonyl)imide is described. The method includes one or more different recovery sections A, B, C, D and / or E, corresponding to the recovery and post-treatment of the raw and auxiliary materials such as triethylamine, a fluoride ion, an ester solvent, and a crystallization liquid respectively used in the production of lithium bis(fluorosulfonyl)imide. The method for recovering raw and auxiliary materials of the present application enables the production of lithium bis(fluorosulfonyl)imide to have significantly improved economic efficiency and environmental protection.

The present invention relates to a method for producing bis(fluorosulfonyl)imide acid, which can be economically realized on an industrial scale and from which a high-purity product can be obtained.

The application belongs to the technical field of lithium ion battery electrolyte, and relates to a method and system for continuously preparing high-purity liquid bisfluorosulfonylimide lithium. The application generates molten LiFSI through one-pot reaction of bischlorosulfonylimide, anhydrous hydrogen fluoride and lithium fluoride in a micro-reactor at 80-150 DEG C and 0.5-3.0 MPa; the molten salt is dropped into low-temperature dichloromethane for back extraction and crystallization; the crude product is obtained through continuous filtration, washing and drying; the crude product is dissolved in an ester solvent, and then sequentially subjected to continuous membrane filtration, resin deacidification and deep water removal to obtain high-purity liquid LiFSI product. The method realizes one-pot fluorination, salt formation and full-process continuous production from raw materials to liquid product, has the advantages of high safety, high efficiency, high product purity, stable quality and convenience for large-scale industrial production. In the prepared high-purity LiFSI liquid salt, the water content is less than 10 ppm, the free acid (calculated by HF) is less than 20 ppm, the Cl ‑ 5 ppm, the SO4 2‑ 5 ppm, and the single content of various metal impurity ions (such as calcium, iron, magnesium, sodium and potassium) is less than or equal to 2 ppm.

The present invention relates to a high purity ammonium salt of bis(fluoro sulfonyl)imide (NH4FSI), to a process for its manufacturing and to its use as an intermediate to produce high purity lithium bis(fluorosulfonyl)imide (LiFSI).

The present invention relates to: a lithium bis(fluorosulfonyl)imide (LiFSI) having a sulfamic acid content of 20 ppm by weight or less; a composition comprising same; and a preparation method thereof. The lithium bis(fluorosulfonyl)imide having a sulfamic acid content of 20 ppm by weight or less according to the present invention has the effect of not reducing the room-temperature lifespan and high-temperature lifespan of a lithium secondary battery when used as an electrolyte salt for the battery, and thus can be used in battery manufacturing.

This disclosure relates to lithium-ion conductive materials and methods for purifying the same, and provides a lithium-ion conductive material comprising lithium sulfonylimide represented by the following general formula (I): where X and Y may be the same or different, and each is independently C. m F 2m+1 (m≥0). A method for purifying the aforementioned lithium-ion conductive material is also provided. The method disclosed herein provides high-purity lithium sulfonylimide lithium-ion conductive material.

The application relates to the technical field of electrolyte imine lithium salt material preparation, in particular to a preparation method of low-water high-purity electrolyte imine lithium salt, which comprises the following steps: (1) ammonium fluoride and acetonitrile are added into a reactor, the reactor is sealed and cooled at a temperature of 0-5 DEG C, vacuum is drawn to a negative pressure, then sulfuryl fluoride gas is introduced to normal pressure, a secondary amine with a boiling point of not more than 100 DEG C is added, sulfuryl fluoride gas is continuously introduced to continuously react, the reaction is ended when the reaction pressure in the sealed system does not change any more, and the reaction liquid is subjected to reduced pressure distillation to obtain an intermediate product; (2) under a protective atmosphere, an organic solution containing a secondary amine lithium salt compound is added dropwise into the obtained intermediate product, and a lithiation reaction is carried out while stirring, the reaction is ended after concentration, and the final product lithium bisfluorosulfonylimide is obtained through crystallization under anhydrous conditions, filtration and drying. The lithium bisfluorosulfonylimide obtained by the method has high purity, and the water content is less than 20 ppm.

The invention relates to a process for preparing bis(fluorosulfonyl) imide, comprising the steps of: i) providing a stream A1 containing HF and a reactor containing a liquid phase A2 that contains bis(chlorosulfonyl) imide; ii) in said reactor, bringing said liquid phase A2 into contact with said stream A1 to produce bis(fluorosulfonyl) imide, said process being characterized in that said stream A1 is injected into said liquid phase A2.

The present invention relates to a method for preparing a salt of bis(fluorosulfonyl)imide, preferably lithium bis(fluorosulfonyl)imide (LiFSI).

The present invention relates to a method for producing a carbonate solution of alkali metal or alkaline earth metal bis(fluorosulfonyl)imide, and more particularly to a method for producing alkali metal or alkaline earth metal bis(fluorosulfonyl)imide with a carbonate and a solvent other than the carbonate, and then removing the solvent other than the carbonate to obtain a carbonate solution of alkali metal or alkaline earth metal bis(fluorosulfonyl)imide.

This invention relates to the field of organic chemistry and provides a method for preparing high-purity lithium difluorosulfonylimide liquid salt. The steps include: mixing difluorosulfonylimide with lithium fluoride and reacting, followed by a first filtration to obtain crude lithium difluorosulfonylimide salt; dissolving the crude lithium difluorosulfonylimide salt in a good solvent, adding an acid-removing agent, and then performing a second filtration to obtain lithium difluorosulfonylimide liquid salt; wherein the good solvent is a carbonate solvent; in this invention, difluorosulfonylimide is both a raw material and a reaction solvent, reacting with lithium fluoride at a certain temperature to generate lithium difluorosulfonylimide salt; after the reaction is completed, the crude lithium difluorosulfonylimide salt is obtained by a first filtration; the filtrate obtained after the first filtration of the reaction solution is unreacted difluorosulfonylimide, which can be reused; the preparation method of this invention produces less waste, is economical and environmentally friendly, has a simple process, high yield, and good product quality, and is suitable for industrial production.

A process for producing bis(fluorosulfonyl) imide includes providing a solution comprising fluorosulfonic acid and urea, the solution maintained at a solution temperature from about 0° C. to about 70° C.; reacting the solution in the presence of a reaction medium at a reaction temperature from 80° C. to about 170° C. to produce a product stream including bis(fluorosulfonyl) imide, ammonium fluorosulfate and the reaction medium; separating the ammonium fluorosulfate from the product stream to produce an intermediate product stream; and separating the intermediate product stream into a concentrated product stream and a first recycle stream, the concentrated product stream including a higher concentration of bis(fluorosulfonyl) imide than the first recycle stream.

Provided in the present disclosure are hydrogen fluoride and a preparation method therefor, and a battery material. The preparation method for hydrogen fluoride comprises: reacting fluosilicic acid with first sulfuric acid, so as to generate mixed gas and first mixed sulfuric acid, wherein the first mixed sulfuric acid is a sulfuric acid solution comprising hydrogen fluoride, and the mixed gas comprises silicon tetrafluoride gas and hydrogen fluoride gas; washing the mixed gas with second sulfuric acid, so as to obtain second mixed sulfuric acid and washed silicon tetrafluoride gas, wherein the second mixed sulfuric acid is obtained by absorbing the hydrogen fluoride gas by the second sulfuric acid; washing water-containing hydrogen fluoride with the second mixed sulfuric acid, so as to obtain crude hydrogen fluoride gas; and purifying the crude hydrogen fluoride gas, so as to obtain anhydrous hydrogen fluoride.

The application belongs to the technical field of chemical production equipment, and particularly relates to a stirrer and a reaction kettle. The stirrer comprises a stirring shaft arranged in a vertical direction, a driving mechanism connected to the top end of the stirring shaft, and a plurality of radial stirring paddles arranged on the stirring shaft in a vertical direction. All the radial stirring paddles are arranged in parallel on the stirring shaft in a horizontal direction, and the radii of rotation of adjacent radial stirring paddles gradually increase in a direction away from the driving mechanism. The application avoids problems such as time consumption and labor consumption caused by removing excessive sulfamic acid from a reaction solution by filtration, deposition and other methods.

The present invention relates to a bis(fluorosulfonyl)imide lithium salt (LiFSI) having a methyl sulfate content of 100 ppm by weight or less, a composition comprising same, and a method for preparing same. The lithium bis(fluorosulfonyl) imide having a methyl sulfate content of 100 ppm by weight or less according to the present invention suppresses side reactions occurring on the surface of an electrode and improves the voltage stability of a lithium-ion secondary battery, thereby increasing the lifespan of the battery.

Provided are a liquid bis(fluorosulfonyl)imide metal salt and a preparation method therefor. The preparation method comprises the following steps: reacting a bis(fluorosulfonyl)imide with a fluorinated metal compound, so as to obtain a molten reaction solution; devolatilizing the reaction solution until the EP1 acidity in terms of HF is less than or equal to 0.5 ppm, so as to obtain a bis(fluorosulfonyl)imide compound; and dissolving same in a solvent, and then performing a resin-based deacidification treatment, so as to obtain a liquid bis(fluorosulfonyl)imide metal salt, wherein the heating temperature in the devolatilization treatment is lower than 140°C.

The present invention relates to a method for preparing the sodium salt of bis(fluorosulfonyl)imide (NaFSI).

The present invention provides a solid electrolyte-containing dispersion suitable for forming an oxide-based solid electrolyte layer containing a combination of lithium tetraborate and a lithium salt, which contains finer solid particles while exhibiting excellent stability over time, as well as an all-solid-state lithium-ion secondary battery including a solid electrolyte layer formed using the solid electrolyte-containing dispersion, and a method for manufacturing the same. [Solution] In an all-solid-state lithium-ion secondary battery 10 having a positive electrode layer composed of a positive electrode active material layer 4, a solid electrolyte layer 3 formed using a solid electrolyte-containing dispersion, and a negative electrode layer composed of a negative electrode active material layer 2, the solid electrolyte-containing dispersion contains lithium tetraborate, a lithium salt, a carboxymethylcellulose compound, and water, the water content in the solid electrolyte-containing dispersion is 15 to 68% by mass, and the particle size measured by a particle gauge determined using the solid electrolyte-containing dispersion is 50 μm or less.

The present application provides lithium fluoride, and a preparation method therefor and a use thereof. The mass content of a carbonate in the lithium fluoride is less than or equal to 1000 mg / kg. The lithium fluoride has a D10 of less than or equal to 10 pm, a D50 of less than or equal to 20 pm, and a bulk density of 0.9-1.2 g / cm3.