257results about "Nitrosyl chloride" patented technology

The invention relates to a preparation method of a bis (fluorosulfonyl) imide salt solution. The preparation method comprises the following steps: S1, mixing a certain A salt and a polar non-aqueous solvent, and dropwise adding bis (fluorosulfonyl) imide for reaction; and S2, after the reaction is completed, adding a salt B into the reaction liquid to remove impurities. Water is not generated in the reaction process, and the imidodisulfuryl fluoride cannot be decomposed to generate corrosive substances; the hydrogenation form of the byproduct salt is insoluble in the non-aqueous solvent and can be recycled through reaction; by adding the salt A and the salt B, trace unfavorable impurities are removed at a time, the requirement for the purity of the raw material imidodisulfuryl fluoride is low, subsequent complex purification processes such as crystallization and drying do not exist, the product can be directly used for preparation of a battery electrolyte after concentration adjustment, large-scale production of the product is facilitated, and the product has good storage stability.

The application provides a preparation method of sodium bisfluorosulfonimide, which comprises the following steps: (1) sulfuryl fluoride and hexamethylsilazane are reacted in an inert atmosphere to obtain a crude product, and the crude product is subjected to gas phase separation to obtain bisfluorosulfonimide; (2) the bisfluorosulfonimide obtained in the step (1) is reacted with sodium fluoride to obtain the sodium bisfluorosulfonimide. The sulfuryl fluoride and the hexamethylsilazane are used as raw materials to prepare the bisfluorosulfonimide by one-step method, the cost is reduced, and the production safety is improved, then the sodium bisfluorosulfonimide is prepared by ion exchange reaction of the bisfluorosulfonimide and sodium fluoride, the three wastes and solvent use are reduced, the impurities are reduced, and the production safety and product quality are improved.

The invention discloses a preparation method of high-purity bis (fluorosulfonyl) imide alkali metal salt. The method comprises the following steps: (1) synthesizing bis (chlorosulfonic acid) imide by taking sulfamic acid, chlorosulfonic acid, thionyl chloride and chlorosulfonic acid isocyanate as raw materials; (2) fluorinating the bis (chlorosulfonic acid) imide by ammonium fluoride to obtain bis (fluorosulfonyl) imide ammonium salt; (3) treating the imidodisulfuryl fluoride ammonium salt solution with a strong acid ion exchange column and concentrating under reduced pressure to obtain imidodisulfuryl fluoride; (4) reacting the alkali metal salt with bis (fluorosulfonyl) imide to obtain bis (fluorosulfonyl) imide alkali metal salt; and (5) carrying out a series of purification processes on the bis (fluorosulfonyl) imide alkali metal salt to obtain the high-purity bis (fluorosulfonyl) imide alkali metal salt. The preparation method has the advantages of mild reaction conditions, low danger coefficient in the technological process, easiness in control, no use and generation of corrosive acid, greenness and environmental protection, and high yield and high purity of the bis (fluorosulfonyl) imide alkali metal salt, and is suitable for large-scale industrial application.

The invention provides a preparation method of liquid-state lithium bis (fluorosulfonyl) imide, and relates to the technical field of organic synthesis.The preparation method comprises the steps that bis (fluorosulfonyl) imide acid, ester substances and a non-aqueous solvent are mixed to form a mixed solution, and lithium carbonate is dropwise added into the mixed solution for a reaction to obtain a liquid-state lithium bis (fluorosulfonyl) imide solution. According to the invention, the imidodisulfuryl fluoride acid and the ester substance are used as raw materials, and the obtained liquid imidodisulfuryl fluoride lithium product does not need to be subjected to additional water removal, so that the quality of the product is improved, and meanwhile, the synthesis process is simple.

The invention provides a bis (fluorosulfonyl) imide alkali metal liquid salt and a preparation method and application thereof, the preparation method comprises the following steps: 1) stirring alkali metal fluoride and a hydrogen fluoride solution at-20-10 DEG C to form a mixed system; 2) adding imidodisulfuryl fluoride into the mixed system, and reacting at 50-120 DEG C to obtain an imidodisulfuryl fluoride alkali metal system; and 3) purifying the bis (fluorosulfonyl) imide alkali metal system to obtain the bis (fluorosulfonyl) imide alkali metal liquid salt, the molar ratio of bis (fluorosulfonyl) imide to the hydrogen fluoride solution to the alkali metal fluoride being 1: (5-10): (0.9-1.05). The preparation method provided by the invention is helpful for obtaining the bis (fluorosulfonyl) imide metal liquid salt with higher purity.

The invention belongs to the technical field of secondary batteries, and particularly relates to a preparation method of bis (fluorosulfonyl) imide salt. The preparation method of the bis (fluorosulfonyl) imide salt provided by the invention comprises the following steps: reacting hydrofluoric acid, alkali metal fluoride and bis (chlorosulfonyl) imide under a closed condition at the temperature of 100 DEG C or above, cooling to 10 DEG C or below after the reaction is completed, carrying out primary filtration to obtain a filter cake, heating to 100 DEG C or above, carrying out secondary filtration to obtain a filtrate, and drying to obtain the bis (fluorosulfonyl) imide salt. And removing impurities to obtain the bis (fluorosulfonyl) imide salt particles or a bis (fluorosulfonyl) imide salt solution. By controlling the reaction temperature and the temperature of two times of filtration after the reaction, the product and impurities are separated by utilizing the crystallization characteristics and solubility of the components in the reaction system at different temperatures, so that the high-purity bis (fluorosulfonyl) imide salt is prepared by a solvent-free one-pot method.

The present invention relates to a process for the preparation of bis(fluorosulfonyl)imide salt (MFSI), which comprises at least a step of reacting ammonium salt of bis(fluorosulfonyl)imide (NHFSI) with fluorine-containing alkoxide. The present invention also relates to a process for the preparation of fluorine-containing alkoxide.

The present disclosure relates to a method for preparing a solid form of the lithium salt of bis(fluorosulfonyl)imide (LiFSI), wherein the solid form of LiFSI salt is extracted from a solution comprising at least one solvent by supercritical anti-solvent extraction. The present invention also relates to the solid form of LiFSI obtained therefrom, as well as the use of such LiFSI in a battery electrolyte.

The present invention relates to a method for producing high-purity cesium bisfluorosulfonylimide to improve stability against the explosion of a battery by forming an effective solid electrolyte interphase (SEI) layer on an electrode surface.

To provide a solid electrolyte for an anode-free metal battery cell.SOLUTION: The present invention relates to a solid-state electrolyte (SSE) for an anode-free metal battery cell, wherein the metal is an alkali metal, an alkaline earth metal or a metal of group Ib, IIb or IIIa of the periodic table, the SSE comprising a non-aqueous solvent, a metal salt of an alkali metal, an alkaline earth metal or a metal of group Ib, IIb or IIIa of the periodic table, an aluminum-based halogenated compound AlXn, and a bis (fluorosulfonyl) imide anion, wherein X is a halogen atom and n is from 1 to 6. The invention further relates to a method of making such an SSE, the method comprising preparing a liquid precursor and exposing the liquid precursor to a temperature between 20 °C and 80 °C to solidify the liquid precursor, thereby obtaining a solid electrolyte.SELECTED DRAWING: Figure 1

A titanium-containing oxide powder which is mainly composed of a titanium-containing oxide represented by Li4Ti5O12 or Ti1-X / 2Nb2O7-X (wherein 0 ≤ X < 2), and which is characterized by containing particles of the titanium-containing oxide and a solvation ionic liquid that is composed of an Li salt and an organic solvent.

The invention belongs to the technical field of electrolyte materials, and discloses a high-purity lithium bis (fluorosulfonyl) imide solution as well as a preparation method and application thereof. The preparation method of the high-purity lithium bis (fluorosulfonyl) imide solution comprises the following steps: 1) mixing inert chloralkane and lithium carbonate to form a suspension, dropwise adding bis (fluorosulfonyl) imide into the suspension at reaction temperature and pressure for reaction, after the reaction is finished, performing filter pressing, washing, and performing filter pressing again to obtain a filter cake; and 2) crushing the filter cake, feeding the crushed filter cake into a closed-loop circulating fluidized bed, sequentially drying in a low-temperature area and a medium-temperature area, instantaneously contacting and dissolving the obtained hot powder with an atomized and sprayed carbonate solvent to form a solution, and performing microfiltration to obtain the high-purity lithium bis (fluorosulfonyl) imide solution. The lithium bis (fluorosulfonyl) imide solution has ultra-high purity and ultra-low moisture, the content of other impurities such as chloride ions, free acids and metal ions is extremely low, additional steps of dehydration, purification or acidity adjustment and the like are not needed, and the lithium bis (fluorosulfonyl) imide solution can be directly used for preparing a high-performance lithium ion battery electrolyte.

The invention relates to a process for the at least partial removal of fluorosulfonic acid and / or derivatives thereof from a crude bis(fluorosulfonyl)imide mixture, containing a hydrogen bis(fluorosulfonyl)imide compound, and fluorosulfonic acid and / or derivatives thereof so as to create a purified mixture by reacting said crude mixture in the molten phase with a halide or sulfate salt.

The present application relates to a preparation method of an alkali metal salt of bis(fluorosulfonyl)imide, comprising the following steps: carrying out a metallization reaction on bis(fluorosulfonyl)imide, an alkali metal halide salt and an acid-binding agent at ≥65 °C without adding an additional solvent to prepare the alkali metal salt of bis(fluorosulfonyl)imide. The acidic gas generated by this method can directly react with the acid-binding agent to form a hydrogen halide organic salt. Through the synergistic effects in multiple aspects, the yield and purity of the alkali metal salt of bis(fluorosulfonyl)imide can be effectively improved; moreover, the raw materials are easily available, the operation is simple, no solvent is required, the reaction conditions are relatively mild, the requirements for equipment in the reaction process and the product are relatively low, and industrial production can be carried out.

The present invention relates to a bis(fluorosulfonyl)imide salt and a method for preparing the same. More specifically, the present invention provides a novel salt of bis(fluorosulfonyl)imide containing 0.01 ppm to 10,000 ppm of a halogenated alcohol. The present invention further relates to a method for producing the salt of bis(fluorosulfonyl)imide, which comprises crystallizing a raw salt of bis(fluorosulfonyl)imide in a crystallization solvent containing at least a halogenated alcohol. Uses of the salt of bis(fluorosulfonyl)imide are also disclosed.

The present invention relates to a method for producing a lithium salt of a bis(fluorosulfonyl)imide.

A method for recovering lithium bis(fluorosulfonyl)imide is provided in the present application. The method of the present application comprises: mixing a slag from lithium bis(fluorosulfonyl)imide production process with a solvent of carbonate ester, to obtain a mixed material; subjecting the mixed material to solid-liquid separation, to obtain a discharged liquid and a solid slag; monitoring the chromaticity of the discharged liquid and comparing the chromaticity of the discharged liquid with a chromaticity reference; recycling the discharged liquid to the mixed material, if the chromaticity of the discharged liquid is higher than the chromaticity reference; and recycling the discharged liquid to lithium bis(fluorosulfonyl)imide production process, if the chromaticity of the discharged liquid is lower than or equal to the chromaticity reference.

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 present invention relates to a method for producing bis(fluorosulfonyl)imide, which is economically feasible at industrial scale and which provides a high-purity product.

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).

The present disclosure relates to a process for purifying the lithium salt of bis(fluorosulfonyl)imide (LiFSI), in which the purified LiFSI is extracted from crude LiFSI through supercritical fluid extraction. The present invention also relates to the purified LiFSI obtained therefrom and the use of such LiFSI in an electrolyte for a battery.

The invention belongs to the technical field of synthesis of bis (fluorosulfonyl) imide, and discloses a method for synthesizing bis (fluorosulfonyl) imide by using sulfuryl fluoride chloride, which comprises the following steps: 1) adding amino sulfuryl fluoride into sulfuryl fluoride chloride for reaction at a reaction temperature; and 2) after the reaction is finished, removing the solvent and unreacted raw materials in the synthetic liquid, and rectifying to obtain the bis (fluorosulfonyl) imide. The byproduct sulfuryl fluoride chloride in the sulfuryl fluoride industry is used as a raw material, the method has the advantages of low cost and high added value, the method is simple to operate, mild in reaction condition and high in conversion rate and yield, and the prepared imidodisulfuryl fluoride is high in purity, good in quality and suitable for large-scale industrial production of imidodisulfuryl fluoride.

The application provides a method for reducing residual solvent of lithium bisfluorosulfonylimide, to solve the technical problems of poor removal effect of residual ester reagent in lithium bisfluorosulfonylimide and low yield in the prior art. The method comprises the following steps: (1) dissolving lithium bisfluorosulfonylimide with residual solvent in a good solvent to prepare a solution; (2) adding a first poor solvent to the solution to prepare a mixed solution; (3) evaporating the good solvent from the mixed solution under negative pressure to obtain a dispersion; (4) filtering the dispersion to remove the poor solvent and obtain a primary product; (5) washing the primary product with a second poor solvent, and filtering the second poor solvent to obtain a secondary product; and (6) performing negative pressure drying treatment on the secondary product. The method can remove the residual ester solvent in lithium salt, realizes the effect of reducing residual solvent, and has high lithium salt yield and is simple and easy to implement.

The present invention relates to a new synthetic pathway for manufacturing bis(halogeno sulfonyl)imide, which are useful intermediates in the synthesis of lithium bis(fluorosulfonyl)imide (LiFSI).

The present invention relates to compositions containing alkali metal salts of bis(fluorosulfonyl)imides and to the use of such compositions in electrolytes for batteries.

In order to overcome the problem of high-temperature decomposition in the existing extraction of lithium bisfluorosulfonylimide from an aqueous solvent system, the present application provides a preparation method of lithium bisfluorosulfonylimide, comprising the following operation steps: providing an aqueous solution of lithium bisfluorosulfonylimide containing an alkaline lithium salt; distilling and concentrating the aqueous solution of lithium bisfluorosulfonylimide to obtain an aqueous concentrated solution of lithium bisfluorosulfonylimide; adding a non-aqueous organic solvent to the aqueous concentrated solution of lithium bisfluorosulfonylimide, distilling water to obtain an organic solution of lithium bisfluorosulfonylimide. In the preparation method of lithium bisfluorosulfonylimide provided by the present application, the addition of an alkaline lithium salt to the aqueous solution of lithium bisfluorosulfonylimide can effectively inhibit the decomposition of lithium bisfluorosulfonylimide during the concentration process, thereby improving the yield and purity of lithium bisfluorosulfonylimide.

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 new synthetic pathway for manufacturing bis(halogeno sulfonyl)imide, which are useful intermediates in the synthesis of lithium bis(fluorosulfonyl)imide (LiFSI).

The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to a preparation method of a Zr2N2X two-dimensional material. The preparation method comprises the following steps: firstly, by taking layered ZrNCl as a working electrode, applying constant current into an electrolyte containing organic ammonium salt, and carrying out electrochemical intercalation reaction to prepare an intercalated ZrNCl two-dimensional nanosheet; and mixing the ZrNCl subjected to electrochemical intercalation treatment with anhydrous Na2X (X = S, Se or Te), carrying out sealed reaction in a protective atmosphere, and carrying out solid-phase topological chemical conversion to generate the Zr2N2X two-dimensional material. Through the synergistic effect of electrochemical intercalation pretreatment and topological chemical conversion, the harsh degree of reaction conditions is reduced, meanwhile, the product quality and the process controllability are comprehensively improved, and a solid foundation is laid for industrial application of the two-dimensional semiconductor material.