176results about "Nitrosyl chloride" patented technology

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 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 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.

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 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.

The application discloses a preparation method of lithium bisfluorosulfonimide, and aims to provide a preparation method of lithium bisfluorosulfonimide by using easily separated N-alkyl bisfluorosulfonimide instead of ammonium salt of lithium bisfluorosulfonimide, and lithium salt, wherein the preparation steps are short, the whole separation and purification process is simple and easy to implement, and the danger degree of materials is relatively low. The technical scheme is as follows: N-alkyl bisfluorosulfonimide and alkaline lithium salt are used as raw materials, and reaction is carried out in an organic solvent A at room temperature to obtain the product; and the application relates to the technical field of new energy.

The invention relates to the technical field of bis (fluorosulfonyl) imide organic amine salt, in particular to a bis (fluorosulfonyl) imide organic amine salt treatment system and a bis (fluorosulfonyl) imide organic amine salt treatment method. The bis (fluorosulfonyl) imide organic amine salt treatment system comprises decolorizing equipment and regeneration equipment, the decolorizing equipment comprises a shell and an adsorption assembly, the shell is provided with a containing space, a feeding port and a discharging port, the feeding port and the discharging port are communicated with the containing space, and the adsorption assembly is arranged in the containing space; and the regeneration equipment is communicated with the accommodating space and is set as cleaning medium providing equipment of the adsorption assembly. According to the decolorizing equipment, the chromaticity of a material containing imidodisulfuryl fluoride organic amine salt is reduced, and the purity is improved; the regeneration equipment cleans the adsorption assembly, and cyclic utilization of the adsorption assembly is achieved.

The application discloses a method for removing fluorosulfonic acid in bisfluorosulfonylimide, and the method comprises the following steps: reacting crude bisfluorosulfonylimide containing fluorosulfonic acid with inorganic acid salt or organic acid salt, and distilling the reaction product to remove fluorosulfonic acid in the bisfluorosulfonylimide. The application effectively solves the problem that fluorosulfonic acid is difficult to be completely removed in the prior art, and has the advantages of simple operation, low cost, high efficiency and good effect.

The invention belongs to the technical field of lithium ion battery electrolyte, and particularly relates to a method for jointly preparing bis (fluorosulfonyl) imide and monofluorophosphate. The preparation method comprises the following steps: reacting urea, chlorosulfonic acid and phosphorus pentafluoride serving as raw materials to generate a mixture of bis (fluorosulfonyl) imide acid and monofluorophosphoric acid, distilling to remove HCl and PF5 impurities in the mixture, and reacting the mixture with alkali metal salt under the poor solvent condition of monofluorophosphate to obtain a solid-liquid mixture; and carrying out solid-liquid separation on the solid-liquid mixture, and drying the obtained solid to obtain monofluorophosphate, and concentrating the obtained filtrate, adding a poor solvent for recrystallization, filtering and drying to obtain the bis (fluorosulfonyl) imide salt. According to the method, two acids can be synthesized through one-step reaction, the synthesis process flow is simple, the reaction time is short, the production efficiency can be remarkably improved, and the production cost is saved. And the prepared monofluorophosphate and bis (fluorosulfonyl) imide salt are high in quality and can be widely applied to lithium ion battery electrolyte.

This invention relates to a method for preparing lithium bis(fluorosulfonyl)imide, comprising the following steps: reacting bis(fluorosulfonyl)imide and phenolic lithium in an organic solvent to obtain a reaction solution containing lithium bis(fluorosulfonyl)imide, followed by post-treatment to obtain lithium bis(fluorosulfonyl)imide. This invention selects phenolic lithium as the lithium source, reacting it with bis(fluorosulfonyl)imide in an organic solvent. The phenol generated in the reaction is soluble in the organic solvent, while the lithium bis(fluorosulfonyl)imide is insoluble in the selected organic solvent. This solves the problem of synthesizing lithium bis(fluorosulfonyl)imide in aqueous or relatively hazardous systems. The prepared lithium bis(fluorosulfonyl)imide has a purity of over 98.7% and a yield of over 86%. The preparation method of this invention is simple to operate, and subsequent purification is convenient, featuring environmental friendliness and high efficiency, meeting the needs of industrialization.

This application belongs to the field of chemical technology. It provides a method for purifying bis(fluorosulfonyl)imide, as well as the purified bis(fluorosulfonyl)imide and its salt. The purification method includes: reacting the bis(fluorosulfonyl)imide to be purified with a decontaminating agent to obtain a mixture; the decontaminating agent includes a resin with a nitrogen-containing aromatic ring group; the bis(fluorosulfonyl)imide to be purified includes fluorosulfonic acid; and separating the mixture to obtain purified bis(fluorosulfonyl)imide. The decontaminating agent provided in this application contains a resin with a nitrogen-containing aromatic ring group. This resin reacts with fluorosulfonic acid to ultimately form an ammonium fluorosulfonate salt. The fluorosulfonic acid is chemically adsorbed onto the resin with the nitrogen-containing aromatic ring group, thus facilitating the separation of fluorosulfonic acid and bis(fluorosulfonyl)imide without introducing new anionic impurities.

The utility model discloses crystallization equipment. The crystallization equipment comprises a rotating shaft and a spiral blade, the spiral blade is arranged on the side wall of the rotating shaft and spirally extends in the axial direction of the rotating shaft, the spiral blade is provided with a cooling channel, a material channel and a heating channel, and the cooling channel, the material channel and the heating channel are sequentially arranged in the thickness direction of the spiral blade. And a plurality of liquid drainage holes are formed in one side, far away from the rotating shaft, of the spiral blade. Materials are firstly cooled through a cooling medium in the cooling channel, the materials are condensed into crystals, and the rotating shaft is rotated to discharge mother liquor through the liquid discharge hole. Then the materials are heated through a heating medium, after the temperature rises to a certain degree, the perspiration liquid is changed into a liquid state, the rotating shaft is rotated, the perspiration liquid is discharged through a liquid discharging hole, and refining of bis (fluorosulfonyl) imide is achieved. The utility model also discloses a preparation system for the lithium bis (fluorosulfonyl) imide.

The application relates to a purification method of a bifluorosulfonylimide lithium salt, comprising the following steps: modifying a polytetrafluoroethylene film by using plasma and formic acid, immersing the polytetrafluoroethylene film in bifluorosulfonylimide acid after the modification is completed, heating and drying to obtain a modified polytetrafluoroethylene film; dispersing lithium carbonate in dimethyl carbonate, then adding bifluorosulfonylimide acid, obtaining a reaction liquid after the reaction is completed, filtering the reaction liquid to obtain a filtrate, concentrating the filtrate once to obtain a bifluorosulfonylimide lithium electrodialysis crude solution; using the modified polytetrafluoroethylene film to purify the bifluorosulfonylimide lithium electrodialysis crude solution by electrodialysis, then concentrating and crystallizing the obtained electrodialysis liquid to obtain battery-grade bifluorosulfonylimide lithium. The method provided by the application can reduce the purity requirement of raw material lithium carbonate from battery grade to industrial grade, which is beneficial to industrial production.