97results about "Nitrosyl chloride" patented technology

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.

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 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).

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.

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.

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.

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 invention relates to a method of removing one or more target chlorinated impurities from crude bis(fluorosulfonyl)imide mixture containing a hydrogen (bisfluorosulfonyl)imide compound, and the one or more target impurities so as to create a purified mixture by reacting said crude mixture in the molten phase with water or with an aqueous mineral acid.

The present invention relates to a compound of formula (I): TIFF2024504040000020.tif27170 anion and at least one onium cation; The ionic liquid comprises The ionic liquid has a color of less than 115 Hazen units on the APHA scale. The present invention also relates to a method for purifying an ionic liquid comprising an anion of formula (I) and at least one onium cation.

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.

The invention relates to a composition comprising a salt composed of a sodium cation and an anion of formula (II):wherein R1 and R2 independently represent a fluorine atom or a perfluorinated group, the composition having an acetamide content of from 0.1 to 1000 ppm by weight. The invention also relates to a process for preparing this composition and to an electrolyte comprising same.

The invention discloses a method for recovering triethylamine in a preparation process of bis (fluorosulfonyl) imide triethylamine salt, which comprises the following steps: (a) taking sulfuryl fluoride, ammonia gas and triethylamine as raw materials, and reacting in an organic solvent to obtain a reaction solution containing bis (fluorosulfonyl) imide triethylamine salt and triethylamine hydrofluoride; (b) adding a phase transfer catalyst and an inorganic alkaline substance, and carrying out heat preservation reaction; (c) filtering to obtain solid fluoride salt and filtrate; and (d) carrying out vacuum evaporation concentration on the filtrate to obtain a concentrate and a triethylamine-containing recovered solvent, and using the triethylamine-containing recovered solvent for the next batch of reaction. According to the method, under the action of the phase transfer catalyst, the added inorganic alkaline substance reacts with the triethylamine hydrofluoride to generate the solid fluoride salt and dissociate the triethylamine, and the triethylamine can be recovered through vacuum evaporation and concentration, so that the method is simple to operate and convenient for industrial implementation, the triethylamine recovery cost is greatly reduced, and the method is suitable for industrial production. Meanwhile, the wastewater treatment difficulty is also reduced.

A fluorosulfonylimide salt is disclosed. This fluorosulfonylimide salt represented by chemical formula (Ib) of the present invention contains at least one of an impurity represented by chemical formula (IIb), [NS2O5F]2-, and an impurity represented by chemical formula (IIIb), [NS2O6]3-, wherein the content of [NS2O5F]2- is 10,000 ppm or less, and the content of [NS2O6]3- is 10,000 ppm or less (in chemical formula (Ib), M2 is one of Li, Na, K, Ca, Mg, Zn, Sb, Rb, and Cs; and A1 is a fluorine atom, or an alkyl group having 1 to 6 carbon atoms in which at least one hydrogen atom is substituted with a fluorine atom).... chemical formula (Ib) ... chemical formula (IIb) ... chemical formula (IIIb) The fluorosulfonylimide salt according to the present invention can reduce the corrosion of electrolytes, additives, and current collectors.

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.

The present invention relates to a process for the preparation of salts of bis (fluorosulfonyl) imide, preferably lithium bis (fluorosulfonyl) imide (LiFSI).

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.

An MFSI mother liquor, a preparation method therefor and a use thereof are provided. The MFSI mother liquor of the present application comprises MFSI, MFSO3, and a solvent, wherein based on the total weight of the mother liquor, the concentration of MFSI is in a range from 15 wt% to 30 wt%, the concentration of MFSO3 is in a range from 0.5 wt% to 10 wt%, and the concentration of the NH2SO3H is less than or equal to 20 ppm by weight; and wherein the MFSI is bis(fluorosulfonyl)imide salt, and M comprises at least one of K, Na, and Li.

A method for preparing lithium bis(fluorosulfonyl)imide, includes reacting bis(fluorosulfonyl)imide with lithium carbonate in a mixed organic solvent to obtain lithium bis(fluorosulfonyl)imide after post-treatment. In the synthetic route of the lithium bis(fluorosulfonyl)imide, the reaction process stays at the stage of lithium bicarbonate, so there is little water in the reaction system, and it is very easy to recover the generated lithium bicarbonate. The process is simple and can be used to prepare lithium bis(fluorosulfonyl)imide of high quality at a high yield.

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.