450results about "Nitrosyl chloride" patented technology

The invention belongs to the technical field of preparation of lithium bis (fluorosulfonyl) imide, and particularly relates to a preparation method of lithium bis (fluorosulfonyl) imide, which comprises the following steps: step 1, reacting chlorosulfonic acid with chlorosulfonyl isocyanate under the action of a first catalyst to generate bis (fluorosulfonyl) imide; 2, hydrogen fluoride gas is introduced into the bis (chlorosulfonyl) imide generated in the step 1, and bis (fluorosulfonyl) imide is obtained under the action of a first catalyst; and 3, adding a first lithium salt into an organic solvent, adding the imidodisulfuryl fluoride obtained in the step 2 in the stirring process, and carrying out ion exchange to obtain the lithium imidodisulfuryl fluoride. According to the invention, the conversion rate is high, the usage amount of the catalyst is reduced, the steps are simplified, and the yield is further improved.

Methods for making high-purity LiFSI salts and intermediate products using one, the other, or both of a reactive-solvent removal / replacement method and an LiFSI purification method. In some embodiments, the reactive-solvent removal / replacement method includes using non-reactive anhydrous organic solvents to remove and / or replace one or more reactive solvents in a crude LiFSI. In some embodiments, the LiFSI purification method includes using anhydrous organic solvents to remove impurities, such as synthesis impurities, from a crude LiFSI. In some embodiments, crude LiFSI can be made using an aqueous-based neutralization process. LiFSI salts and products made using methods of the disclosure are also described, as are uses of such salts and products and electrochemical devices that include such salts and products.

The invention discloses hydrogen fluoride, a preparation method thereof and a battery material. The preparation method of hydrogen fluoride comprises the steps that fluosilicic acid and first sulfuric acid react to generate mixed gas and first mixed sulfuric acid, the first mixed sulfuric acid is a sulfuric acid solution containing hydrogen fluoride, and the mixed gas comprises silicon tetrafluoride gas and hydrogen fluoride gas; washing the mixed gas with second sulfuric acid to obtain second mixed sulfuric acid and washed silicon tetrafluoride gas; the second mixed sulfuric acid is obtained by absorbing the hydrogen fluoride gas by second sulfuric acid; washing the water-containing hydrogen fluoride with second mixed sulfuric acid to obtain crude hydrogen fluoride gas; and purifying the crude hydrogen fluoride gas to obtain anhydrous hydrogen fluoride. According to the preparation method of the hydrogen fluoride, through washing treatment of the second sulfuric acid and washing treatment of the second mixed sulfuric acid, the recovery rate of the hydrogen fluoride is remarkably increased.

The invention provides a bis (fluorosulfonyl) imide metal liquid salt and a preparation method thereof, and the preparation method comprises the following steps: reacting bis (fluorosulfonyl) imide with a fluorinated metal compound to obtain a molten reaction liquid, and carrying out devolatilization treatment on the reaction liquid until the EP1 acidity (calculated as HF) is less than or equal to 0.5 ppm to obtain a bis (fluorosulfonyl) imide compound, the preparation method comprises the following steps: dissolving difluorosulfonylimide in a solvent, and carrying out resin deacidification treatment to obtain difluorosulfonylimide metal liquid salt at a heating temperature of lower than 140 DEG C. The invention further discloses a preparation method of the difluorosulfonylimide metal liquid salt. The purity of the molten-state imidodisulfuryl fluoride metal liquid salt prepared through the preparation method of the imidodisulfuryl fluoride metal liquid salt is high, and the method has the advantages of being high in preparation efficiency and low in cost.

The present invention relates to a process for preparing lithium bis(fluorosulfonyl)imide, comprising the following steps of: contacting of bis(fluorosulfonyl)imide with a lithium base in a solvent selected from carbonates, ethers and nitriles, to obtain a mixture comprising lithium bis(fluorosulfonyl)imide and water; diafiltration of the mixture on a nanofiltration membrane so as to obtain, firstly, a concentrate enriched in lithium bis(fluorosulfonyl)imide and depleted in water and, secondly, a permeate depleted in lithium bis(fluorosulfonyl)imide and enriched in water. The present invention also relates to a process for preparing an Li-ion battery electrolyte.

The invention provides lithium fluoride as well as a preparation method and application thereof. The mass content of carbonate in the lithium fluoride is less than or equal to 1000mg / kg; d10 of the lithium fluoride is smaller than or equal to 10 microns, D50 of the lithium fluoride is smaller than or equal to 20 microns, and the bulk density of the lithium fluoride is 0.9-1.2 g / cm < 3 >. The lithium fluoride provided by the invention has a specific size specification and relatively low carbonate impurity content, and the lithium fluoride is beneficial to preparation of electrolyte salt capable of improving the electrical performance of a battery.

The present invention relates to a method for preparing lithium bis(fluorosulfonyl)imide, the method comprising the steps of: contacting the bis(fluorosulfonyl)imide with a lithium base in a solvent selected from carbonates, ethers, and nitriles to obtain a mixture comprising lithium bis(fluorosulfonyl)imide and water; Diafiltering the mixture through a nanofiltration membrane to obtain first a lithium bis(fluorosulfonyl)imide-enriched, water-depleted concentrate and then a lithium bis(fluorosulfonyl)imide-depleted, water-enriched permeate. The present invention also relates to a method for producing an electrolyte for a Li-ion battery.

In order to solve the problem of safety risk and high residual potassium content in existing methods for preparing sodium fluorosulfonyl imide or lithium fluorosulfonyl imide from potassium fluorosulfonyl imide, the present invention provides a preparation method for a bis(fluorosulfonyl)imide alkali metal salt, comprising the following operation steps: providing an alcohol solution of an alkali metal salt XFSI; providing a cation exchange resin column, the cation exchange resin column being filled with a strongly acidic cation exchange resin, and the strongly acidic cation exchange resin adsorbing second alkali metal ions Z; and performing ion exchange: introducing the alcohol solution of the alkali metal salt XFSI into the cation exchange resin column for ion exchange, replacing first alkali metal ions X on the alkali metal salt XFSI with the second alkali metal ions Z to obtain an alcohol solution containing an alkali metal salt ZFSI, and purifying to obtain the alkali metal salt ZFSI. The preparation method provided by the present invention involves simple operations and has high safety, the purity of the obtained alkali metal salt ZFSI is high, and the purification difficulty is effectively reduced.

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 present invention discloses a method for heterogeneous catalytic synthesis of a key intermediate of a lithium bis(fluorosulfonyl)imide electrolyte (chemical name: bis(chlorosulfonyl)imide). The heterogeneous catalytic method comprises: reacting chlorosulfonic acid with chlorosulfonyl isocyanate under the action of a heterogeneous catalyst, filtering the catalyst directly after the reaction is completed, and directly applying it to the next batch of synthetic reactions, filtering the mother liquor and performing vacuum distillation to collect the target intermediate bis(chlorosulfonyl)imide fraction. Compared with the prior art, the present invention has the advantages of reusable catalyst, less residual waste, low cost, extremely high industrial application value, and is also in line with the upgrading of the green chemical industry alternative industry.

The present invention belongs to the technical field of compound preparation, and specifically relates to a method for preparing sodium bis(fluorosulfonyl)imide, which comprises at least the following steps: the first step is to add anhydrous formic acid to chlorosulfonic acid isocyanate, and stir the reaction to prepare chlorosulfonamide; the second step is to add an organic solvent to the chlorosulfonamide prepared in the first step, and then add sodium fluoride, and then add sulfuryl chloride in batches, and stir the reaction after the feeding is completed; the third step is to filter the reaction product obtained in the second step, remove the filter residue, and concentrate the filtrate under reduced pressure to remove the solvent to obtain a crude sodium bis(fluorosulfonyl)imide; the fourth step is to dissolve the crude product in a protic solvent for recrystallization, and then filter and dry under reduced pressure to obtain a pure sodium bis(fluorosulfonyl)imide. The process is not only simple to operate, but also has a short reaction time and a high yield, and can effectively control metal ion and anion impurities, and can prepare a high-purity target product of sodium bis(fluorosulfonyl)imide.

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 separation and purification, and provides a purification method of imidodisulfuryl fluoride, purified imidodisulfuryl fluoride and imidodisulfuryl fluoride lithium. The purification method comprises the operation of removing impurities by using an impurity removing agent, wherein the impurity removing agent comprises bis (fluorosulfonyl) imide salt; the purification method comprises the following steps: mixing an impurity removal agent with to-be-purified bis (fluorosulfonyl) imide, and carrying out ion exchange reaction on fluorosulfonic acid in the to-be-purified bis (fluorosulfonyl) imide and bis (fluorosulfonyl) imide salt to obtain a liquid-phase mixture; and carrying out separation treatment on the liquid phase mixture to obtain purified bis (fluorosulfonyl) imide. The molar ratio of the bis (fluorosulfonyl) imide radical to the fluorosulfonate radical is more than 1: 1; in the step of carrying out the ion exchange reaction on the bis (fluorosulfonyl) imide salt and the fluorosulfonic acid, the reaction temperature is controlled to be 20 DEG C or above. The purification method provided by the invention can effectively reduce regeneration impurities.

The invention relates to the technical field of preparation methods of lithium bis (fluorosulfonyl) imide, in particular to a method for continuously preparing lithium bis (fluorosulfonyl) imide, which comprises the following steps: reacting chlorosulfonic acid with chlorosulfonyl isocyanate under the action of a copper complex catalyst to generate bis (fluorosulfonyl) imide; the method comprises the following steps: introducing hydrogen fluoride gas into bis (chlorosulfonyl) imide, and obtaining bis (fluorosulfonyl) imide under the action of an iron complex catalyst; the preparation method comprises the following steps: adding lithium salt into an organic solvent, and adding imidodisulfuryl fluoride in a stirring process to obtain the product imidodisulfuryl fluoride lithium. According to the method, a reaction container does not need to be replaced in different steps, an intermediate product does not need to be separated and purified and then put into the next step of reaction, the product is obtained through direct continuous reaction, and the high yield is kept; in addition, due to the introduction of the copper complex catalyst and the iron complex catalyst, the temperature required by the reaction is further reduced, and the safety of the reaction process is improved while the energy is saved.

A method for purifying an aqueous sulfonylimide solution includes heating an aqueous sulfonylimide solution containing a sulfonylimide compound represented by the general formula (1). A method for producing a non-aqueous electrolyte solution includes adding an electrolyte solution solvent to the aqueous sulfonylimide solution purified by the purification method to dehydrate the aqueous sulfonylimide solution. A method for producing an electrolyte composition includes distilling off the electrolyte solution solvent from the non-aqueous electrolyte solution obtained by the production method.

The invention belongs to the technical field of chemical engineering, and provides a purification method of imidodisulfuryl fluoride, purified imidodisulfuryl fluoride and imidodisulfuryl fluoride salt. The purification method provided by the invention comprises the following steps: reacting to-be-purified imidodisulfuryl fluoride with an impurity removal agent to obtain a mixture; the impurity removing agent comprises resin with nitrogen-containing aromatic ring groups; the bis (fluorosulfonyl) imide to be purified comprises fluorosulfonic acid; and separating the mixture to obtain the purified bis (fluorosulfonyl) imide. The impurity removal agent provided by the invention contains the resin with the nitrogen-containing aromatic ring group, the resin with the nitrogen-containing aromatic ring group can react with the fluorosulfonic acid to finally form the ammonium fluorosulfonate salt, and the fluorosulfonic acid is chemically adsorbed on the resin with the nitrogen-containing aromatic ring group, so that the separation of the fluorosulfonic acid and the bis (fluorosulfonyl) imide is conveniently realized, and the impurity removal efficiency is improved. New anion impurities are not introduced.

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 relates to a monitoring method for a preparation process of bis (fluorosulfonyl) imide metal salt and a preparation method. The monitoring method is used for monitoring the preparation process of synthesizing the bis (fluorosulfonyl) imide metal salt through double decomposition reaction of bis (fluorosulfonyl) imide and metal salt, and comprises the following steps: taking a real-time reaction solution sample of the double decomposition reaction; testing the real-time total mass content W2 of the free acid in the reaction solution sample and the real-time mass content W3 of the free acid HR in the reaction solution sample; according to the initial mass content W1 of the free acid in the imidodisulfuryl fluoride raw material, the real-time total mass content W2 of the free acid in the reaction solution sample and the mass content W3 of the free acid HR in the reaction solution sample, the percentage content X of the mass of the residual imidodisulfuryl fluoride in the reaction solution to the mass of the imidodisulfuryl fluoride raw material is obtained; and judging the preparation process of the bis (fluorosulfonyl) imide metal salt according to the X value. According to the method, the preparation process of the bis (fluorosulfonyl) imide metal salt can be effectively monitored.

The invention relates to a production method of imidodisulfuryl fluoride and a production method of lithium imidodisulfuryl fluoride, the production method of imidodisulfuryl fluoride takes sulfamic acid, chlorosulfonic acid and thionyl chloride as raw materials, imidodisulfuryl fluoride is obtained through chlorination reaction, imidodisulfuryl fluoride and hydrofluoric acid or imidodisulfuryl fluoride and hydrogen fluoride gas are taken as raw materials, imidodisulfuryl fluoride and hydrogen fluoride gas are subjected to chlorination reaction to obtain imidodisulfuryl fluoride. The invention discloses a method for producing bis (fluorosulfonyl) imide, which comprises the following steps: by taking bis (fluorosulfonyl) imide as a raw material, carrying out fluoridation reaction to prepare a bis (fluorosulfonyl) imide crude product, adding metal salt into the bis (fluorosulfonyl) imide crude product, and then carrying out melt crystallization and / or rectification. According to the method, the metal salt is added into the difluorosulfonyl imide crude product, so that the metal salt can react with a light component in a fluorination reaction system or a component with a boiling point similar to that of the target product difluorosulfonyl imide, and the impurities react to generate salt with a relatively high boiling point; therefore, the components can be separated from the target product imidodisulfuryl fluoride in the subsequent purification process, and the purity of imidodisulfuryl fluoride is further improved.

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 provides a bis(fluorosulfonyl)imide impurity removal and purification system and a bis(fluorosulfonyl)imide impurity removal and purification method. The system comprises a light-component stripping tank, a gas-liquid separator, a product buffer tank, an impurity removal reactor, and a film evaporator. The light-component stripping tank is connected to a reaction product liquid supply source. The gas-liquid separator is connected to the light-component stripping tank and also connected to the light-component product recovery device. The product buffer tank is connected to the light-component stripping tank and also connected to the gas-liquid separator. The impurity removal reactor is connected to the product buffer tank and also connected to an impurity removal reactant supply source. The film evaporator is connected to the impurity removal reactor, connected to a gas-phase separation system, and also connected to an impurity collection tank. The bis(fluorosulfonyl)imide impurity removal and purification system and the bis(fluorosulfonyl)imide impurity removal and purification method according to the invention make it possible to remove impurities from bis(fluorosulfonyl)imide continuously and efficiently and purify it.

The invention is applicable to the technical field of lithium ion batteries, and provides a production device and method of lithium bis (trifluorosulfonyl) imide, and the device comprises a raw material buffer tank, a feeding bin, a neutralization kettle, a phase splitting kettle, a dehydration reaction kettle, a three-in-one treatment kettle, a neutralization condenser, a tail gas condenser and a secondary filter, the method mainly comprises a synthesis section, a dehydration section and a product refining section. The equipment is simple in structure, low in investment, convenient to operate and beneficial to industrial popularization; the adopted process is simple and efficient, and isopropyl ether and dichloromethane can be recycled; all impurities generated in the production process are gas and are convenient to separate, so that the obtained lithium bis (trifluorosulfonyl) imide is high in purity.

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.