34results about "Imidodisulfonic/nitrilotrisulfonic acid" patented technology

The invention relates to the field of lithium batteries and lithium capacitors, in particular to a preparation method for difluorosulfimide lithium salt and application of the difluorosulfimide lithium salt. The preparation method for the difluorosulfimide lithium salt, provided by the invention, comprises the following steps: (1) performing fluorination reaction: synthetizing midbody difluorosulfimide from dichlorosulfimide and hydrogen fluoride under the action of a catalyst; (2) performing reaction between the difluorosulfimide obtained in the step 1 and alkaline lithium, and performing solid-liquid separation after the reaction to obtain an LiFSI product. The preparation method for the difluorosulfimide lithium salt, provided by the invention, is low in cost, few in by-product and simple in post-treatment, and the quality and the purity of the product are ensured, therefore the preparation method which is capable of obtaining the high-quality and high-purity product and is economic and practical is provided; the preparation method is suitable for industrial production.

The present invention provides methods for producing bis(fluorosulfonyl) compounds of the formula:

F—S(O)₂—Z—S(O)₂—F  I

by contacting a nonfluorohalide compound of the formula:

X—S(O)₂—Z—S(O)₂—X

with bismuth trifluoride under conditions sufficient to produce the bis(fluorosulfonyl) compound of Formula I, where Z and X are those defined herein.

The invention provides a method for producing hydrogen bis(fluorosulfonyl)imide (HFSI) by reacting hydrogen bis(halosulfonyl)imide (HXSI) with hydrogen fluoride, where each X is independently a nonfluoro-halide, such as Cl, Br, or I.

The invention relates to a preparation method of bifluorosulfonyl imide onium salt. The preparation method comprises the following step: by adopting hydrogen fluoride as a fluorination reagent and a reaction solvent, reacting with dichlorosulfonyl imide and an onium ion halide to obtain bifluorosulfonyl imide onium salt. Therefore, by adopting the preparation method disclosed by the invention, the raw material cost can be reduced, the material consumption and waste generation can be reduced, the raw material utilization rate and the product yield and purity can be improved, products can be more easily purified, a preparation technological process can be simpler and more efficient, and a good technological base for preparing bifluorosulfonyl imide onium salt massively and industrially can be provided.

A fluorination process for obtaining fluorinated compounds including at least one fluorosulfonyl group. More particularly, a process for preparing a fluorinated compound of formula (II), including at least one step of reacting a compound of formula (I) with anhydrous hydrofluoric acid in at least one organic solvent, in which R1 is equal to R2 except in the specific case where R1=Cl, then R2=F, and when R1 is equal to R2, R1 and R2 represent an electron-withdrawing group which has a Hammett parameter op of greater than 0, such as F, CF₃, CHF₂, CH₂F, C₂HF₄, C₂H₂F₃, C₂H₃F₂, C₂F₅, C₃F₇, C₃H₂F₅, C₃H₄F₃, C₃HF₆, C₄F₉, C₄H₂F₇, C₄H₄F₅, C₅F₁₁, C₃F₅OCF₃, C₂F₄OCF₃, C₂H₂F₂OCF₃, CF₂OCF₃, C₆F₁₃, C₇F₁₅, C₈F₁₇ or C₉F₁₉, and M represents a hydrogen atom, an alkali metal, an alkaline-earth metal or a quaternary ammonium cation.

The invention relates to a method for the preparation of bis(fluorosulfonyl)-imide, the method starts from bis(chlorosulfonyl)-imide or its respective derivatives, which is reacted with HF in the presence of chlorosulfonyl isocyanate, and uses a certain extraction step for extraction of bis(fluorosulfonyl)-imide from an aqueous solution; the invention is also useful for the preparation of certain salts of bis(fluorosulfonyl)-imide and its derivatives.

The present invention provides an alkali metal salt of fluorosulfonyl imide having favorable heat resistance and a reduced content of specific impurities and a water content, and provides a method for producing an alkali metal salt of fluorosulfonyl imide, which is capable of easily removing a solvent from a reaction solution. An alkali metal salt of fluorosulfonyl imide of the present invention is represented by the following general formula (I) and has a mass loss rate of 2% or less when the alkali metal salt of fuluorosulufonyl imide is kept at 100° C. for 8 hours under an air current. A method for producing an alkali metal salt of fluorosulfonyl imide of the present invention comprises a step of concentrating a solution of the alkali metal salt of fulorosulfonyl imide by bubbling a gas into a reaction solution containing the alkali metal salt of fulorosulfonyl imide, and/or concentrating a solution of the alkali metal salt of fulorosulfonyl imide by thin layer distillation.

The invention discloses a method for electrochemical synthesis of lithium imidodifluorosulfonate. The preparation method comprises: regulating the temperature of an electrolytic tank to 0-18 DEG C, respectively taking two nickel plates as an anode and a cathode, adding a proper amount of anhydrous hydrofluoric acid into the electrolytic tank, and carrying out electrolysis; after the current in theelectrolytic tank is stabilized, adding a proper amount of imidodichlorosulfonate into the electrolytic tank, and after the imidodichlorosulfonate is dissolved, adjusting the working voltage of the electrolytic tank to 5-8 V; when the current is reduced to below 5 mA, taking out the solution in the electrolytic tank; distilling the solution taken out from the electrolytic tank under normal pressure to separate the imidodifluorosulfonate from the anhydrous hydrofluoric acid, and cooling to obtain the high-purity colorless liquid imidodifluorosulfonate; and reacting with lithium hydroxide, filtering, and re-crystallizing to obtain high-purity lithium imidodifluorosulfonate. According to the invention, water and chlorine ions are electrochemically pre-removed while fluorination is performedthrough electrochemistry without introduction of a metal halide as a catalyst, so that the method is simple in process, low in energy consumption and low in cost, and the prepared LiFSI is high in purity.

Methods of removing target impurities from a crude lithium bis(fluorosulfonyl)imide (LiFSI) to make a purified LiFSI product. In some embodiments, a purification method includes contacting crude LiFSI with a first anhydrous organic solvent to create a solution containing LiFSI and the target impurity(ies), wherein the LiFSI is soluble and the impurity(ies) is/are substantially insoluble. In some embodiments, a second anhydrous organic solvent is added to the solution to precipitate the target impurity(ies), which is then filtered to obtain a filtrate. In some embodiments, solvent is removed from the filtrate to obtain a solid mass containing LiFSI, which may then be contacted with a third anhydrous organic solvent in which the LiFSI is insoluble. The LiFSI may then be isolated from the third anhydrous organic solvent to obtain the purified LiFSI product. Also disclosed are purified LiFSI products and electrochemical devices utilizing purified LiFSI products, among other things.

A composition containing: at least 99.75% by weight of bis(fluorosulfonyl)imide lithium salt; and acetic acid in a content by mass greater than 0 and less than or equal to 400 ppm. A process for preparing the composition, including a) step of preconcentrating a composition C1 including an organic solvent OS1, water and bis(fluorosulfonyl)imide salt, to give a composition C2 including: the lithium salt of bis(fluorosulfonyl)imide in a content ranging from 35% to 50% relative to the total weight of composition C2; water in a mass content of less than or equal to 500 ppm relative to the total mass of composition C2; said preconcentration step being performed at a temperature of less than or equal to 50° C.; b) a step of concentrating composition C2; c) an optional step of crystallizing the composition obtained in step b).

The invention discloses a method for preparing imidodisulfuryl fluoride through micro-channel reactor. The method comprises the following operation steps: S1, preparation of materials: preparing a certain amount of ammonia gas, an organic solvent, ammonium salt, an organic alkali acid-binding agent, sulfuryl fluoride gas, alkali and acid, and preparing a plunger pump, a gas flowmeter, a micro-mixer, a silicon carbide micro-channel reactor, a rectification device and the like; S2, preparation of a reaction solution: introducing the ammonia gas into the organic solvent or dissolving ammonium salt in the organic solvent, and adding the organic alkali acid-binding agent to prepare a solution; and S3, gas-liquid mixing: adding the solution obtained in the step S2 and sulfuryl fluoride gas into a micro-mixer through the plunger pump and the gas flowmeter respectively. The method for preparing imidodisulfuryl fluoride through the micro-channel reactor is realized through the mature silicon carbide micro-channel reactor, is safe, short in reaction time, stable and reliable in process and simple to operate, does not have the problem of equipment corrosion, and brings better application prospects.

The present invention relates to a process for preparing a compound having the following formula (II):

F—SO₂—N⁻—SO₂—R₁NH₄⁺  (II)

wherein R₁ represents F or a linear or branched alkyl radical, substituted with at least one fluorine atom, said process comprising a step of bringing an anhydrous flow F1 comprising ammonia (NH₃) into contact with a compound of formula (I):

F—SO₂—NH—SO₂—R₁  (I)

R₁ is as defined above.