42results about "Amidosulfonic acid" 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 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.

An electrolyte composition includes: a sulfonylimide compound represented by the following general formula (1) as an electrolyte salt; and an amidosulfuric acid component.LiN(X1SO2)(X2SO2)  (1)(where X1 and X2 are identical to or different from each other, and each represent a fluorine atom, an alkyl group with a carbon number of 1 to 6, or a fluoroalkyl group with a carbon number of 1 to 6).

Provided in the present application is a method for treating a heavy bis(fluorosulfonyl)imide residue, comprising the following step: causing a starting material system comprising the heavy bis(fluorosulfonyl)imide residue and an acidic aqueous solution to react to obtain a fluorine-containing acid solution and a crude sulfamic acid product, wherein the fluorine-containing acid solution can be used as a by-product acid, thereby saving treatment costs; and the crude sulfamic acid product can also be directly sold as a product, thereby reducing treatment costs, bringing economic benefits, and achieving resource recycling of the heavy bis(fluorosulfonyl)imide residue.

The invention provides a method for treating bis (fluorosulfonyl) imide heavy slag, which comprises the following steps: reacting a raw material system comprising bis (fluorosulfonyl) imide heavy slag and an acidic aqueous solution to obtain a fluorine-containing acid solution and a sulfamic acid crude product; wherein the fluorine-containing acid liquid can be used as a byproduct acid, so that the treatment cost is saved; and the sulfamic acid crude product can also be directly sold as a product, so that the treatment cost is reduced, economic benefits are brought, and resource recycling of the bis (fluorosulfonyl) imide heavy slag is realized.

The present invention relates to a process for preparing a compound of structural formula (I), comprising reacting a compound of structural formula (II) with water in the presence of an organic amide or an organic amine, and to the use of a compound of structural formula (I) for preparing a compound of structural formula (IVa), (IVb) or (IVc).

The invention relates to a method for producing a compound of structural formula (I), comprising reacting a compound of structural formula (II) with water in the presence of an organic amide or an organic amine, and to the use of a compound of structural formula (I) for producing a compound of structural formula (IVa), (IVb) or (IVc).

The application provides a method for recycling calcium sulfate in lithium mica production of lithium carbonate, and belongs to the technical field of smelting.The lithium mica is calcined with the calcium sulfate clinker, the pressure filtration residue after the lithium ion is leached by water is put into an aqueous sulfamate solution and is stirred again, the calcium sulfate in the residue is reacted with the sulfamate and is dissolved, ion exchange is carried out through a sodium type ion exchange resin, backwashing and precipitation processes are carried out, the calcium sulfate is generated again, and the calcium sulfate is returned as a lithium mica auxiliary material, so that the recycling of the calcium sulfate is realized, and the treated filter residue is used as a mixed material and does not affect the performance of the prepared cement.The process can significantly improve the consumption amount of the lithium mica residue in the cement industry, saves the land resources occupied by the stacking or landfill of the lithium mica residue, reduces the environmental protection pressure, and has a wide application prospect.

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 disclosure relates to a lithium-ion-conducting material and a purification method therefor, and provides a lithium-ion-conducting material, which comprises lithium sulfonimide represented by the following general formula (I), wherein X and Y may be the same or different, and are each independently CmF2m+1 (m≥0). Further provided is a purification method for the lithium-ion-conducting material. The method of the present disclosure provides a lithium sulfonimide lithium-ion-conducting material having a high purity.

The invention discloses a preparation method of nickel aminosulfonate, and relates to the technical field of nickel-containing chemical production, and the method comprises the following specific steps: multi-element metal pretreatment: mixing and ball-milling nickel, aluminum and magnesium powder, adding an acyclic boroxane-containing aqueous solution, and carrying out ultrasonic treatment to form a suspension; a reaction system is constructed by mixing the suspension liquid, sulfamic acid and an acyclic organic phosphorus compound, a segmented stirring reaction is carried out under the conditions of oxygen introduction and proper temperature and humidity, programmed crystallization and cooling are carried out to form wet crystals, and nickel sulfamic acid is finally prepared through segmented vacuum drying; through collaborative design of multi-metal pretreatment and a reaction system, reaction preparation and proportion are optimized, reaction activity and conversion rate are improved, and side reactions are reduced; and by matching with segmented stirring, substance transfer is promoted, the product purity is guaranteed, program crystallization and segmented vacuum drying are combined, crystal growth and drying conditions are controlled, impurities are removed, the product purity, stability and production efficiency are improved, and the large-scale production requirement is met.

A process for producing a sulfamyl fluoride composition includes providing a solution comprising fluorosulfonic acid, urea and a solvent; reacting the solution at a reaction temperature from 80°C to about 170°C to produce a mixture including sulfamyl fluoride, bis(fluorosulfonyl) imide, ammonium fluorosulfate and the solvent; separating the ammonium fluorosulfate from the mixture; and separating the mixture into a sulfamyl fluoride composition and a recycle composition, the sulfamyl fluoride composition including a higher concentration of sulfamyl fluoride and bis(fluorosulfonyl) imide than the recycle composition. A mole ratio of the fluorosulfonic acid to the urea in the solution is from about 1.80:1 to about 2.00:1.

The invention discloses a method for preparing bis (fluorosulfonyl) imide lithium salt by a one-pot method. The preparation method comprises the following steps: mixing sulfuryl fluoride, ammonium fluoride, lithium hydroxide (lithium carbonate) and specific amine according to a certain proportion, synthesizing bis (fluorosulfonyl) imide lithium salt in an organic solvent, and then carrying out solid-liquid separation and purification to obtain the high-purity bis (fluorosulfonyl) imide lithium salt. The preparation method comprises the following steps: sequentially adding ammonium fluoride, organic amine and lithium hydroxide (lithium carbonate) under the condition of shielding gas, and stirring and reacting at a proper temperature; the method is simple to operate and is carried out in one reactor. The reaction conditions are mild, and the use of dangerous chemicals in the traditional method is avoided. The core of the invention is innovation of the synthesis method. The method is simpler to operate, and the reaction process is safer and more green.

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.

This invention proposes an environmentally friendly and efficient method for preparing aminosulfonic acid, belonging to the field of chemical technology. It includes: (1) sulfonation reaction; (2) crude product filtration; (3) dissolution and crystallization; and (4) drying and packaging. The reaction process of this invention features mild reaction conditions, short reaction time, and a yield exceeding 97%. The process, using fuming sulfuric acid and urea at a lower temperature, significantly reduces polluting components in the waste gas. It has many advantages, including simple operation, low cost, high yield, and greater environmental friendliness.

The present invention relates to the technical field of additives to an electrolytic solution of salt batteries; in particular, the present invention relates to a method for preparing a high-purity bisfluorosulfonylimide salt. The preparation raw materials include at least bisfluorosulfonylimide, and M+nXn-; wherein M is selected from any one of Li, Na, K, Rb and Cs, X is an anion including at least one element of B, O, N, P and Si, and n≥2. In the method for preparing a bisfluorosulfonylimide salt provided by the present disclosure, a conversion rate for a target product is high, there is only a single reaction product with almost no side reactions, and the purity of the product is high; during the implementation, there is substantially no generation of the "three wastes", and the byproducts and solvent can be recycled.

The present invention addresses the problem of suppressing the influence of a sulfur component derived from a salt of an electrolyte solution when recovering a positive electrode active material from a positive electrode mixture. The present invention provides a method for recycling a lithium ion battery using LiFSI as a salt of an electrolyte solution, the method comprising: a treatment agent mixing step for mixing lithium carbonate with a positive electrode mixture recovered from a waste lithium ion battery; and a heating step for heating a mixture obtained by mixing lithium carbonate with the positive electrode mixture to a heating temperature that is equal to or higher than the melting point of LiFSI and equal to or lower than the melting point of lithium carbonate.

The invention relates to a purification technology of bis (chlorosulfonyl) imide containing chlorosulfonic acid impurities, and provides a purification method of bis (chlorosulfonyl) imide, which is simple to operate and can give consideration to both high purity and higher yield in the process of purifying bis (chlorosulfonyl) imide containing chlorosulfonic acid. The purification method comprises the following steps: (1) supercooling a bis (chlorosulfonyl) imide solution containing chlorosulfonic acid impurities to obtain a supercooled solution; (2) continuously dropwise adding the supercooled solution onto a conveyor belt from a liquid outlet positioned above the conveyor belt, and simultaneously meeting the following conditions in the dropwise adding process: the dropwise adding flow F of the supercooled solution is 0.1-1L / min, and the linear velocity V of the conveyor belt is 0.01-1m / s, the height difference h between the liquid outlet and the surface, used for receiving the dropwise added supercooled solution, of the conveying belt is 0.1-1m; the A value calculated according to the following relational expression needs to be controlled between 5 and 30: A = F / V / (h / 4.9) 0.5; and (3) carrying out solid-liquid separation on the solid-liquid mixture.

A process for producing a sulfamyl fluoride composition includes providing a solution comprising fluorosulfonic acid, urea and a solvent; reacting the solution at a reaction temperature from 80° C. to about 170° C. to produce a mixture including sulfamyl fluoride, bis(fluorosulfonyl) imide, ammonium fluorosulfate and the solvent; separating the ammonium fluorosulfate from the mixture; and separating the mixture into a sulfamyl fluoride composition and a recycle composition, the sulfamyl fluoride composition including a higher concentration of sulfamyl fluoride and bis(fluorosulfonyl) imide than the recycle composition. A mole ratio of the fluorosulfonic acid to the urea in the solution is from about 1.80:1 to about 2.00:1.

The invention discloses a process for producing sulfamic acid by a solid-phase dilution method. The invention relates to a sulfamic acid production process by a solid phase dilution method. The process comprises the following steps: S1, preparing a pre-reaction material with the sulfuric acid concentration of 105.5%; s2, adding the pre-reaction material and urea into a pre-sulfonation reactor for reaction, enabling reaction liquid to overflow into the sulfonation reactor, and performing sulfonation reaction to obtain a liquid mixture; s3, carrying out immobilization on the liquid mixture through speed-adjustable centrifugal anti-spiral immobilization equipment, and feeding an obtained immobilization material into a dilution kettle; s4, adding mother liquor into the dilution kettle to dilute and adjust the viscosity of the material; and S5, performing solid-liquid separation on the liquid material with the adjusted viscosity to obtain a sulfamic acid crude product and dilute sulphuric acid, and performing crystallization purification on the sulfamic acid crude product to obtain sulfamic acid. The sulfamic acid production process is improved, excessive fuming sulphuric acid entering the dilution process in the reaction process is remarkably reduced, the generation of a new byproduct dilute sulphuric acid is reduced, and the production cost is reduced.

The invention discloses a sulfamic acid reactor with a quantitative feeding structure, which belongs to the technical field of sulfamic acid production equipment. The reactor body assembly comprises a reactor body, a feeding assembly is installed on the upper end of the reactor body, a quantitative assembly is installed inside the feeding assembly, and a stirring assembly is installed inside the reactor body. The spherical feeding assembly cooperates with a rotating ball, and a first holding mechanism and a second holding mechanism are used alternately, so that not only the interior of the reactor body assembly is replenished with raw materials, but also the external environment is prevented from being connected to the interior of the reactor body. The weighing pan is used to improve the accuracy of feeding, the steel balls and elastic rods are used to reduce the adhesion of dust falling off the urea particles, and the bulk material pan is used to evenly sprinkle the urea particle raw materials into the interior of the reactor body, so as to improve the uniformity during the reaction, and the inclined screw conveyor is used to reduce the height of the storage hopper, so as to facilitate the replenishment of raw materials and the operation.

The present invention provides a method for preparing bis(trifluoromethanesulfonyl)imide lithium by a one-step method, belonging to the field of fine chemicals. Trifluoromethanesulfonyl chloride and lithium amide are reacted in an organic solvent under the action of an alkaline catalyst, reaction temperature 5-25 DEG C, reaction time 20-60min, bis(trifluoromethanesulfonyl)imide lithium crude product can be obtained by filtration, after purification by recrystallization and drying, bis(trifluoromethanesulfonyl)imide lithium purity is more than 99%, and yield is more than 96%. The present invention can prepare bis(trifluoromethanesulfonyl)imide lithium through one-step reaction, and reaction temperature is relatively low, catalyst raw material is cheap and easy to obtain, process route is simple, by-products are few, and yield is high; the bis(trifluoromethanesulfonyl)imide lithium obtained has high purity and meets battery-grade requirements; when the bis(trifluoromethanesulfonyl)imide lithium of the present invention is used as a lithium battery electrolyte solute, performance is better than commonly used lithium hexafluorophosphate, and has broad industrialization and application prospects.

The present invention provides a process for the preparation and purification of lithium bis(fluorosulfonyl) imide (LiFSI). More particularly, the present invention provides a process for the preparation of battery grade lithium bis(fluorosulfonyl) imide (LiFSI) having high purity with reduced content of moisture, metal and anionic impurities, which is cost-effective and industrially scalable.

A method of purifying a crude lithium bis(fluorosulfonyl)imide, includes adding a water removal agent to a pretreatment liquid containing the crude lithium bis(fluorosulfonyl)imide to perform a dehydration reaction at a temperature ranging from 20°C to 40°C, reacting the same for an additional 1 h to 6 h after an acid gas stops escaping from the reaction system, and filtering the reaction system to obtain a filtrate; the water removal agent is bismuth trichloride or antimony trichloride. Evaporating and concentrating the filtrate, and recrystallizing the concentrated filtrate are performed to obtain a purified lithium bis(fluorosulfonyl)imide.

The invention relates to a method for electrochemical synthesis of bis (fluorosulfonyl) imide alkali metal salt. The method comprises the following steps that under the action of an external electric field, alkali metal cations penetrate through the cation exchange membrane to enter the product chamber (2), bis (fluorosulfonyl) imide anions penetrate through the anion exchange membrane to enter the product chamber (2), and the alkali metal cations and the bis (fluorosulfonyl) imide anions in the product chamber (2) are combined to form bis (fluorosulfonyl) imide alkali metal salt. The bis (fluorosulfonyl) imide alkali metal salt prepared by the method has extremely high purity and hardly contains other water-soluble impurities, so that the synthesis steps are simplified, and the subsequent purification process is greatly simplified.

The invention relates to the technical field of batteries, in particular to a lithium bis (fluorosulfonyl) imide treatment method, lithium bis (fluorosulfonyl) imide, an electrolyte, a battery and electric equipment. The lithium bis (fluorosulfonyl) imide treatment method comprises the following steps: providing a mixture containing lithium bis (fluorosulfonyl) imide; and reacting the mixture containing the lithium bis (fluorosulfonyl) imide with the porous adsorbent under an alkaline condition to obtain a purified solution containing the lithium bis (fluorosulfonyl) imide. Under the alkaline condition, chromaticity substances in the mixture containing the lithium bis (fluorosulfonyl) imide are adsorbed through the porous adsorbent, so that the chromaticity of the lithium bis (fluorosulfonyl) imide is reduced, materials are prevented from becoming acid, and meanwhile equipment is prevented from being corroded.

The present invention discloses a continuous crystallization device for sulfamic acid production and its usage method, belonging to the technical field of sulfamic acid preparation. A top cover is movably installed between the outer ring platform and the inner ring platform, and the threaded ring triggers multiple locking rods and lifting blocks to double-lock the top cover; the end of the diversion pipe is provided with multiple spray heads located inside the condensation cylinder; multiple condensation pipelines are opened on the inner wall of the condensation cylinder, an air inlet annular groove communicating with the condensation pipelines is opened on the inner wall of the first closed cover, a second closed cover is further installed on the right side of the condensation cylinder, an air outlet annular groove communicating with the condensation pipelines is opened on the inner wall of the second closed cover, and an air outlet nozzle is arranged on the outer wall of the second closed cover. The present invention can quickly crystallize the sulfamic acid solution through the condensation cylinder. After the waste liquid is discharged from the condensation cylinder, the discharge motor is started and the sector plate is driven to rotate to open the discharge cavity. With the cooperation of the inner cylinder and the scraping strip, the sulfamic acid crystals are scraped off. This design improves the practicability of the continuous crystallization device.

The present invention belongs to the technical field of lithium-ion battery electrolyte preparation, and specifically relates to a method for preparing lithium bis(fluorosulfonyl)imide, comprising: reacting a lithium source with bis(chlorosulfonyl)imide to obtain lithium bis(chlorosulfonyl)imide; and reacting the lithium bis(chlorosulfonyl)imide with a fluorination agent to obtain lithium bis(fluorosulfonyl)imide. The present invention provides a novel synthetic route for lithium bis(fluorosulfonyl)imide, utilizing lithiation followed by fluorination to prepare the lithium bis(fluorosulfonyl)imide. The method can be carried out under mild reaction conditions and does not require the use of high-temperature hydrogen fluoride, resulting in a simple process, low energy consumption, and high safety.

The application provides a treatment method of bisfluorosulfone imide heavy residue, which comprises the following steps: reacting a raw material system comprising bisfluorosulfone imide heavy residue and an acidic aqueous solution to obtain a fluorine-containing acid liquid and an amino sulfonic acid crude product; wherein the fluorine-containing acid liquid can be used as a by-product acid to save treatment costs; the amino sulfonic acid crude product can also be directly sold as a product to reduce treatment costs, bring economic benefits, and realize resource recycling of the bisfluorosulfone imide heavy residue.

The present invention provides a preparation method of bis(trifluoromethanesulfonyl)imide salt, belonging to the chemical engineering field. Using NH2M, where M = Li, Na, K, Rb or Cs, HSO2X and CX4, where X is F, Cl, Br or I, and anhydrous hydrogen fluoride as synthetic raw materials to prepare bis(trifluoromethanesulfonyl)imide salt. The preparation method has simple synthesis, convenient operation, low energy consumption and low labor consumption, which is beneficial to industrial production.