102results about "Amidosulfonic 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 invention discloses a preparation method of difluorosulfimide salt. The preparation method comprises the following steps: (1) adding dichlorosulfimide and a nitrogen-containing hydrogen fluoride complex which are used as reaction raw materials into an organic solvent for reaction at 0-100 DEG C, and after reaction, distilling to remove the organic solvent to obtain a difluorosulfimide and nitrogen-containing ion compound; (2) adding the ion compound obtained in the step (1) into a water solution of metal alkali or salt, neutralizing until the solution is neutral, distilling, drying, re-crystallizing by using the organic solvent, and purifying to obtain difluorosulfimide salt. According to the preparation method, the nitrogen-containing hydrogen fluoride complex is adopted as a fluorating agent, so that the whole reaction is carried out in a homogeneous system, the fluorating reaction is relatively safe, the efficiency is relatively high, and the product yield is more than 98%; a process route is simple, the yield is high, and the production cost is relatively low.

The invention relates to a preparation method of a difluoro-sulfonyl imine salt, and belongs to the field of fine chemical engineering. The difluoro-sulfonyl imine salt is MN(SO2F)2, wherein M is Li, Na, K, Rb or Cs. The preparation method comprises the following steps: mixing FSO2X, a nitrogen source, an acid-binding agent and an aprotic solvent to obtain a mixture, wherein X is F, Cl, Br or I, the nitrogen source is anammonium salt or anhydrous NH3, the acid-binding agent is a lithium, sodium, potassium, rubidium or cesium salt, the mole ratio of NH3 or ammonium ion to FSO2X is 1:(2-10), and the mole ratio of NH3 or the ammonium ion to the acid-binding agent is 1:(3-10); heating to perform reflux reaction on the mixture for 5-8 hours; cooling to obtain a filtrate; and removing the solvent to obtain a crude product, and performing vacuum drying to obtain the difluoro-sulfonyl imine salt. The preparation method has easily available raw material, is safe and pollution-free, is high in yield, is easy to realize separation and purification, is simple in step, is not severe in requirement of operation equipment, and is suitable for industrial production.

The invention discloses a preparation method for coproducing bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide, which comprises the following steps: S1, adding sulfuryl chloride into a first solvent, dropwisely adding octamethylcyclotetrasilazane for reaction, and carrying out purification to obtain bis(chlorosulfonyl)imide; S2, taking bis(chlorosulfonyl)imide and anhydrous hydrofluoric acid to react under the action of a catalyst to obtain bis(fluorosulfonyl)amide; and S3, taking the bis(fluorosulfonyl)amide and lithium fluoride to react in a second solvent, and carrying out purification to obtain the lithium bis(fluorosulfonyl)imide. According to the invention, proper raw materials are selected and matched with a solvent method to co-produce bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide. The method has the advantages of simple preparation process, few and recyclable byproducts, high yield, no water participation in the production process, high purity of the obtained bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide, no wastewater generation and green and environment-friendly process route, and is suitable for industrial production.

The invention provides a method for preparing disinfected-decolorized fish-squamosum organic acid calcium and non-denatured collagen. The method comprises the following steps: adding disinfected decolorized fish squamosum solids to 10 to 20 percent organic acid in a solid-liquid ratio of 1:5-10; using energy-gathering ultrasonic wave to treat the obtained product for 4 to 24 hours; performing filtration and solid-liquid separation to obtain a crude product of collagen fish squamosum; standing filtrate at 10 DEG C for 4 to 15 hours to obtain organic acid calcium precipitate; filtering and drying the obtained product to obtain a finished product of disinfected-decolorized fish-squamosum organic acid calcium; adding 0.5 to 1 percent organic acid and/or 0.1 to 1 percent acidproof protease solution to the crude product of fish squamosum collagen in a solid-liquid ratio of 1:5-10; using energy-gathering ultrasonic wave to treat the obtained product at 10 to 35 DEG C for 2 to 4 hours until the crude product of fish squamosum collagen dissolves in the solution; removing impurities; and drying filtrate to obtain non-denatured collagen. The method has the advantages of low production cost and capability of obtaining disinfected-decolorized fish-squamosum organic acid calcium and non-denatured collagen at a time.

The invention relates to a preparation method of an electronic grade high-purity nickel sulfamic acid solution, comprising the following steps of: (1) dissolving industrial grade nickel vitriol raw materials in purified water, filtering and concentrating a solution for crystallization to obtain a refined nickel vitriol crystal; (2) preparing the obtained nickel vitriol crystal into the solution to react with sal volatile; (3) precipitating and putting prepared alkaline nickel carbonate in a sodium oxide solution, cooking and washing the alkaline nickel carbonate to be neutral by purified water; and (4) reacting the washed alkaline nickel carbonate with sulfamic acid to obtain the nickel sulfamic acid solution. The preparation method has the advantages of high product purity, lower contents of sulfate and sodium ions than those of products prepared by an ordinary carbonate method, simple process condition, easy control and low production cost.

The invention discloses a fast production method of high-purity metal sulphamate. The fast production method comprises the following steps of: adopting excess metal powder and sulphamic acid, wherein the average particle size of the metal powder is less than 100nm; introducing pure water at the temperature of 40-60 DEG C; grinding and stirring for reaction in a drum type closed reaction tank with a grinding device under the participation of high-pressure oxygen; filtering to obtain a sulphamate solution with the concentration which can be up to 180g/L (by weight of metal); and recovering the filter residue (the metal powder) for reutilizing nickel sulphamate and cobalt sulphamate. As raw materials are simple and strong acid, base and other initiators are not added during the production process, the pollution caused by other hetero ions is avoided, and the purity of the sulphamate is only affected by the metal powder and the purity of the sulphamic acid; the smaller the average particle size of the metal powder, the higher the yield; and sulfate radicals are less than 600ppm, and the content of sodium ions and other metal ions is very low, which can not be detected by a conventional method.

A synthetic method of novel lithium bis(fluorosulfonyl)imide is provided. Compared with the prior art, the method is characterized in that the lithium bis(fluorosulfonyl)imide is prepared through reacting an aromatic methylamine that is adopted as an initial compound with organoboron, reacting with halogen sulfonyl to obtain a sulfonyl-containing aromatic methylamine, performing a hydrogenation reduction reaction to obtain bis(fluorosulfonyl)imide, and performing ion exchange with resin lithium. In a final strong base reaction for preparing the lithium bis(fluorosulfonyl)imide, the method adopts a resin lithium ion exchange technique, thus breaking away from convention, and the method researches the possibility that the reaction is performed without a solvent for the first time at home and abroad and synthesizes the lithium bis(fluorosulfonyl)imide in an ion exchange manner. The method has advantages of a simple process, convenience, simple after-treatment, no complex operation, and cyclic use of the resin lithium, and the like.

The invention discloses a method for preparing lithium bis (fluorosulfonyl) imide by using an organic metal lithium reagent. The method comprises the following steps: S1, using the organic metal lithium reagent as a raw material, carrying out mixed reaction with bis (fluorosulfonyl) imide acid to obtain a lithium bis (fluorosulfonyl) imide crude product; S2, performing vacuum pumping on the crudeproduct, adding a poor organic solvent of lithium bis (fluorosulfonyl) imide for multiple times of washing, and then performing vacuum pumping to obtain a solid; and S3, adding an organic solvent intothe solid, extracting, filtering, concentrating, adding a low-polarity aprotic solvent into the concentrated solution, standing, crystallizing, filtering, and carrying out vacuum drying on the crystal to obtain the lithium bis (fluorosulfonyl) imide. The preparation steps are carried out without water under the protection of inert gas. According to the preparation method, high-purity lithium bis(fluorosulfonyl) imide can be prepared, the yield is high, the product quality is stable, and the content of impurities such as potassium ions, sodium ions, calcium ions, fluorine ions, chloride ions,sulfate ions and water in the product is effectively reduced.

The invention relates to the technical field of chemical industry production, and specifically relates to an energy-saving environment-friendly co-production technology of cyanuric acid, food-grade sulfuric acid and sulfamic acid. The co-production process comprises the steps of (1) cyanuric acid production; (2) food-grade sulfuric acid production including sulfur melting, sulfur burning, conversion, absorption and drying, and residual heat recovery; and (3) sulfamic acid production. With the co-production process, defects in independent production links of cyanuric acid, food-grade sulfuric acid and sulfamic acid are solved, and no additional environmental treatment equipment is needed, such that the production process is greatly simplified, and the production period is shortened. The process is safe, energy-saving and environment-friendly.

The invention discloses a continuous preparation method of bis(fluorosulfonyl)imide. The continuous preparation of bis(fluorosulfonyl)imide is carried out in a microchannel reactor, and comprises the following steps: A1, preheating a first raw material chlorosulfonic acid and a second raw material chlorosulfonyl isocyanate in a preheating module at the preheating temperature of 30-150 DEG C; A2, feeding a third raw material hydrogen fluoride, the preheated first raw material chlorosulfonic acid and the preheated second raw material chlorosulfonyl isocyanate into a reaction module for mixed reaction, wherein the molar ratio of the hydrogen fluoride to the chlorosulfonic acid to the chlorosulfonyl isocyanate is (2-2.5):1:1, the flow rate of the chlorosulfonic acid is 1-100g/min, the flow rate of the chlorosulfonyl isocyanate is 1-100g/min, the reaction temperature is 30-150 DEG C, the reaction pressure is 0-0.5 MPa, and the retention time is 1-100s; and A3, carrying out gas-liquid separation on the product at the outlet of the reaction module to obtain bis(fluorosulfonyl)imide. The method has the advantages of simple process, low equipment loss, high yield and the like.

The invention provides a method for comprehensive utilization of cyanide tailings. According to the method, sulfur concentrates with the sulfur content greater than or equal to 46% are screened out, and sulfuric acid is prepared from the sulfur concentrates, so that the quality of the sulfuric acid is guaranteed; by mixing the tailings, fly ash and clay according to a specific ratio and carrying out roasting at high temperature, cyanide ions and organic agents contained in the tailings can be decomposed, and thus, the tailings are changed into non-toxic products; the tailings contain a small amount of sulfur during roasting, internal structures of ceramsite can have gaps along with the volatilization of the sulfur, and crystal forms are changed, so that the strength of the ceramsite is greatly improved. According to the method for the comprehensive utilization of the cyanide tailings, provided by the invention, the cyanide tailings are completely utilized while virulent cyanide ions are removed from the cyanide tailings, so that the method is environmentally friendly, the prepared ceramsite and sulfuric acid are excellent in quality, and huge economic benefit is brought.

The invention discloses a low-sulfate radical sulfamate concentrated liquid preparation method and a device thereof. The method comprises: taking 1 to 3 portions of nickel carbonate, or cobalt carbonate, or nickel hydroxide or cobalt hydroxide (counted in metal weight) and 3 to 9 portions of dry powder sulfamic acid; stirring uniformly in a reaction can, then adding 5 to 15 portions of pure hot water with the temperature of 30-40 DEG C and stirring for 50 to 70 minutes in the closed reaction can; a mode of rotating the reaction can is employed by the stirring; a fixed stirring device is arranged in the closed reaction can for stirring, and ball milling grinding, stirring while grinding, pressurizing and filtering are carried out to collect the concentrated liquid of nickel sulfamic acid or cobalt sulfamate; the concentration can achieve about 210g/L; the sulfate radicals are less than 600PPM; and crystallization can be obtained by heating and vaporizing for a while. The special device designed for the method integrates reaction and filtering, shortens the reaction time and improves the reaction effect.

The invention relates to a process for producing nickel sulfamic acid, which is characterized in that the preparation process comprises (1) nickel sulfate or nickel chloride is carried on nickel ammonia complex reaction with ammonia to obtain nickel ammonia complex solution, (2) nickel hydroxide is prepared by the reaction of the produced nickel ammonia complex solution and sodium hydrate, (3) the produced nickel hydroxide solution is washed and filtered, (4) nickel sulfamic acid solution is produced by the reaction of the filtered nickel hydroxide solution and sulfamic acid, and (5) nickel sulfamic acid is prepared by condensing and crystallizing nickel sulfamic acid solution. The process of the invention has the advantages that the cost is reduced by producing through combining with nickel sulfate, the product purity is high, the process condition is simple and the reaction endpoint is clear.

The invention discloses a method for preparing nickel aminosulfonate with solid sulfamic acid, comprising the following steps: carrying out P204 extraction on a nickel-containing solution to obtain a nickel-containing loaded organic phase; directly carrying out back extraction on the nickel-containing loaded organic phase with solid sulfamic acid to convert the nickel-containing loaded organic phase to a high concentration of a nickel aminosulfonate solution, evaporating, crystallizing, centrifuging, drying and screening to obtain a nickel aminosulfonate product. The invention has beneficial effects as follows: as resources are fully utilized and solid sulfamic acid is directly used in the reaction, an acid dissolution process is reduced, cost is saved and labor intensity of operators is also minimized; due to over-dose of sulfamic acid during the back extraction, the prepared nickel aminosulfonate solution has a high concentration (150g/L-200g/L), evaporation time is short, steam consumption is reduced, and production cycle is shortened.

The invention relates to the technical field of production of bis (chlorosulfonyl) imide, in particular to a production process of bis (chlorosulfonyl) imide. The production process of the bis (chlorosulfonyl) imide comprises the steps of adding sulfamic acid and thionyl chloride into a reaction kettle until solids are completely dissolved, then adding sulfur trioxide into the reaction kettle at a constant speed, after the sulfur trioxide is completely added, heating to the temperature of 90-120 DEG C, continuing to react for 5-10 hours, restoring to normal pressure, opening a condensate outlet valve of a condenser, continuing to react for 1-3 hours, carrying out reduced pressure rectification until no condensate flows out of the condenser, and obtaining the target product bis (chlorosulfonyl) imide. Compared with an original chlorosulfonic acid method process, the production process has the advantages that the hydrogen chloride waste gas amount is reduced by 1/3, the sulfur dioxide tail gas can be recycled and reused in a thionyl chloride production device, the yield of three wastes is further reduced, and the production process belongs to an innovative process meeting the development requirements of the green chemical industry.

The invention belongs to the technical field of lithium ion battery electrolyte salt synthesis, and particularly relates to a preparation method of lithium bis (fluorosulfonyl) imide. Comprising the following steps: (1) in the presence of an organic solvent, mixing bis (fluorosulfonyl) imide triethylamine salt and an alkaline lithium salt, carrying out a stirring reaction, carrying out reduced pressure distillation, and removing triethylamine and water generated in the reaction until no bis (fluorosulfonyl) imide triethylamine salt exists in a reaction solution; and (2) filtering the reaction liquid after the reaction in the step (1) under the protection of nitrogen, concentrating the filtrate, adding a poor solvent, crystallizing, filtering and drying to obtain the product lithium bis (fluorosulfonyl) imide. The preparation method disclosed by the invention is simple and convenient to operate, the lithium ion exchange reaction is thorough, and the product is easy to crystallize and separate, so that the generated lithium bis (fluorosulfonyl) imide is high in yield and high in purity.