188 results about "Chlorosulfonic acid" patented technology

The invention relates to the technical field of pesticide production, in particular to a synthesis method of 1-methyl-3-trifluoromethyl-4-chloromethyl-5-difluoromethoxy-1-H-pyrazole, which at least comprises the following steps: firstly, mixing trioxymethylene and 1-methyl-3-trifluoromethyl-5-difluoromethoxy-1-H-pyrazole to prepare a solution A; the solution A and chlorosulfonic acid are mixed and then subjected to a chloromethylation reaction, 1-methyl-3-trifluoromethyl-4-chloromethyl-5-difluoromethoxy-1-H-pyrazole is obtained through aftertreatment after sampling detection is qualified, and the method is high in product yield, high in purity, low in production cost, high in production efficiency, easy to operate, capable of meeting the green and environment-friendly requirements and suitable for industrial production. The industrial production is easy to realize.

The invention relates to the technical field of pollen polysaccharides, and discloses a preparation method and application of rape pollen polysaccharides, and the preparation method comprises the following steps: treating degreased rape pollen with a mixed enzyme solution of cellulase and pectinase, and centrifuging to obtain a polysaccharide-containing supernatant; mixing the supernate with absolute ethyl alcohol, centrifuging, and dissolving the precipitate with distilled water to obtain a polysaccharide solution; the polysaccharide solution is sulfonated and modified by a chlorosulfonic acid and pyridine mixed solution, and then carboxymethylated with a monochloroacetic acid and NaOH mixed solution to obtain a modified polysaccharide solution. And finally, dialyzing to remove impurities, and freeze-drying to obtain the rape pollen polysaccharide. Through the extraction and modification technology, the application range of polysaccharide products in agriculture is expanded, crop growth can be more effectively promoted, the yield and quality are improved, and meanwhile negative influences on the environment are reduced.

The invention provides an antistatic agent for fuel oil and a preparation method thereof, and belongs to the technical field of petrochemical engineering, and the preparation method comprises the following steps: S1, adding soybean lecithin and chlorosulfonic acid into dichloroethane, uniformly mixing, under the protection of nitrogen, heating and stirring for reaction, neutralizing reaction liquid, and performing rotary evaporation to obtain sulfonated soybean lecithin; the preparation method comprises the following steps: adding sulfonated soybean lecithin and ethidene diamine into absolute ethyl alcohol, then adding p-toluenesulfonic acid, heating and stirring for reaction, and carrying out reduced pressure distillation to obtain modified soybean lecithin; s2, dispersing the SiO2 particles in absolute ethyl alcohol, adding KH-550, and performing ultrasonic treatment, centrifugation and drying to obtain pretreated SiO2 particles; and uniformly mixing the modified soybean lecithin and the pretreated SiO2 particles, adding the mixture into a supercritical fluid reactor, heating and pressurizing, ultrasonically dispersing, and drying to obtain the antistatic agent. The antistatic agent has the advantages of good dispersibility, strong stability and strong antistatic capability.

The invention belongs to the technical field of sulfonamide synthesis, and particularly relates to a green and environment-friendly sulfonamide amidation preparation method. Comprising the following steps: adding chlorosulfonic acid into a reactor, stirring, heating, adding o-nitrochlorobenzene, carrying out staged heat preservation, cooling, and adding thionyl chloride to obtain 2-nitro-4-chlorine sulfonate-chlorobenzene; the method comprises the following steps: separating and filtering 2-nitro-4-chlorine sulfonate-chlorobenzene, adding ammonia water, stirring, preserving heat, and carrying out filter pressing to obtain 2-nitro-4-amine sulfonate-chlorobenzene; the preparation method comprises the following steps: adding liquid caustic soda into 2-nitro-4-amine sulfonate-chlorobenzene, stirring, heating, and adjusting the pH value to obtain 2-nitro-4-amine sulfonate-phenol; the method comprises the following steps: adding water, a catalyst and hydrazine hydrate into 2-nitro-4-amine sulfonate-phenol, heating, stirring, and carrying out filter pressing to obtain 4-sulfonamide-2-amino-phenol. According to the preparation method of sulfonamide, generated tail gas is subjected to falling film absorption treatment, and the product prepared by the preparation method is high in purity.

The invention belongs to the technical field of preparation of single-walled carbon nanotube fibers, and particularly relates to a preparation method of high-conductivity single-walled carbon nanotube fibers, which comprises the following steps: preparing a single-walled carbon nanotube crude product by a chemical vapor deposition method, pickling and purifying, and oxidizing and purifying at high temperature to obtain a single-walled carbon nanotube; the preparation method comprises the following steps: adding a single-walled carbon nanotube into a poly [2, 5-dihydroxy-1, 4-phenylene pyridine diimidazole] aqueous solution, dispersing, and collecting supernatant liquid to obtain a single-walled carbon nanotube purified liquid; adding chlorosulfonic acid into the single-walled carbon nanotube purified solution in an argon atmosphere to obtain a single-walled carbon nanotube spinning solution; and injecting the single-walled carbon nanotube spinning solution into a coagulating bath in an argon atmosphere to prepare the single-walled carbon nanotube fiber. According to the invention, the poly [2, 5-dihydroxy-1, 4-phenylenediimidazole] is adopted to selectively disperse the metallic single-walled carbon nanotubes, and the gold single-walled carbon nanotubes in the single-walled carbon nanotube fibers are high in purity, so that the conductivity can be improved.

The invention relates to a preparation method of triethylene glycol diacetate, and belongs to the technical field of organic synthesis. The method comprises the following steps: adding triethylene glycol, an acetylation reagent and a multifunctional catalyst into a reaction kettle provided with a stirrer, a thermometer and a reflux condensing tube, and stirring and heating for reaction under the protection of nitrogen; after the reaction is finished, cooling reaction liquid to room temperature, and filtering and recovering the catalyst; performing reduced pressure distillation and silica gel column purification on the filtered reaction liquid to obtain triethylene glycol diacetate; the multifunctional catalyst is prepared from mesoporous silicon dioxide microspheres, 3-mercaptopropyltrimethoxysilane, 4-vinyl benzo-18-crown ether, sodium ethoxide, absolute ethyl alcohol, an ethanol solution of tetrabutyl titanate and chlorosulfonic acid. The preparation method comprises the following steps: preparing the mesoporous silicon dioxide microspheres, 3-mercaptopropyltrimethoxysilane, 4-vinyl benzo-18-crown ether, sodium ethoxide, absolute ethyl alcohol, the ethanol solution of tetrabutyl titanate and chlorosulfonic acid; the triethylene glycol diacetate prepared by the method has high yield and high purity, and can meet industrial production and market requirements.

The present disclosure is directed polymer-free, non-composite densified carbon nanotube (DCN) structures from thin carbon nanotube (CNT) films and methods of making the same. CNT thin films can be cut, folded, stacked and pre-arranged in the form of cylinders, discs, domes, frames, gaskets, jars, rings, sacks, seals and sheets on a smooth reaction vessel surface and subsequently densified with the use of chlorosulfonic acid (HClSO3) at elevated temperatures. The disclosed DCN structures can be used as EMI shielding, lightweight structural and functional components in extreme conditions commonly encountered in space exploration, polar expeditions and military operations, and also as hydrophilic filtration media that resist surface fouling and provide high flux.

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 discloses a system for improving pollution reduction and carbon reduction of a constructed wetland-microbial electrolysis cell by adding fulvic acid and an operation method thereof, and belongs to the field of ecological environment governance, the system comprises a water inlet system, a purification system, a water outlet system, an adder and an intelligent detection system; the purification system comprises more than one purification unit, and different connection relations are constructed through opening and closing of valves; wastewater input from the water inlet system is discharged from the water outlet system after reaching the standard through the adsorption-electrolysis purification effect of the purification system, the intelligent detection system dynamically judges whether fulvic acid needs to be added or not and the adding amount according to the water quality condition of inlet water, meanwhile, the operation mode is accurately adjusted, the treatment effect is remarkably improved, and carbon emission is remarkably reduced. The method has the advantages of being good in treatment effect, stable in operation, convenient to operate and run and the like, particularly realizes precise dynamic addition according to different working conditions to improve the pollution and carbon reduction effect of the constructed wetland, and has the advantages of high intelligence, low carbon and greenness.

Disclosed are sulfated cellulose nanofibrils, methods of making sulfated cellulose nanofibrils, and methods of spinning the sulfated cellulose nanofibrils into high-strength fibers. The sulfated cellulose nanofibrils may be formed using a chlorosulfonic acid treatment.

The invention belongs to the technical field of insecticides, and particularly relates to a synthetic method of a hexythiazox intermediate, which comprises the following four steps: S1, preparing erythro-1-p-chlorophenyl-2-amino-1-bromo-propane; s2, preparation of the erythro-1-p-chlorophenyl-2-aminopropanethiol, and preparation of the erythro-1-p-chlorophenyl-2-aminopropanethiol; s3, preparation of the trans-1-p-chlorophenyl-2-amino-propyl-O-isopropyl thiocarbonate hydrochloride, and preparation of the trans-1-p-chlorophenyl-2-amino-propyl-O-isopropyl thiocarbonate hydrochloride; and S4, preparation of a hexythiazox intermediate, namely, trans-5-(4-chlorphenyl)-4-methyl thiazolidone. According to the invention, the use of highly toxic carbon disulfide, corrosive chlorosulfonic acid, carcinogenic benzyl chloride and other high-risk reagents is completely abandoned, the operation risk is reduced, no malodorous gas is discharged, the occupational health and safety of operators and the environment are fundamentally guaranteed, meanwhile, the generation of acidic wastewater and sulfur-containing hazardous waste is solved, and the production cost is reduced. And a green chemical atom economy principle is met.

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 is suitable for the technical field of fine chemical engineering, and provides a synthesis method of sulpiride impurity 2-hydroxy-5-sulfanilamide benzamide, which comprises the following specific steps: Step 1, taking salicylic acid as a raw material, taking DMF as a catalyst, and carrying out acylation reaction with thionyl chloride to obtain acylation liquid, and entering the next process; 2, ammoniating the acylation liquid with ammonia water at a low temperature to obtain salicylic acid formamide, and drying to obtain an intermediate 1; 3, TMS-Cl is used for protecting phenolic hydroxyl groups, then chlorosulfonic acid is dropwise added, a chlorosulfonation reaction is carried out, and an intermediate 2 solution is obtained after the reaction is completed; and Step 4, dropwise adding the solution of the intermediate 2 into stronger ammonia water for reaction, carrying out suction filtration, and recrystallizing with ethanol to obtain the sulpiride impurity 2-hydroxy-5-sulfanilamide benzamide. The route synthesis is simple, and the quality can reach 95% or above; in addition, the method has the advantages of cheap and easily available raw materials, mild reaction conditions, low energy consumption, simple process structure, easy operation and the like.

The invention provides fluorenyl magnolol light-cured solder resist ink and a preparation method thereof, the solder resist ink comprises the following raw material components by mass: 20%-60% of fluorenyl magnolol light-cured resin, 10%-25% of a reactive diluent, 10%-30% of a nano filler, 1%-5% of a photoinitiator, 0.1%-5% of an auxiliary agent, and the balance of a solvent, the fluorenyl magnolol light-cured resin is prepared by reacting 9-fluorenylidene acetic acid with thionyl chloride to generate an intermediate product fluorenyl anhydride, and then reacting the intermediate product fluorenyl anhydride with magnolol. Wherein the molar ratio of magnolol to thionyl chloride to 9-fluorenylidene acetic acid is 1: (2-4): (2-4). The preparation process is simple, toxic by-products are avoided, the prepared solder resist ink has excellent flame retardance, heat resistance and adhesive force, low dielectric constant and high hardness, the problems of high dielectric loss, insufficient flame retardance and BPA toxicity of traditional ink are solved, and the solder resist ink is completely suitable for production and manufacturing of PCB substrates for high-frequency communication.

The invention discloses a carbon nanotube / graphene composite fiber and a preparation method thereof, and the preparation method comprises the following steps: mixing graphene powder with chlorosulfonic acid to obtain a graphene / chlorosulfonic acid dispersion liquid; immersing a carbon nanotube into the graphene / chlorosulfonic acid dispersion liquid, and drafting the carbon nanotube fiber; and taking out the carbon nanotube fiber, and carrying out heat treatment under a protective atmosphere to obtain the carbon nanotube / graphene composite fiber silk yarn. According to the invention, chlorosulfonic acid is used for generating protonation on carbon nanotube fibers, so that the carbon nanotube fibers are swelled, combination between tube bundles is removed, and conditions are provided for recombination and re-orientation of an internal structure; the graphene two-dimensional sheet structure is axially inserted into gaps of the carbon nanotubes in the drafting process to cooperatively construct an orderly arranged three-dimensional network structure, so that the orientation degree is improved, the pore structure is compressed, the defect density is reduced, the interface bonding force and the load transmission efficiency are enhanced, and the mechanical properties of the fiber under quasi-static state and high strain rate are remarkably improved.

The invention discloses a PVDF / PFA composite filter material for sewage treatment and a preparation method of the PVDF / PFA composite filter material, and relates to the technical field of water treatment. When the filtering material is prepared, firstly, N-propenylimidazole and 1-chloro-3-phenylpropane react to prepare vinyl imidazolium salt, PVDF subjected to alkali treatment is grafted with the vinyl imidazolium salt, then the PVDF and 5-aza-uracil react, and modified PVDF is obtained; secondly, enabling resorcinol, 3, 5-dihydroxybenzoic acid and formaldehyde to react to obtain porous microspheres, and sulfonating the porous microspheres through chlorosulfonic acid to obtain modified microspheres; finally, PVDF, PFA, polyoxyethylene and the modified microspheres are mixed and subjected to melt spinning, and a fiber membrane is prepared; and carrying out in-situ generation of ferroferric oxide, and activating with hypochlorous acid to obtain the PVDF / PFA composite filter material for sewage treatment. The filter material prepared by the invention has good antibacterial, hydrophilic and photocatalytic degradation properties.

The invention relates to an isoindole thioimine compound, preparation thereof and application of the isoindole thioimine compound as a sigma-2 receptor inhibitor. Catechol and isobutene are subjected to a series of reactions under certain conditions to obtain a solid product; carrying out a series of reactions on o-xylene and chlorosulfonic acid under certain conditions to obtain an oily product; and reacting the solid product with the oily product under a certain condition to obtain the isoindole thioimine compound. Compared with the prior art, when the isoindole thioimine compound prepared by the invention is combined with a sigma-2 receptor and allosteric regulates a sigma-2 receptor compound, the combination of adjacent A beta oligomers and a receptor on synapse is unstable, so that the A beta oligomers are removed from the synapse, the activity of the sigma-2 receptor can be effectively inhibited, and the activity of the sigma-2 receptor can be inhibited. The compound can be further used for preparing new medicines for treating tumors and neurodegenerative diseases.

The invention discloses a synthesis method of mannitol carbonate sulfate, and belongs to the technical field of organic synthesis. The synthesis method provided by the invention comprises the following steps: reacting 1, 3, 4, 6-tetrachloro-2, 5-hexanediol with chlorosulfonic acid in the presence of an acid-binding agent to obtain an intermediate solution as shown in a formula (II); formula (II); and mixing the intermediate solution as shown in the formula (II) with anhydrous carbonate, heating to a first set temperature for reaction, and then heating to a second set temperature for reaction in the presence of a phase transfer catalyst to obtain the mannitol carbonic sulfate. The whole process route is short, the yield is high, and the total yield of two steps reaches 88% or above; meanwhile, few by-products are generated, the purification difficulty is low, the reaction time is short, few hazardous wastes are generated, operation is easy and convenient, and industrial large-scale production is facilitated.

This invention relates to the field of mineral processing technology, specifically to an environmentally friendly copper-molybdenum separation inhibitor, its preparation method, and its application. The method includes: mixing starch and formamide, stirring at room temperature, cooling in an ice-water bath at -5°C, slowly adding chlorosulfonic acid at this temperature to initiate a sulfonation reaction, neutralizing to pH 7-8 with sodium hydroxide solution after the reaction, adding anhydrous methanol to precipitate the product, and washing and drying to obtain the sulfonated anionic starch polymer DGSS. The inhibitor is applied to the flotation separation of copper-molybdenum mixed concentrates, combined with a closed-circuit process of one roughing, one scavenging, and four cleaning stages, employing a gradient reagent reduction and staged kerosene replenishment system from roughing to cleaning. This allows for selective inhibition of copper sulfide minerals such as chalcopyrite at extremely low dosages, with minimal impact on the floatability of molybdenite. It completely avoids the use of toxic substances such as cyanide, Knox reagent, or sodium sulfide, exhibiting good selectivity, low reagent consumption, environmental friendliness, and a simple preparation process that is easy to industrialize.

A macroporous cation exchange resin and its preparation and application method are disclosed. The method involves dispersing polystyrene-divinylbenzene microspheres in dichloroethane to obtain a microsphere suspension. A sulfonating agent, a mixture of fuming sulfuric acid and chlorosulfonic acid, is then slowly added dropwise under cooling and stirring conditions. After the addition is complete, heating is initiated to trigger a polysulfonation reaction. Once the reaction is complete, the reaction mixture is slowly poured into ice water and continuously stirred and diluted until the solution pH reaches 2.5. The solution is then filtered, washed, and dried to obtain a solid resin. This invention simultaneously introduces a matched number of sulfonic acid groups and sulfone groups onto the polystyrene-divinylbenzene backbone. Utilizing the electron-withdrawing effect of the sulfone groups and the rigid framework they form, the stability of the C-H and C-S bonds in the resin is enhanced. This solves the problems of resin structure damage, rapid decline in separation performance, and significantly shortened service life associated with existing cation exchange resins used in treating chromium plating aging solutions.

The invention relates to the technical field of intermediate synthesis, and provides a method for synthesizing 2-methyl-3, 4, 5-trifluorophenol, which comprises the following steps: S1, carrying out chloromethylation reaction on 3, 4, 5-trifluorobromobenzene serving as a raw material under the action of paraformaldehyde and chlorosulfonic acid to obtain 2-chloromethyl-3, 4, 5-trifluorobromobenzene; s2, the 2-chloromethyl-3, 4, 5-trifluorobromobenzene is subjected to a reduction reaction, and 2-methyl-3, 4, 5-trifluorobromobenzene is obtained; s3, 2-methyl-3, 4, 5-trifluorobromobenzene is subjected to a substitution reaction, hydrolysis, crystallization and filtration, and 2-methyl-3, 4, 5-trifluorophenylboronic acid is obtained; s4, 2-methyl-3, 4, 5-trifluorophenylboronic acid is subjected to an oxidation reaction, and 2-methyl-3, 4, 5-trifluorophenol is obtained; the crystallization solvent is composed of an ether solvent and water. According to the technical scheme, the problems of high cost and low yield in synthesis of 2-methyl-3, 4, 5-trifluorophenol in related technologies are solved.

The invention discloses a synthesis method of sulfachloropyrimidine, which comprises the following steps: taking paranitroaniline and 4, 6-dichloropyrimidine as raw materials, synthesizing acyl chloride by diazotization and sulfonylation of paranitroaniline, generating aminopyrimidine by ammonification of 4, 6-dichloropyrimidine, condensing aminopyrimidine and acyl chloride, and then synthesizing sulfachloropyrimidine by reduction. According to the method, chlorosulfonic acid is not used in the reaction process, the reaction treatment is simple, and the safety risk is reduced. Acid used in the chlorosulfonation process and ammonia used in the ammonification process can be recycled and reused, the product yield reaches 76.2%, and the quality meets the standard requirement. The process can improve the yield and reduce the production cost, the production process is easy to control, less three wastes are generated, and the environmental pollution is small.

The invention relates to the technical field of fine chemical engineering, in particular to a method for recycling kettle residues in the production process of bis (chlorosulfonyl) imide. The innovative method focuses on effective recovery and reutilization of the kettle residues generated in the existing production process for the first time, so that many challenges such as high difficulty in treatment of the kettle residues, high environmental pollution risk, strong substance corrosivity and operation danger are successfully handled; the atom economic efficiency of a synthesis path of sulfamic acid, chlorosulfonic acid and thionyl chloride is also obviously improved. The comprehensive yield of the method can reach up to 99%, and the purity of the bis (chlorosulfonyl) imide product prepared through the kettle residue recovery reaction exceeds 98.5%, so that the strict requirement of downstream application on the purity of the bis (chlorosulfonyl) imide product is fully met.

This invention discloses a method for directly preparing bis(fluorosulfonyl)imide from aminosulfonic acid, chlorosulfonic acid, and oxaloyl fluoride in a one-step reaction. This method has the advantages of simple operation, mild reaction conditions, fast reaction speed, and easy product purification.

The invention discloses a synthesis method of a thioether compound. The synthesis method comprises the following steps: reacting 3-fluorotoluene with chlorosulfonic acid to obtain 4-fluoro-2-methylbenzenesulfonyl chloride; the preparation method comprises the following steps: dissolving 4-fluoro-2-methylbenzenesulfonyl chloride with acetic acid, adding acetic anhydride and red phosphorus, heating to 80-90 DEG C, adding elemental iodine in batches, and reacting to obtain (2-methyl-4-fluorophenyl) thioacetate; the preparation method comprises the following steps: dissolving (2-methyl-4-fluorophenyl) thioacetate with methanol, adding sodium formaldehyde sulfoxylate and potassium carbonate under the protection of nitrogen, and reacting; cooling the system to room temperature, dropwise adding 2, 2, 2-trifluoroethyl trifluoromethanesulfonate, and reacting to obtain (4-fluoro-2-methylphenyl) (2, 2, 2-trifluoroethyl) sulfane; the preparation method comprises the following steps: dissolving (4-fluoro-2-methylphenyl) (2, 2, 2-trifluoroethyl) sulfane with concentrated sulfuric acid, adding NBS (N-bromosuccinimide), and reacting to obtain (4-fluoro-5-bromo-2-methylphenyl) (2, 2, 2-trifluoroethyl) sulfane.

The application belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of furosemide. The preparation method of furosemide comprises the following steps: chlorosulfonation: reacting chlorosulfonic acid and 2,4-dichlorobenzoic acid, hydrolyzing, filtering, and obtaining 2,4-dichloro-5-sulfonyl chlorobenzoic acid; amination: adding 2,4-dichloro-5-sulfonyl chlorobenzoic acid into ammonia water, reacting, neutralizing, filtering, purifying, and obtaining 2,4-dichloro-5-sulfonamidobenzoic acid; condensation: reacting 2-furfurylamine and 2,4-dichloro-5-sulfonamidobenzoic acid, and obtaining furosemide crude product; decolorization: adding the furosemide crude product into a saturated sodium bicarbonate solution, adding activated carbon for decolorization, neutralizing, and crystallizing, and thus furosemide product is obtained. The raw material used in the application is easy to obtain and low in price, the comprehensive reaction period is short, the amount of hazardous waste generated is small, the prepared furosemide is high in purity and high in total yield, the comprehensive cost of the whole preparation process is low, and the application is suitable for industrial production.

The utility model relates to the technical field of waste acid recycling, in particular to a chlorine-containing waste sulfuric acid regeneration device which comprises a first chloroethylene clean sulfuric acid storage tank, a chlorine dry sulfuric acid storage tank, an unqualified sulfuric acid storage tank, a first sulfuric acid storage tank, a second sulfuric acid storage tank, a second chloroethylene clean sulfuric acid storage tank and a cracking furnace. The chloroethylene clean sulfuric acid storage tank and the chlorine dry sulfuric acid storage tank are respectively communicated with the first sulfuric acid storage tank and the second sulfuric acid storage tank through sulfuric acid pipelines, and a jumper pipeline is arranged between the first sulfuric acid storage tank and the second sulfuric acid storage tank. The device is reasonable and compact in structure and convenient to use, sulfuric acid generated by cleaning vinyl chloride acetylene and sulfuric acid generated by electrolyzing and drying chlorine are mixed according to a certain proportion and then are conveyed to the cracking furnace through the sulfuric acid conveying pump to produce sulfur dioxide, and chloride ions are completely removed by the scrubber; the problems that chlorine-containing sulfuric acid is difficult to transport and chlorine volatilized in the using process seriously pollutes the environment are solved, and the method has the advantages of being safe, labor-saving, simple, convenient and efficient.

The utility model discloses a continuous reaction device for producing bis (chlorosulfonyl) imide, which belongs to the technical field of chemical equipment and comprises a horizontal reaction tank and a heat preservation tank, a feed port of the reaction tank is connected with a mixed feed liquid pipe, and a discharge port of the reaction tank is connected with the heat preservation tank through a conveying component; heating layers are arranged outside the reaction tank and the heat preservation tank, a plurality of communicated areas are arranged in the reaction tank and the heat preservation tank, a stirrer is arranged in each area, and a chlorosulfonic acid feeding hole is formed in the top of each area of the reaction tank; a discharge hole of the heat preservation tank is connected with the distillation device; exhaust pipes and condensation reflux assemblies are arranged at the tops of the reaction tank and the heat preservation tank. The chlorosulfonic acid is added into each area of the reaction tank in a multi-drop mode, the reaction tank heats materials through the heat preservation layer to ensure the temperature needed by reaction, and the materials enter the heat preservation tank to be subjected to continuous heat preservation to ensure full reaction of the materials; thionyl chloride in gas exhausted from the reaction tank and the heat preservation tank is cooled and recycled through the condensation backflow assembly, the production efficiency is improved, raw material waste is reduced, and the production cost is reduced.

The invention relates to the technical field of chlorosulfonic acid preparation, in particular to a chlorosulfonic acid preparation system and method based on plasma pretreatment of sulfur. A gas inlet of a plasma reactor is connected with an inert gas pipeline, and a feeding port of the plasma reactor is connected with a feeding pipeline; a discharge port of the plasma reactor is connected with a feed port of the reaction kettle through a discharge pipeline; a discharge port of the reaction kettle is connected with a feed port of the heat exchanger, a discharge port of the heat exchanger is connected with a feed port of the rectifying tower, and a discharge port of the rectifying tower is connected with the chlorosulfonic acid pipeline. According to the method, the sulfur is pretreated through the plasma, and the surface of the sulfur is bombarded and activated through the low-temperature plasma, so that the reaction activity of the sulfur is effectively improved, the subsequent synthetic reaction with chlorine is more sufficient, and the preparation efficiency and the product purity of chlorosulfonic acid are remarkably improved.

The present application relates to a kind of continuous synthesis device of p-toluenesulfonyl chloride and synthesis method thereof.The synthesis method described in the present application is as follows:(1) the chlorosulfonic acid of first addition, catalyst, organic solvent are mixed in the first static mixer to obtain mixed liquid A, the mixed liquid A, toluene are pumped into first microreactor respectively to carry out reaction to obtain reaction liquid;(2) the reaction liquid is discharged from the outlet of first microreactor and separates out liquid phase, the liquid phase, the chlorosulfonic acid of second addition are pumped into second microreactor with mixed liquid B in the second static mixer respectively and mixed, carry out reaction in second microreactor to obtain secondary reaction mixture;(3) secondary reaction mixture is discharged from second microreactor and separates out intermediate layer frozen crystallization, filtration, washing, obtains p-toluenesulfonyl chloride.The synthesis method of the present application accurately controls reaction temperature, time, material ratio, greatly improves the production efficiency of p-toluenesulfonyl chloride, green, safe and environmentally friendly.