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94 results about "Chlorosulfuric acid" patented technology

Chlorosulfuric acid (IUPAC name: sulfurochloridic acid) is the inorganic compound with the formula HSO₃Cl. It is also known as chlorosulfonic acid, being the sulfonic acid of chlorine. It is a distillable, colorless liquid which is hygroscopic and a powerful lachrymator.

Green and environment-friendly sulfonamide amidation preparation method

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.
Owner:SHANDONG DASIFU MATERIAL TECH CO LTD

Methods of preparing densified carbon nanotube (DCN) structures and the uses thereof

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.
Owner:4TH PHASE TECH INC

Preparation method of high-purity bis (fluorosulfonyl) imide alkali metal salt

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.
Owner:ZHEJIANG UNIV +1

Fluorenyl magnolol light-cured solder resist ink and preparation method thereof

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.
Owner:FUJIAN FUQIANG PRECISION PRINTED CIRCUIT BOARD CO LTD +1

PVDF / PFA composite filter material for sewage treatment and preparation method of PVDF / PFA composite filter material

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.
Owner:GUANGDONG YULIN ENVIRONMENTAL TECHNOLOGY CO LTD

Synthesis method of mannitol carbonate sulfate

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.
Owner:安徽得壹能源科技有限公司

Environment-friendly copper-molybdenum separation depressant, preparation method and application thereof

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.
Owner:YIMEN HONGFA MINING CO LTD

Synthesis method of sulfachloropyrimidine

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.
Owner:ZHENGZHOU FUYUAN ANIMAL PHARMA +1

A method for preparing furosemide

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.
Owner:BEIJING JINGFENG PHARM (SHANDONG) CO LTD

Continuous reaction device for producing bis (chlorosulfonyl) imide

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.
Owner:HEBEI LIUHE CHEM CO LTD

Chlorosulfonic acid preparation system and method based on plasma pretreatment of sulfur

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.
Owner:JINCHUAN GROUP CO LTD +1

A continuous synthesis apparatus and method for p-toluenesulfonyl chloride.

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.
Owner:WUHAN INST OF TECH

Solid beta-h elimination promoter of sodium sulfamate salt and its preparation method and application

This invention discloses a solid sodium aminosulfonate β-H elimination promoter, its preparation method, and its application, relating to the technical field of β-H elimination promoters. The technical solution is as follows: S1, diethylenetriamine is dissolved in an organic solvent; S2, chlorosulfonic acid organic solution is added dropwise to the diethylenetriamine organic solution at 0-10℃ to carry out the reaction; after the addition is complete, the temperature is raised to continue the reaction; S3, the white solid generated by the reaction is filtered and washed with chloroform and ethanol respectively. The washed white solid is poured into anhydrous methanol and dispersed evenly. The reaction temperature is lowered to 0℃, sodium hydroxide is added for neutralization, and the solvent is removed by vacuum distillation. The resulting pale yellow solid is washed with ethanol and finally dried under vacuum to obtain the solid sodium aminosulfonate β-H elimination promoter. The solid sodium aminosulfonate β-H elimination promoter prepared by this invention has advantages such as high metal salt content, strong alkalinity, and easy separation, making it a promising additive for industrial application.
Owner:CHINA PETROLEUM & CHEMICAL CORP +1

Sulfonated calix [4] arene derivative and application thereof in resisting I-type herpes simplex virus

The invention discloses a sulfonated calix [4] arene derivative and application thereof in resisting I-type herpes simplex virus (HSV-1), and belongs to the field of biological medicine. The invention relates to a sulfonated calix [4] arene derivative, which has a structural general formula as follows: R is equal to The preparation method comprises the following steps: adding sodium hydride into a raw material C4A in a polar aprotic solvent to react with alkyl halide to obtain a C4AH or C4AD intermediate; and reacting the intermediate with chlorosulfonic acid in a chlorine-containing solvent, and adding an alkaline alcohol solvent for treatment to obtain the sulfonated calix [4] arene derivative. The calix [4] arene derivative has a relatively good inhibition rate on expression of HSV-1gB and gD genes, and does not have obvious cytotoxicity.
Owner:HENAN NORMAL UNIV

High-temperature-resistant oil displacement agent and preparation method thereof

This invention belongs to the field of petroleum extraction technology, specifically relating to a high-temperature resistant oil displacement agent and its preparation method. The method includes: in a nitrogen-filled reactor, under the action of a catalyst, trimethylolpropane allyl ether and 1,1,1,2,2,3,3,4,4,5,5,6,6-tridecylfluoro-8-iodooctane undergo an addition reaction; next, a sulfonation reaction occurs with chlorosulfonic acid; and finally, a substitution reaction occurs with dodecylamine to obtain the product oil displacement agent. The molar ratio of 1,1,1,2,2,3,3,4,4,5,5,6,6-tridecylfluoro-8-iodooctane, chlorosulfonic acid, dodecylamine, and trimethylolpropane allyl ether is 0.8-1.2:1.8-2.4:0.8-1.2:1. The molecular formulas of the main components of the oil displacement agent are as follows: [Insert molecular formula here]. This invention's high-temperature resistant oil displacement agent features low interfacial tension, good temperature resistance, and a high degree of enhanced oil recovery.
Owner:VICTORY OIL TIAN HUA BIN CHEM CO LTD

Post-treatment method and application for significantly improving the performance of carbon nanotube films

The post-treatment method includes the following steps: immersing the raw state carbon nanotube film in chlorosulfonic acid and allowing it to stand, then leaving it in the air to allow the chlorosulfonic acid molecules inside the carbon nanotube film to react with water molecules in the air, then generating sulfuric acid molecules inside the carbon nanotube film, promoting the introduction of water molecules into the carbon nanotube film, then placing it back in chlorosulfonic acid to chemically react with water molecules to generate hydrogen chloride gas, then expanding the carbon nanotube film, then stretching, immersing it again in the chlorosulfonic acid solution, and finally performing high-temperature vacuum annealing heat treatment. The tensile strength of the carbon nanotube film prepared according to this application is in the order of GPa, and its conductivity is 10 6 It is at the S / m level, has higher surface flatness, and facilitates compounding with other materials.
Owner:SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI

A method for preparing high-purity lithium bis(fluorosulfonyl)imide

The present invention provides a method for preparing high-purity lithium bis(fluorosulfonyl)imide, belonging to the fields of chemical synthesis and lithium battery technology. Bis(chlorosulfonyl)imide is prepared by heating, stirring, and refluxing aminosulfonic acid, stirring thionyl chloride, and chlorosulfonic acid. The bis(chlorosulfonyl)imide is fluorinated and then concentrated and refined with a good solvent. After concentration to a certain concentration, a poor solvent is added for crystallization, and the crude bis(fluorosulfonyl)imide is filtered to obtain a salt. The crude product is then salified with alkaline lithium and slurried with dichloromethane solvent. The lithium bis(fluorosulfonyl)imide is filtered and dried to obtain the lithium bis(fluorosulfonyl)imide. The tourmaline ceramic balls prepared by the present invention are loaded with a thiazole / Sb complex and an organic lithium co-catalyst, which enhances the activity of the catalyst and, together with the metal chloride, improves the selectivity of the fluorination reaction and reduces the occurrence of side reactions.
Owner:QUZHOU JIUZHOU CHEM IND CO LTD

Preparation process of tetrachlorophthalic anhydride

The invention relates to the technical field of preparation of chemical raw materials, in particular to a preparation process of tetrachlorophthalic anhydride, which comprises the following steps: S1, adding phthalic anhydride, chlorine, chlorosulfonic acid and a modified iodine catalyst into a reaction kettle for chlorination reaction to obtain a reacted material; and S2, transferring the reacted material into a crystallization kettle, carrying out cooling crystallization, introducing compressed air to recover chlorosulfonic acid, and carrying out temperature-controlled washing, centrifugal dewatering and drying to obtain a tetrachlorophthalic anhydride product. According to the preparation process, the iodine loss rate can be remarkably reduced, the catalytic efficiency and the reaction selectivity are improved, and finally high-purity and high-yield tetrachlorophthalic anhydride is prepared.
Owner:INNER MONGOLIA YINGLAI NEW MATERIALS CO LTD

Coal-tar pitch-based surfactant, its preparation method and application

The application discloses a coal-tar pitch-based surfactant and a preparation method and application thereof, and belongs to the technical field of surfactants. The coal-tar pitch-based surfactant is prepared by the following steps: taking coal-tar pitch as raw material, removing impurities, introducing chlorosulfonic acid groups on benzene rings in the molecular structure of the coal-tar pitch through a sulfonylation reaction of chlorosulfonic acid and phosphorus oxychloride, and then introducing a hydrophilic chain to the edge of the molecular structure of the coal-tar pitch through an esterification reaction between the chlorosulfonic acid groups and terminal hydroxyl groups on the hydrophilic chain to endow the coal-tar pitch with surface activity, so that the coal-tar pitch-based surfactant containing both a hydrophobic aromatic ring and a hydrophilic long chain is obtained. The central polycyclic aromatic ring structure of the coal-tar pitch-based surfactant is highly similar to the surface structure of Shenhua coal, and the coal-tar pitch-based surfactant and the Shenhua coal have strong pi-pi interaction and hydrophobic interaction, high adsorption fastness, and a long hydrophilic chain grafted at the edge, which can effectively provide steric hindrance and form a physical barrier between adjacent coal particles to effectively prevent the coal particles from gathering, so that the coal water slurry has low viscosity, good dispersibility and stability.
Owner:SHAANXI UNIV OF SCI & TECH

Method for preparing 5-fluoro-2-bromobenzotrifluoride through bromination

The invention relates to a method for preparing 5-fluoro-2-bromobenzotrifluoride through bromination, and relates to the technical field of organic synthesis.The method comprises the following steps that fluorobenzotrifluoride, an acid medium and a catalyst are added into a solvent, bromine is added at the temperature of-10 DEG C to 60 DEG C, the dropwise adding time is 1-6 h, heat preservation is conducted, a bromination reaction is conducted for 2-24 h, and reaction liquid is obtained; the acid medium comprises chlorosulfonic acid; the solvent comprises any one or two of dichloromethane, dichloroethane, trichloromethane and tetrachloromethane; the catalyst comprises any one or two of sulfur, sodium sulfide and potassium sulfide; filtering the reaction liquid, and standing and separating the filtrate to obtain an organic phase; the filter cake is a catalyst and can be repeatedly used; distilling and concentrating the organic phase to obtain a concentrated solution; and carrying out rectification separation on the concentrated solution to obtain the 5-fluoro-2-bromobenzotrifluoride. The method has the advantages of few reaction steps, simplicity in operation and environmental friendliness, and the product has high yield and high purity.
Owner:NANTONG DONGCHANG CHEM IND CO LTD

Carbon nanotube composite fiber, method for preparing the same, and use thereof

The application provides a preparation method of carbon nanotube composite fiber, comprising the following steps: S1, preparation of core layer fiber: mixing to obtain polymer / carbon nanotube composite raw material, dispersing in chlorosulfonic acid to form a spinning stock solution; preparing a flexible high-thermal-conductivity core layer fiber with densification and high-orientation structure through wet spinning; S2, preparation of sheath layer: vacuum plating film is carried out on the fiber prepared in S1 to deposit a layer of insulating film on the surface of the fiber through monomer polymerization, and the carbon nanotube composite fiber is prepared. The carbon nanotube composite fiber prepared by the application has flexibility, high thermal conductivity and high resistivity, and has a very broad application prospect in the fields of thermal interface materials and electronic device thermal management materials.
Owner:PEKING UNIV

Chlorosulfonic acid metering tank

The utility model relates to the related technical field of chlorosulfonic acid, in particular to a chlorosulfonic acid metering tank, which comprises a metering tank, a discharge pipe and a placing frame, the lower surface of the metering tank is connected with the discharge pipe, the placing frame is arranged on the outer side of the metering tank, and a stirring mechanism is arranged on the inner side of the metering tank. And a connecting mechanism is arranged on the upper surface of the metering tank. According to the chlorosulfonic acid metering tank, pipeline connection is easy and convenient, the second connecting pipe is in butt joint with the first connecting pipe, extrusion sealing is achieved through the sealing pipe, the rubber ring and the fixing ring, and the connecting ring is fixed through the bolt, operation is easy, sealing is good, chlorosulfonic acid leakage is effectively prevented, and operation safety is guaranteed; chlorosulfonic acid is uniformly mixed by stirring, concentration difference and precipitation are eliminated, accurate metering is guaranteed, constant concentration of taken components is ensured, accurate control of a subsequent process is facilitated, temperature adjustment of a heating function is realized according to requirements, and chlorosulfonic acid reaches a proper reaction state.
Owner:TONGLIAO XINGLU BIOTECHNOLOGY CO LTD

A method for continuously preparing 4-chlorobenzenesulfonyl chloride

The application discloses a method for continuously preparing 4-chlorobenzenesulfonyl chloride, and the 4-chlorobenzenesulfonyl chloride is prepared through a continuous equipment, and the specific steps are as follows: step one, 4-chlorobenzenesulfonic acid is dissolved in halogenated hydrocarbon to prepare a 4-chlorobenzenesulfonic acid solution for standby; step two, the 4-chlorobenzenesulfonic acid solution and chlorosulfonic acid with a mass concentration of 99% are mixed in a mixing pump; step three, the 4-chlorobenzenesulfonyl chloride is prepared through temperature control and stirring reaction of the mixed solution in an n-stage continuous reaction equipment. The application has the following beneficial effects: through directional selection of halogenated hydrocarbon as chloroform, and through the continuous reaction device, the conversion rate of chlorosulfonic acid in the application reaches more than 92% compared with the selection of other halogenated hydrocarbons, and the molar yield of the 4-chlorobenzenesulfonyl chloride product can reach more than 82%.
Owner:浙江嘉化能源化工股份有限公司

Amphoteric surfactant and application thereof in IGBT (Insulated Gate Bipolar Translator) cleaning

The invention discloses an ampholytic surfactant and a preparation method thereof. The surfactant is a novel surfactant with two hydrophilic head groups and two hydrophobic tail chains and containing a rigid structure, benzoic acid and thionyl chloride are subjected to a substitution reaction to generate benzoyl chloride, then benzoyl chloride and 3-dimethylamino propylamine are subjected to a reaction to obtain N-[3-(dimethylamino) propyl] benzamide, and the N-[3-(dimethylamino) propyl] benzamide is subjected to a reaction to obtain N-[3-(dimethylamino) propyl] benzamide. Reacting N-[3-(dimethylamino) propyl] benzamide with alkyl bromide to obtain a quaternary ammonium salt intermediate product; and finally carrying out addition reaction on the quaternary ammonium salt intermediate and sodium bromoethanesulfonate to obtain the quaternary ammonium salt. According to the ampholytic surfactant prepared by the preparation method disclosed by the invention, the strong acting force of anion and cation bonds is utilized, so that the distance between hydrophilic head groups is smaller than that of a common surfactant, the critical micelle concentration of the ampholytic surfactant is lower, and the ampholytic surfactant has better emulsifying performance and cleaning capability, so that the ampholytic surfactant has better performance in the field of cleaning of IGBT chips.
Owner:FUZHOU UNIV

A PVDF / PFA composite filter material for wastewater treatment and its preparation method

This invention discloses a PVDF / PFA composite filter material for wastewater treatment and its preparation method, relating to the field of water treatment technology. In preparing the filter material, the invention first reacts N-propenylimidazolium with 1-chloro-3-phenylpropane to obtain a vinylimidazolium salt; then, alkali-treated PVDF is grafted with the vinylimidazolium salt and reacted with 5-azauracil to obtain modified PVDF; secondly, resorcinol, 3,5-dihydroxybenzoic acid, and formaldehyde are reacted to obtain porous microspheres, which are then sulfonated with chlorosulfonic acid to obtain modified microspheres; finally, PVDF, PFA, polyethylene oxide, and modified microspheres are mixed and melt-spun to prepare a fiber membrane; then, iron(III) oxide is generated in situ and activated with hypochlorous acid to obtain the PVDF / PFA composite filter material for wastewater treatment. The filter material prepared by this invention exhibits excellent antibacterial, hydrophilic, and photocatalytic degradation properties.
Owner:GUANGDONG YULIN ENVIRONMENTAL TECHNOLOGY CO LTD

Foaming agent for oil extraction and preparation method thereof

The invention belongs to the technical field of oil exploitation, and particularly relates to a foaming agent for oil exploitation and a preparation method thereof. The preparation method comprises the following steps: (1) adding 5-heptylbenzene-1, 3-diol and a catalyst into a high-pressure reaction kettle, purging a pipeline and the reaction kettle with nitrogen, vacuumizing, stirring, heating to 80-85 DEG C, stopping vacuumizing, adding epoxypropane at one time, carrying out heating and heat preservation reaction for the first time, introducing ethylene oxide, carrying out heating and heat preservation reaction for the second time, and cooling to room temperature; and (2) adjusting the pH value to 5-6 by using phosphoric acid, cooling to below 10 DEG C, dropwise adding chlorosulfonic acid, and controlling the temperature to react to obtain the foaming agent. Based on 1 mole part of 5-heptylbenzene-1, 3-diol, the dosage of the propylene oxide is 4-20 mole parts, the dosage of the ethylene oxide is 10-80 mole parts, and the dosage of the chlorosulfonic acid is 1.8-2.8 mole parts. The foaming agent has the advantages of large foaming volume, long drainage half-life period, salt resistance, hardness resistance and temperature resistance.
Owner:VICTORY OIL TIAN HUA BIN CHEM CO LTD

A method for synthesizing 4-tert-butyl-2,6-diformylphenol

The invention provides a synthesis method of 4-tert-butyl-2,6-diformylphenol, and relates to the technical field of electronic material synthesis. The method comprises the following steps: S1, placing chlorosulfonic acid in a reaction bottle 1, connecting an air guide tube, adding 4-tert-butylphenol, CuCl, anhydrous AlCl3 and benzene into a reaction bottle 2, reacting to obtain a mixed reaction liquid, and connecting a tail gas absorption device; S2, placing formic acid in a constant drop, and dropping the acid into the reaction bottle 1 at a constant rate; S3, quenching, filtering and extracting the mixed reactants to obtain a crude 4-tert-butyl-2,6-diformylphenol product; and S4, using a solution for recrystallization comprising cyclohexane, wherein the volume-to-mass ratio of the solution used in the recrystallization to the crude 4-tert-butyl-2,6-diformylphenol product is 10-13:1. The present invention adopts the above-mentioned synthesis method of 4-tert-butyl-2,6-diformylphenol, which solves the problems of low yield and low purity in the synthesis process of 4-tert-butyl-2,6-diformylphenol in the related art.
Owner:HEBEI CHIRAL STAR TECH CO LTD

A method for continuously preparing lithium bis(fluorosulfonyl)imide

The present invention relates to the technical field of preparation methods of lithium bisfluorosulfonyl imide, and in particular to a method for continuously preparing lithium bisfluorosulfonyl imide, comprising the following steps: chlorosulfonic acid and chlorosulfonyl isocyanate react under the action of a copper complex catalyst to generate bischlorosulfonyl imide; hydrogen fluoride gas is introduced into the bischlorosulfonyl imide to obtain bisfluorosulfonyl imide under the action of an iron complex catalyst; a lithium salt is added to an organic solvent, and bisfluorosulfonyl imide is added during stirring to obtain the product lithium bisfluorosulfonyl imide. The present invention does not require changing the reaction vessel in different steps, nor does it require separating and purifying the intermediate product before putting it into the next reaction step, but directly obtains the product by continuous reaction, and maintains a high yield; in addition, the introduction of the copper complex catalyst and the iron complex catalyst further reduces the temperature required for the reaction, saving energy while improving the safety of the reaction process.
Owner:SHANDONG LINGKAI PHARM CO LTD

Cardanol-based sterically hindered sulfonate surfactant and preparation method thereof

The preparation method of the cardanol-based sterically hindered sulfonate surfactant comprises the following steps: dropwise adding a catalyst acidic eutectic solvent into cardanol or hydrogenated cardanol and styrene in a molar ratio of 1: 2.1 for 1 hour, carrying out an alkylation reaction at 50 DEG C for 3.5 hours, carrying out a reaction for 2 hours, and carrying out solid-liquid separation, so as to obtain the cardanol-based sterically hindered sulfonate surfactant. An alkylated product is obtained; and mixing the alkylated product with chlorosulfonic acid according to a certain ratio, taking dichloromethane as a solvent, carrying out sulfonation reaction, carrying out neutralization reaction by using a 20% NaOH solution until the pH value is 8-10, and carrying out rotary evaporation, extraction, washing, suction filtration and drying on the crude product to obtain the cardanol-based sterically hindered sulfonate surfactant. The cardanol-based steric hindrance type sulfonate surfactant has better high temperature resistance, salt resistance, hydrolysis resistance and emulsifying property, can realize a middle-phase microemulsion phase state, and is applied to an oil displacement technology for improving the recovery ratio of an oil field.
Owner:NORTHEAST GASOLINEEUM UNIV

Dichlorosulfimide as well as preparation method and reaction device thereof

The invention provides bis (chlorosulfonyl) imide as well as a preparation method and a reaction device thereof, the preparation method comprises the following steps: 1) preparing mixed slurry containing sulfamic acid and chlorosulfonic acid, pumping the mixed slurry into a continuous micro-channel reactor by using a metering pump, and carrying out amination reaction, so as to obtain an aminated slurry; an intermediate is obtained; 2) carrying out a chlorination reaction on a mixed system containing the intermediate and thionyl chloride in a tubular reactor to obtain a reaction product; and 3) carrying out separation treatment on the reaction product to obtain the bis (chlorosulfonyl) imide. The preparation method provided by the invention can be used for preparing the bis (chlorosulfonyl) imide with high purity, and the preparation method is simple in process and easy to operate.
Owner:GUANGZHOU TINCI MATERIALS TECH