50 results about "Chlorosulfuric acid" patented technology

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 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.

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.

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.

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.

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.

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.

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.

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%.

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.

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.

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.

The present application relates to a kind of continuous preparation of dichlorosulfamide acid method and system, belong to the preparation technical field of nitrogen-containing compound.The continuous preparation of dichlorosulfamide acid method of the present application includes the following steps: chlorosulfonic acid, chlorosulfonyl isocyanate is continuously injected into microchannel reactor and circulates liquid and is reacted under the pressure of 0.5-5MPa, and microchannel reactor effluent material is carried out gas-liquid separation;The circulating liquid is part of liquid in the liquid obtained by gas-liquid separation.The method of the present application, by the liquid after gas-liquid separation part of material as circulating liquid continues to participate in the reaction of chlorosulfonic acid and chlorosulfonyl isocyanate, can improve the utilization rate of chlorosulfonic acid in the reaction system, reduce production cost;And can also improve the absorption rate of carbon dioxide, inhibit the generation of gas-liquid two-phase, avoid the continuous gas phase space in microchannel reactor, make the reaction in homogeneous state, ensure HClSI continuous, stable production.

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

The application discloses a synthesis method of 4-(aminoalkyl) benzene sulfonic acid compound and relates to the technical field of organic synthesis. Benzylamine or phenethylamine is dissolved in a halogenated hydrocarbon solvent, the temperature is lowered to 0-5 DEG C, chlorosulfonic acid is added dropwise for sulfonation reaction, after dropwise addition is completed, the temperature is raised to 40-65 DEG C for reaction until the raw material is completely reacted, the temperature is lowered to 0-5 DEG C, then C1-C4 alcohol solvent containing trace moisture is added into the reaction system as a quenching agent for quenching, after quenching, the halogenated hydrocarbon solvent is recovered by distillation, the remaining substance is cooled, crystallized, filtered and dried, and 4-(aminoalkyl) benzene sulfonic acid is obtained. In the application, n-butanol containing trace moisture (0.5-8%) is used as a quenching agent, the reaction of chlorosulfonic acid and water is diluted and buffered by alcohol, the heat release is gentle, there is no risk of material shock, and the operation safety is far superior to traditional ice water quenching.

The present application relates to the technical field of cyclohexanol preparation, and particularly discloses a catalyst system and a method for preparing cyclohexanol by using the catalyst system. The catalyst system is prepared by mixing silica and chlorosulfonic acid in an organic solvent, stirring and reacting at room temperature until no gas is emitted, and then separating and drying the solid, wherein the specific surface area of the silica is 100-400 m 2 / g; the weight ratio of the silica to the chlorosulfonic acid is 50:5-15. The catalyst system provided by the present application can achieve a high conversion rate of cyclohexene and a high yield of cyclohexanol in the reaction process of preparing cyclohexanol by indirect hydration of cyclohexene, and the selectivity of the cyclohexanol can reach more than 90%. Moreover, the preparation method is simple in process, high in economic benefit, and convenient for industrial production.

The application discloses a high-yield preparation process of tetrachlorophthalic anhydride, relates to the technical field of organic synthesis, and comprises the following steps: dissolving phthalic anhydride in chlorosulfonic acid, adding into a chlorination kettle, adding a catalyst, then performing temperature rising according to a certain procedure, starting to pass in chlorine when the temperature in the reaction kettle rises to 80-100 DEG C, adjusting and controlling the flow of chlorine, reacting while stirring, absorbing tail gas by using lye, and stopping the reaction when there is substantially no HCl gas escaping; filtering the material, recovering the catalyst solvent, and ensuring that the distillation temperature is not higher than 220 DEG C; after cooling, washing with cold water, centrifugal dehydration, and drying at 150-170 DEG C, tetrachlorophthalic anhydride is obtained; wherein the catalyst is a modified montmorillonite supported titanium tetrachloride catalyst. The preparation process of tetrachlorophthalic anhydride provided by the application has high yield and high purity, and is easy to be industrialized.

The invention belongs to the technical field of fracturing, and particularly relates to a temperature-resistant thickening agent for fracturing, and a preparation method of the temperature-resistant thickening agent comprises the following steps: modifying an aromatic ring on the surface of bentonite by using an aromatic ring silane coupling agent, reacting with chlorosulfonic acid to form a sulfonic acid group, and finally modifying a sulfonyl chloride group on the bentonite under the action of a chlorinating agent and a catalyst. Secondly, guar gum is modified with amino through an amino silane coupling agent, then under the catalytic action of triethylamine, the amino-modified guar gum and sulfonyl chloride groups on the modified bentonite are subjected to a nucleophilic substitution reaction to generate sulfonamide groups, and the modified guar gum / bentonite compound, namely the temperature-resistant thickening agent, is better in temperature resistance, salt resistance and anti-shearing effect, and can be used for preparing the high-temperature-resistant thickening agent. And the device can be suitable for more fracturing construction sites.

The present application relates to the field of lithium ion battery electrolyte additives, and particularly relates to a manufacturing method of lithium fluorosulfonate concentrate, comprising the following steps: (1) reacting chlorosulfonic acid with lithium fluoride in a non-aqueous solvent to generate lithium fluorosulfonate, and hydrogen chloride gas is generated in the reaction; (2) performing vacuum degassing on the reaction solution to remove hydrogen chloride and other gases remaining in the solution, and then filtering to remove the insoluble substances such as lithium fluoride contained therein. The present inventors use chlorosulfonic acid and lithium fluoride to prepare lithium fluorosulfonate, and chlorosulfonic acid belongs to a bulk raw material, which is easy to obtain as a raw material. In addition, there is no other side reaction problem in the reaction process, and the generated product is single. The purity and yield of the obtained product are very high, and it is very suitable for large-scale production in the industry of preparing electrolyte of lithium batteries.

The application provides a cellulose catalytic fermentation preparation method of industrial ethanol and a catalyst thereof, and belongs to the technical field of preparing industrial ethanol fuel from cellulose. The preparation method comprises raw material choline chloride-lactic acid eutectic solvent heat treatment, catalytic hydrolysis fermentation and product separation. The composite catalyst is prepared by compounding Zn-MOF-CNTs-OH composite precursor, lignin-cellulose-PMMA composite precursor, ammonium molybdate and melamine, sintering, NaOH etching, sequentially sulfonating by concentrated sulfuric acid and chlorosulfonic acid to introduce double acid sites, and finally mixing with ammonium iron citrate, nickel acetate, copper acetate and PVP-VA copolymer, and adding sodium borohydride aqueous solution to react. The crystalline structure of cellulose is broken by eutectic solvent pretreatment, the magnetic composite catalyst with double acid sites and metal alloy is used to realize efficient hydrolysis, the in-situ fermentation and catalyst regeneration process are combined, and the conversion efficiency and economy are significantly improved.

The invention discloses a flexible carbon fiber film for a polypyrrole super capacitor and a preparation method and application thereof, and belongs to the technical field of super capacitors. And immersing the polyimide fiber membrane in a mixed solution of chlorosulfonic acid and dichloroethane, sequentially carrying out gradient heating treatment, cleaning, alkali treatment, carbonization treatment at 700-850 DEG C, and immersion in a dilute nitric acid solution for treatment and activation to obtain the flexible carbon fiber membrane for the polypyrrole super capacitor. Experimental results show that the specific capacitance of the flexible carbon fiber membrane prepared by the method can reach 335 F / g, the flexible cycle stability is still kept at 89.7% after the flexible carbon fiber membrane is bent for 1000 times at 180 degrees, the surface resistance is as low as 0.78 omega / sq, the average pore size is controlled in a mesoporous interval of 5.5 nm, the preparation process is mild, and the prepared flexible carbon fiber membrane can integrate material flexibility, conductivity and capacitive performance and has good application prospects. And a new path is provided for a high-performance flexible super capacitor electrode material.

The application relates to a carbon-based liquid-liquid separation membrane and a preparation method and application thereof. First, a controllable oxidation method is adopted, graphite or carbon nanotubes and other carbon materials are oxidized by potassium permanganate in a high-chloric acid or chlorosulfonic acid aqueous solution, then a vacuum filtration method is adopted to uniformly deposit the oxidized carbon materials on the surface of a filter membrane, thus an excellent liquid-liquid separation membrane is obtained. The separation membrane can be used for efficient separation of a mixed liquid or emulsion of a polar solvent and a non-polar solvent, has a series of remarkable advantages such as simple method, high separation efficiency, repeated use and the like, and has a good market application prospect.

The invention provides a method for improving the reaction conversion rate of propyl acetate. The method for improving the reaction conversion rate of propyl acetate comprises the following steps: L1, adding propyl alcohol and acetic acid into an esterification tower, and carrying out esterification reaction under the catalysis of a blend of a solid acid catalyst and a filler to obtain crude propyl acetate at the top of the esterification tower; wherein the middle part of the esterification tower is provided with a filler area, and the filler area is filled with a blend of a solid acid catalyst and an inorganic filler; the filler area of the esterification tower is filled with a blend compounded by a solid acid catalyst and an inorganic filler. The preparation method comprises the following steps: firstly, carrying out surface modification on silicon dioxide through KH-560, and introducing an epoxy group; then reacting with polyethyleneimine to form amino-functionalized silicon dioxide; then reacting with amino POSS (Polyhedral Oligomeric Silsesquioxane) and epoxy polystyrene to obtain an intermediate product with a three-dimensional network structure; and finally, sulfonating through chlorosulfonic acid, and introducing a strongly acidic sulfonic acid site.

The invention discloses an on-line recovery system for a carbon nanotube composite fiber acetone coagulating bath solution. The system comprises a coagulating bath tank for bearing an acetone coagulating bath, an adsorption device for purifying the acetone coagulating bath, a liquid storage device for supplementing acetone and a corresponding circulation control unit, the control unit comprises a coagulating bath liquid level detection device, an acetone purity detection device, a circulating pump and a circulating controller. The method solves the problem that the coagulating bath gradually loses efficacy due to the reaction of chlorosulfonic acid and acetone during the batch preparation of the carbon nanotube fiber under the existing chlorosulfonic acid system, can realize the effective recovery of acetone, and reduces the cost. In addition, through systematic cooperative control, the preparation efficiency of the carbon nanotube fibers is improved, and large-scale preparation of the carbon nanotube fibers is promoted.

This invention discloses a method for preparing composite copper foil by electrochemical co-deposition of sulfonated graphene and copper sulfate electrolyte, comprising the following steps: S1, preparing sulfonated graphene: dispersing graphene or graphene oxide in an anhydrous organic solvent, and reacting it with chlorosulfonic acid under an inert atmosphere to generate sulfonated graphene functionalized with sulfonic acid groups; S2, preparing composite copper foil by electrochemical co-deposition: adding the sulfonated graphene prepared in step S1 to an acidic copper sulfate electrolyte to form a co-deposition electrolyte, and performing electrochemical co-deposition in an electrodeposition device, so that the sulfonated graphene and metallic copper are co-deposited on the cathode surface, thereby obtaining the composite copper foil. The sulfonated graphene / copper nanocomposite copper foil prepared by the method of this invention has significantly improved comprehensive performance compared with traditional 6μm pure copper foil and low-concentration dispersed samples.

The invention relates to a synthesis method of a sulfentrazone chloride intermediate. The method comprises the following steps: adding an intermediate A into a solvent, adding a catalyst, and stirring and mixing; the solvent is an inorganic solvent; the catalyst is ferric trichloride hexahydrate; slowly heating the mixture to 50-100 DEG C, adding a chlorination reagent, reacting for 1-10 hours, and keeping the temperature for 1 hour; the chlorination reagent is one of chlorine, liquid chlorine, thionyl chloride and sulfonyl chloride; separating out solid, filtering, washing a filter cake with dilute alkaline water, collecting to obtain a brown solid chloride intermediate B, drying in vacuum at 80 DEG C for 24 hours to obtain a product, and applying filtrate to the next batch. The method has the advantages that different chlorination reagents and different reaction solvents and catalysts are used in the chlorination reaction, reaction conditions are optimized, impurities are reduced, and higher reaction yield is obtained.

The invention relates to a preparation method of a sildenafil intermediate, and belongs to the field of pharmaceutical chemicals. A compound 4 is obtained through a nucleophilic substitution reaction of a compound 3 and a chlorosulfonation reagent, and generation of a regional impurity M4-01 is fundamentally avoided by adopting a strategy that the position of an ethyoxyl para-position of the compound 3 is occupied in advance. According to the preparation method, the intermediate is stable, the reaction condition avoids ultralow temperature, and the energy consumption is reduced; use of chlorosulfonic acid is avoided, and the process is green and environment-friendly; the post-treatment quenching operation is simple and convenient; the total yield can reach 90% or above, and the method is more suitable for large-scale industrial production.

The invention relates to the technical field of fiber reinforcement, in particular to a method for improving the braid ability of carbon nanotube fibers through continuous surface modification, which comprises the following steps: S1, preparing carbon nanotube fibers, and carrying out catalytic growth on a reaction liquid containing a carbon source, an additive and a catalyst under a chemical vapor deposition condition to obtain carbon nanotube fiber monofilaments; s2, carrying out continuous surface modification sizing treatment on the carbon nanotube fiber monofilaments, and sequentially drafting and introducing the carbon nanotube fibers into a slurry tank containing chlorosulfonic acid and ethylene glycol for infiltration and densification treatment; s3, twisting and bundling the carbon nano tube fibers subjected to surface modification treatment, and twisting and drafting the carbon nano tube fibers through a twisting device, so that a plurality of carbon nano tube fibers form a bundled fiber bundle; through a continuous surface modification process, the original properties such as the force, the electrical property and the wear resistance of the carbon nanotube fiber are changed, so that the weaving property of the carbon nanotube fiber is improved.