14 results about "Chlorosulfonic acid" patented technology

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.

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.

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 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.

A kind of microporous sulfonated poly (ether ether ketone) membrane for reverse electrodialysis energy conversion, preparation method and application thereof belong to ion exchange membrane technical field. First, bisphenol fluorene, 4,4'-difluorobenzophenone, alkaline catalyst and water-removing agent are added into solvent to carry out nucleophilic polycondensation reaction to obtain poly (ether ether ketone) ;Second, it is dissolved in anhydrous dichloromethane, and chlorosulfonic acid / dichloromethane solution is added to carry out sulfonation reaction to obtain sulfonated poly (ether ether ketone) with different sulfonation degrees;Finally, it is dissolved and formed into film by solution casting method, the main chain is the copolymer of bisphenol fluorene and 4,4'-difluorobenzophenone, and the main chain contains rigid fluorenyl structural unit.The rigid fluorenyl structural unit of the application limits the conformational rotation of the main chain by steric hindrance, forms size-stable intrinsic microporous ion channel, realizes the rigidification of ion channel and the intrinsic microporous structure while maintaining the excellent film-forming property of SPEEK;Long-term operation stability is excellent, preparation process is simple, raw material cost is controllable, and it is suitable for reverse electrodialysis energy conversion field.

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 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 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.

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 present application belongs to the technical field of fine chemical intermediates, and particularly relates to a green process for continuously preparing 3-nitro-4-methyl benzene sulfonyl chloride. The present application discloses a method for continuously preparing 3-nitro-4-methyl benzene sulfonyl chloride, wherein o-nitrotoluene, sulfur trioxide I, polysulfide inhibitor and organic solvent I are mixed in a first static mixer, and then input into a first micro-reactor for reaction; a primary reaction mixture discharged from the first micro-reactor is mixed with chlorosulfonic acid, sulfur trioxide II, organic solvent II and sulfonyl chlorination promoter in a second static mixer, and the obtained mixture is input into a second micro-reactor for reaction; and a secondary reaction mixture discharged from the second micro-reactor is subjected to post-treatment to obtain 3-nitro-4-methyl benzene sulfonyl chloride.

The application discloses a chlorination process of sucrose-6-acetate, which comprises the following steps: preparing a Vilsmeier reagent by using DMF and chlorosulfuric acid under low-temperature conditions, releasing sulfur dioxide by heating, mixing the Vilsmeier reagent with 1,1,2-trichloroethane as a reaction raw material liquid, mixing the reaction raw material liquid with a pre-cooled DMF solution of sucrose-6-acetate through a pipeline mixer, performing high-temperature chlorination reaction and removing hydrogen chloride by using a three-stage continuous reactor, and sequentially neutralizing the chlorination liquid by using ammonia water and sulfuric acid, so that the target product can be obtained by controlling pH=7-7.5. The process flow is simple, the continuous process of low-temperature mixing, high-temperature reaction and neutralization reaction is realized, the complicated process of separating hydrogen chloride and sulfur dioxide can be omitted, the product yield is improved, the number of production equipment is reduced, the production cost is lowered, and the process has good industrial application value.

The application discloses a preparation method of a sulfonic acid-based porous organic polymer and application of the sulfonic acid-based porous organic polymer in adsorption of uranyl ions and trace metal ions. The preparation method comprises the following steps: firstly, benzylization modification is conducted on a cyclodextrin to obtain a benzylated cyclodextrin monomer; then, the benzylated cyclodextrin monomer is subjected to a Friedel-Crafts alkylation polymerization reaction with a linker under catalysis of a catalyst to construct a porous organic polymer with high crosslinking degree; and finally, chlorosulfonic acid is used for sulfonation modification to introduce high-density sulfonic acid group active sites. The obtained polymer combines the host-guest recognition ability of the cyclodextrin and the rapid mass transfer effect of the porous skeleton, and exhibits extremely fast adsorption kinetic response and excellent adsorption capacity. The material has simple preparation process and high stability, and is especially suitable for superfast extraction of ultra-low-concentration uranyl ions in seawater.