342 results about "Thionyl chloride" patented technology

The invention belongs to the technical field of wave-absorbing materials, and particularly relates to a monatomic modified carbon composite wave-absorbing material and a preparation method thereof. The method specifically comprises the following steps: S1, uniformly dispersing a pyrrole monomer and molybdenum trioxide hydride by using a solvent, and reacting at room temperature for 3-6 hours to obtain an HM-PPy compound; s2, adding metalloporphyrin and thionyl chloride into N, N-dimethylformamide, uniformly mixing, and then adding 4-dimethylaminopyridine to obtain a raw material solution; s3, dispersing the HM-PPy compound into a N, N-dimethylformamide solution containing triethylamine, so as to obtain a turbid liquid; s4, dropwise adding the raw material solution into the turbid liquid, and stirring and reacting at room temperature for 20-25 hours to obtain HM-PPy-MPor; and S5, carrying out pyrolysis on the HM (at) PPy-MPor to obtain the monatomic modified carbon composite wave-absorbing material.

The invention provides a polyurethane material for leaking stoppage of a coal mine and a preparation method of the polyurethane material, and belongs to the technical field of polyurethane. The preparation method comprises the following steps: preparing melamine formaldehyde resin balls and ZnAl-LDHs, mixing and reacting the melamine formaldehyde resin balls and the ZnAl-LDHs to prepare LDH-MF composite balls, dipping in an iron salt solution, calcining to prepare composite balls, chloridizing with thionyl chloride, reacting with an ionic liquid and hyperbranched polyester to prepare IL / G composite balls, mixing with polyether polyol and a catalyst, adding into water, adding a foaming agent and silicone oil, heating, stirring and mixing, transferring into a mold, and carrying out extrusion molding to obtain a finished product. And adding diisocyanate, foaming, cooling to room temperature, drying and curing to obtain the polyurethane material for leaking stoppage of the coal mine. The prepared polyurethane material for leaking stoppage of the coal mine has good mechanical property, high temperature resistance and antibacterial property, good flexibility, good antistatic property and obviously improved flame retardance, and has a wide application prospect.

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 provides a method for producing 4, 4 '-dichlorodiphenyl sulfone by continuous reaction of a microchannel reactor, which comprises the following steps: uniformly mixing thionyl chloride and aluminum chloride to obtain a solution A; uniformly mixing hydrogen peroxide and glacial acetic acid to obtain a solution B; a first feeding pump and a second feeding pump are adopted for conveying chlorobenzene and a solution A into a first silicon carbide micro-channel reactor for reaction, an outlet of the reactor is connected with a gas-liquid separator, through separation, a gas phase is used for preparing a byproduct hydrochloric acid, and a liquid phase is a chlorobenzene solution of 4, 4 '-dichlorodiphenyl sulfoxide; and continuously conveying the chlorobenzene solution of 4, 4 '-dichlorodiphenyl sulfoxide to the second silicon carbide microchannel reactor by adopting a third feeding pump, and meanwhile, conveying the solution B to the second silicon carbide microchannel reactor by adopting a fourth feeding pump for reaction to prepare 4, 4'-dichlorodiphenyl sulfone. Compared with the prior art, the micro-channel reactor is used for continuous production, the mass and heat transfer effect is good, impurity generation is effectively inhibited, and the reaction time is shortened.

The invention relates to the technical field of composite materials, and discloses an epoxy resin composite material based on flexible chain segments and rigid fiber particles and a preparation method, the preparation method comprises the following steps: step 1, adding thionyl chloride SOCl2 into a cellulose nanofiber CNF solution, fully mixing, and reacting to obtain a chlorinated cellulose nanofiber CNF-Cl solution; 2, fully mixing the CNF-Cl solution and the aramid nanofiber ANF solution, adding a silane coupling agent, fully mixing and reacting, and removing the solvent to obtain the silane functionalized cellulose nanofiber modified aramid nanofiber fANF (at) CNF; and 3, adding the fANF (at) CNF into an epoxy resin EP matrix containing epoxy functionalized polydimethylsiloxane E-PDMS, fully mixing, adding a curing agent and an accelerant, and carrying out vacuum degassing and curing to obtain the required composite material. According to the composite material obtained by the invention, the strength, toughness and thermal performance of the epoxy composite dielectric are synergistically improved.

The invention discloses an antistatic fabric and a preparation method thereof, and relates to the technical field of fabrics. When the antistatic fabric is prepared, firstly, polyamide is grafted with 2-chloro-6-vinylpyridine under the action of an initiator, then the polyamide reacts with 2-amino-4-methoxypyrimidine-5-boronic acid pinacol ester, methoxyl is removed through boron tribromide, then the polyamide reacts with 2-diphenylphosphinobenzaldehyde, and modified polyamide is obtained; secondly, grafting tea polyphenol on the multi-walled carbon nanotube which is firstly treated by nitric acid and then treated by thionyl chloride, and then reacting with 4-[2, 2 ': 6', 2 ''-terpyridyl]-4 '-yl-thiophenol to obtain a modified multi-walled carbon nanotube; and finally, carrying out melt spinning on the modified polyamide, the modified multi-walled carbon nanotubes and the antibacterial agent to obtain antistatic fibers, and weaving the antistatic fibers to obtain the antistatic fabric. The antistatic fabric prepared by the invention has excellent flame retardance, electrical conductivity, ultraviolet resistance and oxidation resistance.

The invention discloses a preparation method of a high-elasticity optical cable, and relates to the technical field of sheath materials. When the high-elasticity optical cable is prepared, firstly, a carbon source gas is subjected to vapor deposition to prepare a spiral carbon nano tube, and the spiral carbon nano tube is subjected to nitric acid treatment and then reacts with thionyl chloride and aminopropyltrimethoxysilane to prepare a modified spiral carbon nano tube; the preparation method comprises the following steps: reacting 3-furoic acid, 2-mercaptobenzimidazole and neodymium chloride in an ethanol solution to prepare a fluorescent complex solution, reacting a styrene-butadiene-styrene block copolymer with ethyldiallylsilane, diethoxysilane and p-aminostyrene to prepare a pre-modified styrene-butadiene-styrene block copolymer; reacting the pre-modified styrene-butadiene-styrene block copolymer with a fluorescent complex solution to prepare a modified styrene-butadiene-styrene block copolymer, and preparing the sheath material from the modified spiral carbon nanotube, the modified styrene-butadiene-styrene block copolymer and polyethylene. And wrapping the sheath material on the optical cable core material, and rolling to obtain the high-elasticity optical cable. The high-elasticity optical cable prepared by the invention has excellent tensile fracture resistance and anti-aging performance.

The invention belongs to the technical field of synthesis of organic intermediates, and particularly relates to a synthesis method and a synthesis device of benzenesulfonyl fluoride. The synthesis method of the benzenesulfonyl fluoride comprises the following steps: firstly, adding hydrogen fluoride and sulfuryl chloride into a premixer, enabling the hydrogen fluoride and the sulfuryl chloride to sequentially pass through tubular reactors a, b and c, enabling the hydrogen fluoride and the sulfuryl chloride to enter a terminal reaction kettle for mixing reaction, controlling gas-liquid two-phase mixing reaction through the terminal reaction kettle and a vertical condenser a to prepare sulfuryl fluoride chloride, then mixing the sulfuryl fluoride chloride, benzene and a catalyst, and finally adding the benzenesulfonyl fluoride into the premixer to obtain the benzenesulfonyl fluoride. The method comprises the following steps: adding benzenesulfonyl fluoride into a sulfonation reaction kettle for reaction, controlling the sulfonation reaction through the sulfonation reaction kettle and a vertical filler b to obtain a mixed reaction solution, finally distilling the mixed reaction solution, and collecting fractions to obtain benzenesulfonyl fluoride. The synthesis method of the benzenesulfonyl fluoride provided by the invention is low in reaction condition requirement, stable, easy to control, low in unit consumption and easy in subsequent treatment, and the prepared benzenesulfonyl fluoride is high in yield and high in purity. The invention also provides a synthesis device adopted by the synthesis method of benzenesulfonyl fluoride.

The invention relates to a preparation method of high-yield and high-purity polyphenylene sulfide, and belongs to the field of oxidative polymerization. The technical problem to be solved by the invention is to provide a production method of polyphenylene sulfide with mild reaction conditions, high yield and high purity. According to the method, diphenyl disulfide is taken as a raw material, thionyl chloride is taken as a solvent, oxygen is taken as an oxidizing agent, a vanadium-based Lewis acid complex is taken as a catalyst, and the main technological process comprises the steps of feeding, synergistic action of the catalyst and the oxygen, polymerization, filtration, washing, drying and oxidative polymerization at normal temperature and normal pressure to obtain the high-yield and high-purity polyphenylene sulfide. The method is simple in process flow and mild in condition, does not need to introduce other polymerization additives, avoids the influence of metal sodium salt and other by-products generated by many preparation methods on the toughness of the product, and has the yield of almost 100% and high product purity.

The invention discloses a special antistatic polyethylene pipe material and a preparation method thereof. The antistatic polyethylene pipe special material comprises polyethylene, a modified antistatic agent, an antioxidant, a flame retardant and a compatilizer. The preparation method comprises the following steps: reacting thionyl chloride with a carboxylic acid functional group contained in a modifier to obtain a product, reacting the product with 4-amino-2, 6-bis (dimethylaminomethyl) phenol, and finally performing graft modification by using a grafting agent to obtain the modified antistatic agent. And carrying out melt extrusion and blending on the modified antistatic agent and other raw materials to prepare the antistatic polyethylene pipe special material. Compared with the prior art, the prepared special material for the polyethylene pipe is better in flame retardant property.

The invention belongs to the technical field of energy materials, further relates to the field of alkali metal batteries, and particularly relates to an electrolyte for an alkali metal-thionyl chloride secondary battery and application of the electrolyte. The electrolyte is salt capable of transmitting alkali metal ions, thionyl chloride and an additive; the additive is a salt of organic aniline cations. The additive is added into a basic electrolyte adopted by the alkali metal-thionyl chloride secondary battery. According to the present invention, with the introduced additive, the redox couple of the carbon positive electrode interface, which actually participates in the electrochemical reaction, can be changed, the potential and the capacity of the discharge platform under the large current density can be significantly improved, the voltage hysteresis phenomenon can be significantly improved, and the alkali metal-thionyl chloride secondary battery can obtain the excellent specific energy and the excellent energy efficiency. Compared with a comparison sample without addition of the additive, the battery using the additive provided by the invention has the advantages that the charge-discharge polarization is obviously reduced, and the discharge rate capability is improved. According to the battery using the additive provided by the invention, a primary battery is successfully converted into a secondary battery, and after 100 times of circulation, the cycle capacity retention rate of the secondary battery is remarkable.

The utility model provides a compound rectification system which comprises a first-stage rectification tower, a second-stage rectification tower and a third-stage rectification tower, a feed port of the first-stage rectification tower is communicated with a crude product tank through a crude product pipeline, and a steam outlet in the top of the first-stage rectification tower is communicated with a steam inlet of a first condenser through a first steam pipeline; the lower section of the second-stage rectifying tower is communicated with a condensate outlet of the first condenser through a first condensing pipeline, the lower section of the second-stage rectifying tower is communicated with the lower section of the first-stage rectifying tower through a material transferring pipeline, and a steam outlet in the top of the second-stage rectifying tower is communicated with a steam inlet of the second condenser through a second steam pipeline; a condensate outlet of the second condenser is communicated with the refined product tank through a second condensation pipeline; a water inlet of the first condenser and a water inlet of the second condenser are communicated with the condensate water storage tank through water inlet pipelines; wherein sulfur layers are arranged on the upper sections of the primary rectifying tower and the secondary rectifying tower. According to the invention, the separation efficiency of thionyl chloride is improved, so that the purity of thionyl chloride obtained by rectification is relatively high.

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 discloses a preparation method of 3-quinuclidinone hydrochloride, which comprises the following steps: carrying out temperature control reaction on 4-picolinic acid and chloroacetic acid under alkaline water conditions to obtain an aqueous solution of a compound a, and directly entering the next reaction without post-treatment after the reaction is finished; adding a reducing agent alkaline water system into the aqueous solution of the compound a, controlling the temperature to react, controlling the temperature to adjust the pH value to 5-5.5 after the reaction is finished, extracting with n-butyl alcohol, and drying to obtain an n-butyl alcohol solution of a compound b, and directly entering the next reaction step; wherein the reducing agent is one of sodium borohydride and potassium borohydride; dropwise adding thionyl chloride into an n-butyl alcohol solution of the compound b, controlling the temperature to react after dropwise adding is ended, and concentrating to remove the solvent and unreacted thionyl chloride after the reaction is ended, so as to obtain a compound c; carrying out Dieckmann condensation reaction on the compound c at controlled temperature under the condition of organic alkali by using toluene as a solvent, carrying out hydrochloric acid quenching reaction after the reaction is finished, and directly carrying out next-step reaction after extracting and removing impurities from a water phase containing a hydrochloride solution of a compound d by using toluene; and carrying out a decarboxylation reaction on the compound d in a hydrochloric acid aqueous solution at controlled temperature, after the reaction is finished, adjusting the pH value to 10-13, extracting, and salifying to obtain a target compound TM, namely 3-quinuclidinone hydrochloride. The preparation method of 3-quinuclidinone hydrochloride provided by the invention has the advantages of economical and easily available raw materials, mild reaction conditions, efficient reaction, simple operation and low cost, and is suitable for industrial application.

This invention provides a method for preparing and applying a highly insecticidal diamide compound, relating to the chemical and pesticide fields. The method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; and, during the reaction under a hydrogen atmosphere, determining the reaction temperature and hydrogen flow rate in each hydrogenation reaction zone based on the concentration of compound B; reacting compound C with paraformaldehyde to obtain compound D; chlorinating 3-chloro-4-fluorobenzoic acid with thionyl chloride (a chlorinating agent) and dimethylformamide (a catalyst) to obtain compound E; and amide condensing compound E with compound D to obtain the novel diamide compound of this invention. The diamide compound of this invention exhibits excellent insecticidal effects when used in pesticide compositions.

The invention provides a preparation method of fluoride ether bacteria amide, which comprises the following steps: dissolving pentafluorobenzonitrile in a solvent, dropwise adding a sodium methoxide solution at-10-30 DEG C for 2-15 hours, continuing to carry out heat preservation reaction for 0.5-2 hours after dropwise adding, and carrying out post-treatment to obtain 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile; the preparation method comprises the following steps: jointly dissolving 2, 3, 5, 6-tetrafluoro-4-methoxybenzonitrile, 3-chloro-5-(trifluoromethyl) pyridine-2-yl) methanol and a catalyst acid in a solvent, reacting at 50-110 DEG C for 5-32 hours, and performing post-treatment on the obtained reaction liquid to obtain fluoride ether bacteria amide, according to the method, sodium methoxide and pentafluorobenzonitrile which are low in price and easy to obtain are subjected to etherification reaction, thionyl chloride and bis (trichloromethyl) carbonate are not used, the green chemical principle is met, and the method has the advantages of being short in step, safe and easy to operate and the like, so that the method has high implementation value and practical production applicability.

The invention relates to a preparation method of a 4-(dipropyl sulfamoyl)-N, N-dipropyl benzamide impurity reference substance, which is characterized by comprising the following specific steps: 1, carrying out acylating chlorination reaction on probenecid and thionyl chloride under the catalysis of DMF (N, N-dimethylformamide), and distilling and concentrating to obtain an intermediate probenecid acyl chloride; 2, carrying out amidation reaction on probenecid acyl chloride and dipropylamine to obtain a product reaction solution; and 3, purification: adjusting the pH value of the reaction liquid to be alkaline by using a sodium hydroxide solution, adding purified water for extraction, taking an upper organic phase, adding hydrochloric acid, precipitating a solid, filtering, washing a filter cake by using purified water, and drying at low temperature. The sample is a white solid, the HPLC purity is greater than or equal to 98%, the content is greater than or equal to 99%, no solvent residue exists, and the technical requirement of serving as an impurity reference substance is completely met.

The present invention provides a thiadiazole compound containing a hindered phenol group, a preparation method thereof and its use in the field of lubricating oil additives. The preparation method of the thiadiazole compound containing a hindered phenol group comprises the following steps: mixing a carboxylic acid compound containing a hindered phenol group with thionyl chloride, removing impurities under reduced pressure to obtain an acyl chloride compound containing hindered phenol; stirring and mixing 2-mercapto-5-amino-1,3,4-thiadiazole with a halogenated hydrocarbon compound, filtering, washing and drying to obtain a 2-mercapto-5-amino-1,3,4-thiadiazole derivative; adding a hindered phenol acyl chloride compound, 2-mercapto-5-amino-1,3,4-thiadiazole derivative and an alkaline additive to an organic solvent, washing, drying and purifying to obtain a thiadiazole compound containing a hindered phenol group. The thiadiazole compound containing a hindered phenol group is an antioxidant, extreme pressure and anti-wear additive, which can be applied to synthetic ester lubricants and has a good antioxidant, extreme pressure and anti-wear effect.

This invention discloses a magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd, its preparation method, and its applications. Using an amino alcohol as a starting material, an imidazole derivative containing a hydroxyl group on the N-substituent is obtained through a condensation and ring-closing reaction. This derivative is then subjected to substitution reactions with thionyl chloride and cyclohexanethiol sequentially to obtain an imidazole derivative containing a thioether on the N-substituent. This derivative is then reacted with 1,3-dibromopropane to obtain an N-bromopropyl-N'-cyclohexane thioether-substituted imidazole bromium salt. This salt is then reacted with Pd(OAc)₂ or PdCl₂ via a direct metallization reaction to obtain the N-bromopropyl-substituted thioether-chelated nitrogen heterocyclic carbene palladium complex NHC-Pd. The NHC-Pd complex is then reacted with amino-functionalized magnetic nanoparticles (MNPs-NH₂) to prepare the magnetically supported thioether-chelated nitrogen heterocyclic carbene palladium complex MNPs-NHC-Pd. It not only possesses the activity of homogeneous nitrogen heterocyclic carbene palladium catalysts, but also has a simple synthesis method, high yield, and is easy to separate and reuse in catalytic C-C bonding reactions, showing good application prospects in the field of catalysis.

The invention discloses a solvent removal process and a crude product post-treatment method in isophthaloyl chloride / paraphthaloyl chloride production, and belongs to the technical field of chemical processes. A three-stage gradient condensation system is adopted, circulating water, chilled water and chilled saline water are respectively introduced, the recovery rate of thionyl chloride is improved, thionyl chloride is prevented from entering a subsequent vacuum unit, the equipment failure rate is reduced, and the annual overhaul frequency is reduced. A top condenser is arranged, hot water at the temperature of 50-55 DEG C (suitable for producing isophthaloyl dichloride) or hot water at the temperature of 85-90 DEG C (suitable for producing paraphthaloyl dichloride) is adopted as a cooling medium, so that isophthaloyl dichloride / paraphthaloyl dichloride is efficiently captured, and coagulum is thoroughly prevented from entering a subsequent system and blocking equipment and pipelines.

The invention belongs to the field of organic chemical synthesis, and particularly relates to a synthesis method of triaryl sulfonium salt, which comprises the following steps: (1) dissolving a catalyst: dissolving the catalyst in an organic solvent in a preparation kettle in advance to form a uniform solution; and (2) continuous feeding and reaction: enabling reactants thionyl chloride and an aromatic hydrocarbon derivative and the catalyst-containing solution obtained in the step (1) to pass through a continuous reactor at a controllable flow rate, firstly carrying out Friedel-Crafts acylation reaction in an all-solvent system, then heating to carry out addition reaction, and finally obtaining the triaryl sulfonium salt. According to the invention, the problem of solid-liquid non-uniformity is eliminated, and the reaction efficiency and reproducibility are improved; the reaction is fast and uniform, and local overheating and out-of-control risks are avoided.

This invention belongs to the field of insecticide technology, specifically relating to a diamide compound, its preparation method, intermediate preparation equipment, and applications. The preparation method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride in the presence of dimethylformamide to generate compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; substituting compound C with formaldehyde to obtain compound D; and condensing compound D with 3,5-dichloro-4-fluorobenzoyl chloride to obtain the diamide compound. The beneficial effects of this invention are: the diamide compound solves the problem of insecticide resistance and possesses high insecticidal activity, exhibiting good insecticidal effect at low doses. Furthermore, the preparation method uses mild reaction conditions, produces few byproducts, and has a high reaction yield, reducing raw material loss and thus lowering production costs.

The invention provides a synthesis method of L-acetoxypropionyl chloride, and belongs to the field of medical intermediates and fine chemical engineering. The preparation method comprises the following steps: mixing L-lactic acid and acetyl chloride for first reaction; then adding trichlorotoluene and a catalyst to carry out a second reaction; and then rectifying and separating to obtain the product L-acetoxypropionyl chloride. According to the method, two raw materials react to generate two products, no sulfur dioxide or acidic mixed waste gas is generated, the utilization rate of the raw materials reaches 100% theoretically, and the method completely conforms to an environment-friendly and pollution-free green process. The safety of the used trichlorotoluene is far higher than that of thionyl chloride and phosgene, the reaction is mild, the reaction speed can be controlled by controlling the temperature and the input amount of the catalyst, the production operation is relatively safe, and the purity of the prepared L-acetoxypropionyl chloride product is greater than 99%, and the yield is greater than 90%.

The utility model discloses a thionyl chloride synthesis circulating pump, which relates to the technical field of circulating pumps, and comprises a circulating pump, the bottom end of the circulating pump is provided with a quick dismounting mechanism, the surface of the circulating pump is provided with a clamping mechanism, the clamping mechanism comprises a connecting pipe, the connecting pipe is fixedly arranged on the surface of the circulating pump, and the connecting pipe is fixedly connected with the circulating pump. And a groove is formed in the connecting pipe. The clamping ring is aligned with the connecting pipe, the clamping block is aligned with the first clamping groove, at the moment, the connecting base makes contact with the connecting pipe, the clamping block is clamped into the clamping plate and pushes the push plate, the push plate extrudes the second spring, the second spring is shrunk, and the connecting base is rotated till the clamping block on the surface of the connecting base rotates into the second clamping groove; a second spring pushes a push plate to fix a clamping block in a second clamping groove, a waterproof gasket is arranged on the surface of a clamping ring, the clamping ring covers the connecting pipe, so that water flow cannot flow out in the using process, and the adaptability of the device is improved.

The invention discloses a system and method for comprehensive energy utilization of a thionyl chloride catalyst. The system comprises a thionyl chloride catalyst, a heat exchanger, a lithium bromide unit for cooling pure water, and a chilled water system. The outlet end of the thionyl chloride catalyst is connected to the heat exchanger via a pipeline, and gas with a certain amount of heat at the outlet of the thionyl chloride catalyst is directed into the heat exchanger. Pure water is provided in the heat exchanger for continuously passing through the heat exchanger to absorb heat in the gas. The output end of the heat exchanger is connected to the lithium bromide unit via a pipeline, and the output end of the lithium bromide unit is connected to the chilled water system. The invention overcomes the shortcomings of the prior art, recycles energy, reduces production costs, and significantly improves production efficiency. At the same time, the entire production process is optimized for reaction efficiency and material utilization, thereby increasing the economic benefits of the enterprise and having high social use value and application prospects.

The invention discloses a preparation method of a continuously-produced lithium thionyl chloride composite carbon electrode, and relates to the technical field of battery production, and the preparation method comprises the following steps: pre-pressing acetylene black, uniformly mixing the pre-pressed acetylene black with adhesive micro-powder to form powder, and carrying out three working procedures of mixing, rolling to form a film and rolling to fit the film on the powder at the temperature of 80-200 DEG C in sequence to finish fibration, so as to obtain the lithium thionyl chloride composite carbon electrode. The lithium thionyl chloride composite carbon electrode is obtained. The preparation process is free of a baking procedure, energy is saved, emission is reduced by 50% or above, and the production period is shortened to 1 day from 3 days of wet-process film rolling or 2 days of semi-dry powder net loading; and a first-grade flammable and explosive organic solvent with poor production safety is not needed, so that the safety risk and the production cost are reduced. The growth suitability of the bonding strength of each section of fibration is controlled through process design, the purpose of film combination after film formation is achieved, a thick electrode required by higher capacity can be prepared, and the adverse effects of net separation, floating powder and the like are avoided.

The invention relates to the technical field of synthesis of ester compounds, in particular to a preparation method of an ester compound based on a sulfur trioxide compound. The method comprises the following steps: by taking a sulfur trioxide compound as a carboxylic acid activating agent and taking a carboxylic acid-containing compound and a hydroxyl-containing compound as raw materials, carrying out esterification reaction at room temperature in a reaction system of an alkali substance, a sodium salt stabilizer and a solvent, activating carboxylic acid by sulfur trioxide to form an active intermediate, and reacting the active intermediate with hydroxyl to generate an ester compound. The ester compound based on the sulfur trioxide compound is obtained, and sodium sulfate precipitate is obtained at the same time. According to the method, acyl chloride, thionyl chloride or unstable condensation reagents with high corrosivity are not used in the reaction, chlorine-containing wastewater is not generated, the reaction is carried out at room temperature, heating or high temperature is not used, the reaction condition is mild, the product is easy to separate, the use of organic solvents can be effectively reduced through post-treatment, and the product yield is relatively high.

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.

The invention relates to a preparation method of an iopamidol chiral side chain. Specifically, the invention provides a preparation method of (S)-2-acetoxypropionyl chloride, which comprises the following steps: (1) mixing L-lactic acid and ethanol, adding toluene, vinyl acetate, onion pseudomonas lipase and a 3A molecular sieve, reacting, filtering, and concentrating the filtrate under reduced pressure to obtain (S)-2-acetoxypropionic acid; and (2) adding the (S)-2-acetoxypropionic acid prepared in the step (1) into a mixed solution of thionyl chloride and pyridine, stirring for reaction, heating for reflux reaction, and concentrating the obtained reaction solution under reduced pressure to obtain the (S)-2-acetoxypropionyl chloride. The (S)-2-acetoxypropionyl chloride prepared by the method disclosed by the invention has the advantages of excellent purity and yield, mild reaction conditions and simple operation, is beneficial to industrial production, and is further beneficial to preparation of high-purity and high-yield iopamidol as an intermediate, so that the application value of iopamidol is improved.

A method includes providing, within an etch chamber, a base structure including a target layer disposed on a substrate, and an etch mask disposed on the target layer, dry etching, within the etch chamber, the target layer using thionyl chloride to obtain a processed base structure, and after forming the plurality of features. The processed base structure includes a plurality of features and a plurality of openings defined by the etch mask. The method further includes removing the processed base structure from the etch chamber. In some embodiments, the target layer includes carbon. In some embodiments, the dry etching is performed at a sub-zero degree temperature.