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472 results about "Thionyl chloride" patented technology

Thionyl chloride is an inorganic compound with the chemical formula SOCl₂. It is a moderately volatile colourless liquid with an unpleasant acrid odour. Thionyl chloride is primarily used as a chlorinating reagent, with approximately 45,000 tonnes (50,000 short tons) per year being produced during the early 1990s. It is toxic, reacts with water, and is also listed under the Chemical Weapons Convention as it may be used for the production of chemical weapons.

Super-hydrophobic anti-icing coating for power transmission line and preparation method of super-hydrophobic anti-icing coating

The invention discloses a super-hydrophobic anti-icing coating for a power transmission line and a preparation method, and belongs to the technical field of preparation of anti-icing coatings. The super-hydrophobic anti-icing coating for the power transmission line is composed of a coating wrapping the surface of the power transmission line, and the coating is composed of the following components in parts by weight: 34-45 parts of composite resin, 8-14 parts of a composite ice melting agent, 10-18 parts of deionized water, 1-3 parts of hexadecyl trimethoxy silane and 50-58 parts of tetrahydrofuran, the composite resin is prepared from carboxyl multi-walled carbon nanotubes, isopropanol, tetraethoxysilane, a silane coupling agent KH-550, perfluorodecyl trimethoxysilane, butyl acrylate, methyl methacrylate and dodecafluoroheptyl methacrylate, and the composite ice melting agent is prepared from pyridine-2, 6-dicarboxylic acid, thionyl chloride and nicotinic acid hydrazide. The coating prepared by the method has excellent hydrophobicity, wear resistance and anti-icing effect.
Owner:HETONG SHULIAN (BEIJING) TECHNOLOGY ENGINEERING CO LTD

Nano imbibition displacement agent suitable for shale oil reservoir and preparation method of nano imbibition displacement agent

The invention provides a nano imbibition displacement agent suitable for shale oil reservoirs and a preparation method thereof, and the nano imbibition displacement agent comprises the following raw materials in parts by weight: 30-50 parts of sulfonated graphene oxide, 10-15 parts of silane coupling agent modified nano silicon dioxide, 10-20 parts of water-soluble cellulose ether, 10-20 parts of fatty alcohol-polyoxyethylene ether, 5-8 parts of lower alcohol and 50-80 parts of water. Graphene oxide reacts with concentrated nitric acid to prepare acidified graphene oxide, then the acidified graphene oxide reacts with thionyl chloride to prepare acylating-chlorinated graphene oxide, and the acylating-chlorinated graphene oxide reacts with a sodium aminobenzene sulfonate derivative to prepare the graphene oxide. Electrostatic repulsive force is generated among graphene oxide particles through surface sulfonation treatment, the dispersing capacity among the particles is improved, agglomeration and flocculation among the particles are avoided, and the recovery efficiency is improved; sulfonated graphene oxide cooperates with a large-molecular-weight water-soluble cellulose ether surfactant, so that the temperature resistance and the salt resistance of the nano imbibition displacement agent can be remarkably improved.
Owner:DAQING YONGZHU PETROLEUM TECH DEV CO LTD +1

Lubricant additive and preparation method thereof, lubricant, water-based drilling fluid and preparation method thereof

The invention relates to the technical field of petroleum drilling fluids, in particular to a lubricant additive and a preparation method thereof, a lubricant, a water-based drilling fluid and a preparation method thereof, the lubricant additive comprises the following raw materials: 6 parts of taurine, 30-60 parts of 1-bromohexadecane, 8.5-15 parts of potassium hydroxide, 0.5-0.9 part of potassium iodide, 30-60 parts of thionyl chloride, 2-4 parts of N, N-dimethylformamide, 7-17 parts of ammonia water and 30 parts of trichloromethane. The lubricant additive takes sulfonic acid amine as an active adsorption group, and can be stably adsorbed on a drill stem, a sleeve and a mud cake. Meanwhile, two C16 flexible chains are arranged, a compact lubricating film can be formed, and friction resistance is efficiently reduced.
Owner:SOUTHWEST PETROLEUM UNIV

High-breathability fabric and preparation method thereof

The invention discloses a high-breathability fabric and a preparation method thereof, and relates to the field of fabrics. When the high-breathability fabric is prepared, cotton cellulose sequentially reacts with allyl succinic anhydride and 4 '-amino-2, 2': 6 ', 2'-terpyridyl to obtain modified cellulose; the preparation method comprises the following steps: sequentially reacting graphene oxide with thionyl chloride, 2, 4-diamino-6-vinyl-S-triazine and 2, 6-di-tert-butyl-4-bromomethylphenol, so as to obtain modified graphene oxide; uniformly mixing the modified cellulose, the modified graphene oxide, hydrogen-containing silicone oil, polyethylene glycol and silver nitrate, and spinning and weaving to obtain the high-breathability fabric. The high-breathability fabric prepared by the invention has excellent moisture absorption and breathability, lasting antibacterial property, mechanical property and photo-oxidative aging resistance.
Owner:NANTONG JIAYUSI TEXTILE GROUP

Flame-retardant anti-aging electric wire and cable and preparation method thereof

The invention relates to the technical field of wire and cable preparation, and discloses a flame-retardant anti-aging wire and cable and a preparation method thereof. The preparation method of the flame-retardant anti-aging wire and cable comprises the following steps: reacting a ketal compound with thionyl chloride, and then reacting with ricinoleic acid ester to obtain an intermediate product; reacting the thiazolopyridyl compound with the intermediate product to obtain a bio-based plasticizer; modifying the bio-based plasticizer to obtain a modified bio-based plasticizer; mixing polyvinyl chloride resin, linear low-density polyethylene, an ethylene-octylene copolymer, a flame-retardant anti-aging agent, a modified bio-based plasticizer and other components to obtain a sheath layer mixed master batch, and extruding to obtain a sheath layer; and after coating the conductor with the sheath layer, cooling, rolling and packaging to obtain the flame-retardant anti-aging wire and cable. The flame-retardant anti-aging wire and cable sheath layer has good flame retardance, aging resistance and mechanical property, and plays a good role in protecting wires and cables.
Owner:WUHAN FUXUN TECH CO LTD

Monoatom modified carbon composite wave-absorbing material and preparation method thereof

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.
Owner:NANJING UNIV OF SCI & TECH

Polyurethane material for leaking stoppage of coal mine and preparation method of polyurethane 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.
Owner:INNER MONGOLIA JINGRUN MINING SAFETY TECH CO LTD

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

Method for producing 4, 4 '-dichlorodiphenyl sulfone through continuous reaction of microchannel reactor

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.
Owner:新疆兴发化工有限公司 +1

Epoxy resin composite material based on flexible chain segments and rigid fiber particles and preparation method

ActiveCN119775723ACelluloseFirming agent
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.
Owner:SICHUAN UNIV

Antistatic fabric and preparation method thereof

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.
Owner:RUGAO TAIYATE KNITTED FASHION CO LTD

Preparation method of high-elasticity optical cable

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.
Owner:吕清倩

Preparation method of high-purity acyl chloride product

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of a high-purity acyl chloride product, which comprises the following steps: S1, mixing organic acid, thionyl chloride and an amide catalyst, and reacting by adopting multi-stage heating under a stirring condition to obtain crude acyl chloride; the multi-stage heating process is as follows: the first-stage reaction temperature is 20-25 DEG C, and the reaction time is 30-40 minutes; the second-stage reaction temperature is 35 to 45 DEG C, and the reaction temperature is 30 to 40 minutes; the temperature of the third-stage reaction is 50-100 DEG C, and the reaction time is 40-70 minutes; and S2, distilling and purifying the crude acyl chloride to obtain the acyl chloride product. According to the preparation method, the acyl chloride can be continuously prepared, so that the production efficiency of the acyl chloride is improved, the production time is shortened, the product purity is high, the yield is high, and the unreacted organic acid and the catalyst can be reused as raw materials for the next reaction, so that the production cost is saved.
Owner:YANTAI TAYHO ADVANCED MATERIALS RES INST CO LTD +1

Rigid polyamine composite nanofiltration membrane and preparation method thereof

The invention belongs to the field of separation, and particularly relates to a rigid polyamine composite nanofiltration membrane and a preparation method thereof. The preparation method comprises the following steps: coating one side of a base membrane with polyamine with a rigid structure, contacting thionyl chloride with the other side of the base membrane, diffusing thionyl chloride to pass through membrane pore channels of the base membrane in a volatilization manner, and contacting with melamine for reaction to prepare the composite nanofiltration membrane. According to the technical scheme, firstly, based on the low price of thionyl chloride, the cost of preparing the composite nanofiltration membrane is low; secondly, by means of the steam reverse mass transfer reaction, the prepared composite nanofiltration membrane has the double-charge characteristic, and most substances with the charge characteristic can be intercepted. In addition, due to the fact that the molecular chain of thionyl chloride is short, the reaction activity with polyamine is weak, the overall aperture of the prepared polyamide composite nanofiltration membrane is larger, and the flux of the prepared nanofiltration membrane is higher.
Owner:TIANJIN MOTIMO MEMBRANE TECH CO LTD

Synthesis method and synthesis device of benzenesulfonyl fluoride

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.
Owner:ZIBO FEIYUAN CHEM CO LTD

Production method of imidodisulfuryl fluoride and production method of lithium imidodisulfuryl fluoride

The invention relates to a production method of imidodisulfuryl fluoride and a production method of lithium imidodisulfuryl fluoride, the production method of imidodisulfuryl fluoride takes sulfamic acid, chlorosulfonic acid and thionyl chloride as raw materials, imidodisulfuryl fluoride is obtained through chlorination reaction, imidodisulfuryl fluoride and hydrofluoric acid or imidodisulfuryl fluoride and hydrogen fluoride gas are taken as raw materials, imidodisulfuryl fluoride and hydrogen fluoride gas are subjected to chlorination reaction to obtain imidodisulfuryl fluoride. The invention discloses a method for producing bis (fluorosulfonyl) imide, which comprises the following steps: by taking bis (fluorosulfonyl) imide as a raw material, carrying out fluoridation reaction to prepare a bis (fluorosulfonyl) imide crude product, adding metal salt into the bis (fluorosulfonyl) imide crude product, and then carrying out melt crystallization and / or rectification. According to the method, the metal salt is added into the difluorosulfonyl imide crude product, so that the metal salt can react with a light component in a fluorination reaction system or a component with a boiling point similar to that of the target product difluorosulfonyl imide, and the impurities react to generate salt with a relatively high boiling point; therefore, the components can be separated from the target product imidodisulfuryl fluoride in the subsequent purification process, and the purity of imidodisulfuryl fluoride is further improved.
Owner:SHANGHAI DONGGENG CHEM TECH CO LTD

Preparation method of polyphenylene sulfide

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.
Owner:DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES

Special antistatic polyethylene pipe material and preparation method thereof

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.
Owner:SICHUAN YIBIN PUSH BUILDING MATERIALS CO LTD

Electrolyte for alkali metal-thionyl chloride secondary battery and application thereof

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.
Owner:QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI

Compound rectification system

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.
Owner:INNER MONGOLIA ZHONGHE NEW MATERIALS CO LTD

Synthesis method of sulpiride impurity 2-hydroxy-5-sulfanilamide benzamide

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.
Owner:SHAANXI PUCHENG WANDE SCI & TECH

Indeno-aza compound as well as preparation method and medical application thereof

The invention relates to the field of organic chemistry and medicinal chemistry, in particular to an indeno-aza compound I as well as a preparation method and medical application thereof. The method comprises the following steps: adding an amine compound into an indeno-oxa-heptacyclic compound serving as a raw material under solvent-free and additive-free conditions, directly adding stoichiometric thionyl chloride and a solvent acetonitrile into an intermediate product obtained after the reaction without separation and pretreatment to continue the reaction, adding alkali again without separation and pretreatment after the reaction is completed, and separating and purifying to obtain the product. And controlling the reaction temperature to finally prepare the indeno-aza compound. The invention reports a compound with a novel structure, and develops a one-pot continuous operation synthesis method of the compound. The synthesis operation of the method conforms to the concept of green chemistry, and the obvious advantages of chemical synthesis means are embodied. Meanwhile, the compound has a certain inhibition effect on human esophageal cancer cells and human bladder cancer cells.
Owner:GUIZHOU MINZU UNIV +1

Preparation method of 3-quinuclidinone hydrochloride

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.
Owner:CHONGQING ENSKY CHEM

Preparation method, product and application of rosin-based polyamine

The invention discloses a preparation method of rosin-based polyamine, a product and application thereof, and belongs to the technical field of bio-based adhesives, the preparation method comprises the following steps: using toluene as a solvent, using thionyl chloride to carry out acylating chlorination on disproportionated rosin, after the reaction is finished, carrying out rotary evaporation to remove toluene, then reacting with methanol, and carrying out methyl esterification on the disproportionated rosin to obtain methyl esterified rosin; reacting the obtained methyl esterified rosin with acid to obtain nitrated rosin methyl ester; carrying out reduction reaction on the obtained nitrated rosin methyl ester and iron powder to obtain rosin-based polyamine; wherein the acid comprises one or more of nitric acid and sulfuric acid. The prepared rosin-based polyamine is synthesized into rosin-based isocyanate through a phosgenation method, and the rosin-based isocyanate is glued to prepare a shaving board, a fiberboard and a plywood with the thickness of 18 mm; the test method refers to GB / T17657-2013, and each performance of the artificial board meets the requirements of the national standard (P2 type in GB / T 4897-2015) (MDF-FN type in GB / T 18259-2018) (class II board in GB / T 18259-2009).
Owner:INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY

Preparation method and application of a double-amide compound with high insecticidal activity

PendingCN122355853ABenzoic acidAniline
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.
Owner:SHANDONG HUASHENG NEW MATERIAL CO LTD

Preparation method of novel bactericide fluoride ether bacteria amide

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.
Owner:ZHEJIANG UNIV OF TECH

Preparation of 4-(dipropyl sulfamoyl)-N, N-dipropyl benzamide impurity reference substance

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.
Owner:ANHUI KANGZHENG KANGYUAN PHARM CO LTD

A thiadiazole compound containing a hindered phenol group, its preparation method and its use in the field of lubricating oil additives

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.
Owner:DALIAN UNIV OF TECH PANJIN INST OF IND TECH +1

A magnetically supported thioether chelated nitrogen heterocyclic carbene palladium complex, its preparation method and application

ActiveCN118179602BPalladium catalystDibromopropane
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.
Owner:HENAN UNIVERSITY OF TECHNOLOGY

Solvent removal process and crude product post-treatment method in isophthaloyl chloride / paraphthaloyl chloride production

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.
Owner:DEZHOU SHIHUA CHEM