295 results about "Dichloroethane" patented technology

The invention provides an antistatic agent for fuel oil and a preparation method thereof, and belongs to the technical field of petrochemical engineering, and the preparation method comprises the following steps: S1, adding soybean lecithin and chlorosulfonic acid into dichloroethane, uniformly mixing, under the protection of nitrogen, heating and stirring for reaction, neutralizing reaction liquid, and performing rotary evaporation to obtain sulfonated soybean lecithin; the preparation method comprises the following steps: adding sulfonated soybean lecithin and ethidene diamine into absolute ethyl alcohol, then adding p-toluenesulfonic acid, heating and stirring for reaction, and carrying out reduced pressure distillation to obtain modified soybean lecithin; s2, dispersing the SiO2 particles in absolute ethyl alcohol, adding KH-550, and performing ultrasonic treatment, centrifugation and drying to obtain pretreated SiO2 particles; and uniformly mixing the modified soybean lecithin and the pretreated SiO2 particles, adding the mixture into a supercritical fluid reactor, heating and pressurizing, ultrasonically dispersing, and drying to obtain the antistatic agent. The antistatic agent has the advantages of good dispersibility, strong stability and strong antistatic capability.

The invention relates to a preparation method of a lithium difluoro bis (oxalate) phosphate concentrated solution, and belongs to the technical field of lithium battery electrolyte additives. Adding lithium oxalate into a solvent, stirring and dissolving to obtain a lithium oxalate solution; the method comprises the following steps: adding a modified fluorine ion chelating agent into a lithium oxalate solution, stirring, filtering, putting into a reactor, and slowly introducing phosphorus pentafluoride gas; after the introduction is finished, heating and stirring for reaction; after the reaction is finished, filtering reaction liquid to remove unreacted solid impurities, so as to obtain a lithium difluoro bis (oxalate) phosphate concentrated solution; the modified fluorine ion chelating agent is prepared from D301 ion exchange resin, dichloroethane, propylene-1-base boronic acid pinacol ester, mercaptoethyl guanidine dihydro bromide and sodium tert-butoxide. The lithium difluoro bis (oxalate) phosphate prepared by the method is high in purity and high in yield, and meets the use requirements of lithium ion battery electrolyte on lithium salt.

The invention discloses a preparation method of deuterated methylamine hydrochloride and a solid-phase continuous flow synthesis system, and relates to the technical field of deuterated synthesis. The preparation method comprises the following steps: adding out-of-phase polykadexide into methyl trifluoromethanesulfonate and 1, 2-dichloroethane for heating reaction, then adding methanol for quenching reaction, washing and drying to obtain an out-of-phase polykadexide type methyl reagent; the method comprises the following steps: adding a heterophase polysulfide-type methyl reagent into a mixed solvent of a polar solvent and heavy water, and carrying out alkali treatment to complete deuteration conversion, so as to obtain a heterophase polysulfide-type deuterated methyl reagent; the preparation method comprises the following steps: dissolving o-phenylsuccinimide in acetonitrile, and adding a heterophase polysulfide deuterium methyl reagent and inorganic alkali to react, so as to obtain N-(1, 1, 1-trideuterium methyl) benzo-succinimide; the preparation method comprises the following steps: hydrolyzing N-(1, 1, 1-trideuterium methyl) benzo-succinimide and hydrochloric acid in an aqueous solvent to obtain deuterated methylamine hydrochloride. The preparation method is simple, the deuterium source is cheap, the atom utilization rate is high, the deuteration rate is high, and the production cost is low.

The present invention relates to the technical field of polymer synthesis, and provides a carbon dioxide-based polycarbonate diol refining method, which comprises: S1, mixing carbon dioxide-based polycarbonate diol, an extraction agent and water, and washing to obtain a glue liquid; s2, the glue liquid is subjected to flash evaporation and devolatilization, and a carbon dioxide-based polycarbonate diol refined product is obtained; the extracting agent comprises methylbenzene or a mixture of one of methylbenzene, chlorobenzene and ethyl acetate and dichloroethane. According to the technical scheme, the problem of low yield of polycarbonate diol prepared in related technologies is solved.

The utility model belongs to the technical field of waste liquid recycling equipment, and particularly relates to a dichlorofluoroethane waste liquid recycling device which comprises a waste liquid cylinder, the interior of the waste liquid cylinder is of a cavity structure, waste liquid is layered after being poured into the waste liquid cylinder for standing, and the waste liquid in the cylinder is divided into three layers, namely an upper floating oil layer, a middle standing layer and a lower particle layer; an observation window and an air filter are respectively arranged at the top of the waste liquid cylinder; a waste liquid outlet communicated with the waste liquid cylinder is formed in one side of the bottom of the waste liquid cylinder; a collector communicated with the waste liquid cylinder is arranged outside the waste liquid cylinder; and a recycling part is also arranged in the cylinder body of the waste liquid cylinder. According to the recycling device, the recycling component is arranged in the waste liquid cylinder, the purposes of recycling and reusing the dichlorofluoroethane waste liquid and reusing the dichlorofluoroethane waste liquid by using a middle standing layer are achieved by adopting a physical method and through natural standing, layering, semi-automatic liquid taking and filtering of the waste liquid, the purposes of no power consumption, safety and environment-friendly recycling are achieved, the using cost is low, and the recycling device is suitable for industrial production. And benefits are brought to enterprises.

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazole compound under a visible light catalysis condition. The method comprises the following steps: dissolving a compound 1 in 1, 2-dichloroethane, then adding tert-butyl nitrite, tribromomethane, alkali and a photocatalyst, in an inert gas environment, irradiating with visible light and stirring at room temperature to react, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column purification on a crude product to obtain a product, namely the isoxazole compound. The brand-new method for preparing the isoxazole compound through visible light catalysis is developed, the conditions of high temperature and high pressure in a traditional synthesis method are avoided, energy consumption and environmental pollution are remarkably reduced, and the yield of the isoxazole compound is effectively increased by regulating and controlling reaction conditions and optimizing raw material selection and proportion.

The invention discloses a Pd-Ba / C catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps: step 1, pretreating a carbon carrier; step 2, preparing a complexing solution containing a barium complex; step 3, carrying out wet impregnation to obtain a carbon carrier adsorbed with a barium complex; 4, performing low-temperature pyrolysis to obtain a barium pre-modified carrier; 5, a complexing solution containing palladium and barium complexes is prepared; step 6, co-adsorption of bimetals is realized through wet impregnation, and a bimetal adsorption carrier is obtained; step 7, freeze drying; 8, the precursor obtained after freeze drying is subjected to hydrogen reduction, and the Pd-Ba / C catalyst is obtained. The invention provides application of the Pd-Ba / C catalyst in preparation of ethylene by hydrodechlorination of 1, 2-dichloroethane. According to the invention, pre-loaded barium occupies a strong adsorption site on the surface of the activated carbon, so that the stability and dispersity of a palladium active center can be enhanced, and synergistic improvement of chlorine poisoning resistance and catalytic performance of the catalyst is realized.

The invention discloses a preparation method of a hydroxyl-functionalized quaternary phosphonium salt polyion liquid super-crosslinked heterogeneous catalyst and an application of the catalyst in catalysis of a cycloaddition reaction of CO2 and epoxide. Trimethoxytriphenylphosphine and dibromo-p-xylene are firstly subjected to quaternary phosphating to form triphenylphosphine-based ionic liquid, and then the triphenylphosphine-based ionic liquid and biphenyl benzyl dichloride can be subjected to aromatic electrophilic substitution reaction in the presence of 1, 2-dichloroethane serving as a solvent and anhydrous aluminum chloride serving as a Lewis acid catalyst to realize cross-linking, so that the triphenylphosphine-based ionic liquid can be prepared. And methoxy can be removed to form hydroxyl, so that the hydroxyl-functionalized quaternary phosphonium salt polyion liquid super-crosslinked polymer is prepared in one step. The resulting heterogeneous catalyst effectively converts CO2 to cyclic carbonates under milder conditions (80 DEG C, 1 atm) in the absence of a soluble co-catalyst.

The invention belongs to the technical field of synthesis of organic compounds, and particularly relates to a process for preparing fipronil and an intermediate thereof. Toxic 1, 2-dichloroethane is comprehensively replaced by bio-based gamma-valerolactone, low-toxicity cyclopentyl methyl ether is matched, and N, N-dimethylformamide necessary for the process is recycled, so that consumption is greatly reduced; the continuous processes of amination, diazotization and the like are realized through a tubular reactor, a micro-reactor and a static mixer, and separation technologies such as pervaporation membrane and vacuum distillation are combined, so that the reaction time is shortened, the solvent recovery rate is increased, and the production is promoted to be continuously transformed to green. The supported FeCl3 / SiO2-NH2 catalyst disclosed by the invention can be repeatedly used, and byproducts and tail gas can be recycled and reused. In addition, diazonium salt residues are controlled to be smaller than or equal to 0.5% through near infrared spectroscopy, citric acid is subjected to stable oxidation reaction, a purification process is combined, it is ensured that the finished product is high in purity, excellent in yield and small in batch fluctuation, and efficiency and safety are both considered.

The invention relates to the field of chemical equipment, in particular to a 1-nitroanthraquinone continuous production process based on a dynamic liquid membrane continuous flow reactor, which comprises a solid feeding device, a homogeneous emulsifier, a quenching kettle, a solid-liquid separator, a centrifugal separator and a dynamic liquid membrane reactor, a sulfuric acid storage tank is divided into two branches through a sulfuric acid feeding pump, one branch is connected to the dynamic liquid membrane reactor, the other branch is connected to the dynamic liquid membrane reactor through a flow self-control valve, the quenching kettle is connected to a solid-liquid separator, the solid-liquid separator is divided into two branches, one branch is connected to an anthraquinone crude product storage tank, the other branch is connected to a centrifugal separator, and the other branch is connected to a gas-liquid separator. The centrifugal separator is divided into two branches, one branch is connected to the acid water storage tank, and the other branch is connected to the dichloroethane storage tank, so that the reaction selectivity of the anthraquinone nitration reaction can be effectively improved, high-viscosity solids are prevented from being blocked, and the conversion rate of raw materials in the continuous reaction of the anthraquinone nitration reaction is improved.

The invention discloses a method for continuously preparing flake diquat dichloride by a microfluidic reactor, which includes: using a feeding pump to input liquid 2,2'-bipyridine or a 2,2'-bipyridine solution dissolved in a solvent, dichloroethane or a dichloroethane solution into the microfluidic reactor, quickly mixing and precipitating, separating solid from liquid, washing with toluene, and drying to obtain flake diquat dichloride; a dispersant is added to the liquid 2,2'-bipyridine or the 2,2'-bipyridine solution dissolved in a solvent, dichloroethane or the dichloroethane solution, either both or one of them. The method of the invention has the advantages of simple operation, stable process, strong safety, and continuous and stable production. The synthesized diquat dichloride is in a flake structure, which can effectively avoid dust and is helpful for the production and packaging of various pesticide formulations. The method of the invention uses a surfactant, which effectively avoids the agglomeration phenomenon of diquat dichloride.

The subject of the invention is N-substituted derivatives of l-(l-phenyl-3-aryl)-lH-pyrazol-4-yl)methanamine with the general formula 1, where ¥ represents CH or N, R1 represents hydrogen, R2 represents no substituent, R3 represents hydrogen, while R4 represents N-propylbenzamide, benzo[b]furan, dihydrobenzo [b] furan, methylenedioxybenzene, ethyl benzoate, or propyl benzoate, substituted accordingly, their method of production and application, and the method of obtaining and application of N-substituted derivatives of l-(l-phenyl-3-aryl)-IH-pyrazol-4-yl)methanamine with the general formula 1, where Y represents C, CH, or N, R1 represents hydrogen or a methyl group, R2 represents a methyl group or no substituent, R3 represents hydrogen or a methyl group, while R4 represents dimethylpyrazole, methylpyrazole, dimethylimidazo[l,2-a]pyrimidine, or isopropoxybenzene, substituted accordingly. The compounds that are the subject of the invention are obtained through reductive amination using borohydride derivatives as the reducing agent, advantageously sodium triacetoxyborohydride, in the amount of 1.4-2.0 eq, amine in the amount of 1.0-1.1 eq, advantageously in slight excess, base, advantageously triethylamine in the amount of 1.0-1.1 eq (in the case of using amine in the form of hydrochloride), and the starting aldehyde. The reaction is conducted in a nonpolar solvent environment, advantageously dichloroethane at a concentration of about 0.1 M. The crude product is purified by column chromatography on silica gel using a methanol in dichloromethane mixture as the eluent, in concentration ranges from 2% to 5%. In order to obtain a solid form and improve the physicochemical parameters, the free bases are converted into hydrochloride form, and then crystallized from a polar solvent, advantageously ethanol or propanol.

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.

The utility model discloses a distillation and purification device for pesticide precursor production, which relates to the technical field of distillation and purification and comprises a distillation kettle, a circular cover body is arranged at the top end of the distillation kettle, a heating component sleeved on the outer side of the distillation kettle is fixedly connected to the bottom end of the circular cover body, and a mixing component is arranged in the middle of the top end of the circular cover body in a penetrating manner. A vacuum pump penetrates through one side of the top end of the circular cover body, a condensation assembly penetrates through the other side of the top end of the circular cover body, a mother liquor recovery tank is arranged at the bottom end of the condensation assembly, a water injection port penetrates through one side of the mother liquor recovery tank, a backflow assembly penetrates through the bottom end of the mother liquor recovery tank, and a material transferring pipe is arranged at one end of the backflow assembly. One end of the material transfer pipe penetrates through the heating assembly and is connected with the distillation kettle. The dichloroethane distillation kettle is reasonable and reliable in structure, the heat exchange area is greatly increased through the double-layer jacket design, the uniform distribution of the temperature in the distillation kettle is ensured, and the distillation effect of dichloroethane and low-boiling-point organic matters is improved.

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazoline compound. The preparation method comprises the following steps: dissolving a compound 1 and ethyl acrylate in dichloroethane, then adding tert-butyl nitrite, alkali and K2S2O8, in an air environment, irradiating with a 35 W blue LED light source and stirring at room temperature for 12 hours, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column chromatography on a crude product to obtain a product, namely the isoxazoline compound. The synthesis method provided by the invention avoids the problem of residue of a traditional metal catalyst, and provides a new normal form for green synthesis of the isoxazoline compound. As a key intermediate, isoxazoline can derive beta-lactam, beta-amino alcohol and other structures, and a new path is provided for complex molecule synthesis.

The application discloses a preparation method of 1-(2-aminoethyl) pyrrolidine and belongs to the field of chemical synthesis. The application provides a novel synthesis method of 1-(2-aminoethyl) pyrrolidine, which is prepared from 1,2-dichloroethane and pyrrolidine as raw materials, addition of a solvent and alkali, heating reaction, extraction, acidification and reduced-pressure distillation after the reaction is finished to obtain N-(2-chloroethyl) pyrrolidine solution; N-(2-chloroethyl) pyrrolidine and ammonia water are used as raw materials, high-pressure heating reaction is carried out, extraction and reduced-pressure distillation are carried out after the reaction is finished to generate 1-(2-aminoethyl) pyrrolidine. The application has the advantages of simple operation process, green process synthesis, convenient product purification and high product purity.

The invention discloses a method for preparing vinyl chloride by electrocatalytic dechlorination of 1, 2-dichloroethane, a working electrode of the method takes a metal oxide as a catalyst, and the metal oxide is selected from at least one of the following metal oxides: Pd, Mn, Fe, Co, Ni, Cu, Ru and Mo. According to the invention, the metal oxide powder is used as the electrocatalyst, the catalyst is coated on the electrode material to prepare the working electrode, the working electrode is applied to electrocatalytic dechlorination reaction of 1, 2-dichloroethane, vinyl chloride can be generated at high selectivity at room temperature, a new way is opened up for production of vinyl chloride by electrocatalytic dechlorination, and the method has wide application prospect. And a green and low-cost solution is provided for efficient synthesis of vinyl chloride.

The invention discloses amido-modified hypercrosslinked resin, a preparation method thereof and application of the amido-modified hypercrosslinked resin to adsorption of chlorine-containing VOCs (Volatile Organic Compounds). The preparation method comprises the following steps: chloromethylation: swelling hypercrosslinked NDA-88 resin in 1, 2-dichloroethane, adding anhydrous FeCl3 as a catalyst, and carrying out chloromethylation reaction at 35-40 DEG C to obtain chloromethylated resin; and amination: mixing the chloromethylated resin with an amination reagent diethylenetriamine, carrying out amination reaction at 140-150 DEG C, and carrying out post-treatment to obtain the amino modified hypercrosslinked resin. The amino-modified hypercrosslinked resin has high adsorption capacity and long penetration time for chlorine-containing VOCs (Volatile Organic Compounds) such as dichloromethane, chlorobenzene and the like, is stable in performance under the relative humidity of 50%, and is small in adsorption performance attenuation after multiple times of thermal regeneration. The resin is simple in preparation method, excellent in performance and suitable for efficient purification treatment of industrial chlorine-containing VOCs waste gas.

The invention relates to a method for producing vinyl chloride by catalytic thermal cracking of 1, 2-dichloroethane, the heat required for the thermal cracking being supplied via a liquid or condensing heat transfer medium (4), the heat transfer medium (4) being heated at least partially by thermal energy obtained when hydrogen (10), ammonia (11) or a hydrogen-ammonia mixture is oxidized according to the invention. The invention also relates to a device for producing vinyl chloride by catalytic thermal cracking of 1, 2-dichloroethane, comprising at least one reactor (1) carrying out thermal cracking and at least one first heating device (6), by means of which a reaction medium (13) in the reactor (1) is heated by a heat transfer medium (4), wherein the at least one first heating device (6) is designed to oxidize hydrogen gas (10) and / or ammonia (11), for example to burn hydrogen gas (10) and / or ammonia (11), in order to generate thermal energy, by means of which the heat transfer medium (4) can be heated.

The invention discloses a method for preparing p-trifluoromethoxyphenol by adopting a micro-channel reactor, and belongs to the field of fine chemical engineering. 4-trifluoromethoxyaniline and dilute sulphuric acid are pumped into the first micro-channel reactor for a reaction; then introducing inert gas, pumping the nitroso sulfuric acid solution, and carrying out diazotization reaction to obtain a diazonium salt solution; pumping the diazonium salt solution into a second micro-channel reactor, carrying out hydrolysis reaction, adding dichloroethane extract liquor into a rectifying tower after the reaction is ended, and rectifying to obtain p-trifluoromethoxyphenol; porous baffles which are inclined downwards are arranged on the inner wall of the rectifying tower in a crossed manner; a heat-conducting filler layer of 50-100 nm is arranged on the porous baffle plate; the heat-conducting filler layer is a three-dimensional net-shaped material layer which is formed by boron nitride nanosheets / titanium oxide nanorods and has a porous structure. The method is simple in process route, convenient to operate, high in controllability, high in safety, high in reaction efficiency, high in product yield, capable of effectively reducing the solid waste amount in production, energy-saving, environment-friendly and suitable for industrial production.

The invention provides flame-retardant polyurethane foam plastic and a preparation method thereof, and belongs to the technical field of macromolecules, and the preparation method comprises the following steps: S1, preparing modified lignin: modifying lignin by using a copper-chromium-loaded HZSM-5 zeolite catalyst; s2, preparing modified polyether polyol: mixing the modified lignin with polyol, and adding a catalyst for reaction to prepare lignin-based polyether polyol; and S3, preparing the flame-retardant polyurethane foaming plastic: uniformly stirring lignin-based polyether polyol, a flame retardant, a charring agent, triethanolamine, dibutyltin dilaurate, dichlorofluoroethane, nano tungsten carbide and water at room temperature, then adding isocyanate, continuously stirring, pouring into a mold for molding after uniform fusion, and curing to obtain the flame-retardant polyurethane foaming plastic. According to the technical scheme provided by the invention, the aims of improving the physical properties of the polyurethane foam plastic while achieving a good flame-retardant effect are achieved.

The invention discloses a method for synthesizing 2-aminopyridine, comprising using polystyrene resin beads as a carrier, a mixed solvent consisting of 1,2-dichloroethane and anhydrous ethanol as a porogen, adding the polystyrene resin beads and the mixed solvent to a flask for swelling; adding N,N-dimethylaniline to the flask, and performing a stirring reflux reaction; repeatedly washing the mixed solution in the flask with anhydrous ethanol and filtering it with suction, and finally vacuum drying it at room temperature. The method for synthesizing 2-aminopyridine utilizes polymer resin beads as a carrier, grafts a preferred highly active phase transfer catalyst molecule - N,N-dimethylaniline, and synthesizes a solid-supported phase transfer catalyst to achieve efficient recycling and regeneration of the phase transfer catalyst, and ensures the yield of the pyridine amination product by the solid-supported phase transfer catalyst, which is conducive to ensuring the efficient resource utilization of basic nitrogen heterocyclic compounds in coal tar.

This invention discloses a highly selective method for preparing triethylenetetramine. The method uses 2-chloroethylamine hydrochloride and ethylenediamine as raw materials, reacting them in an aqueous solution. An aqueous solution of ethylenediamine with a concentration of 1-100 wt% is added dropwise to an aqueous solution of 2-chloroethylamine hydrochloride with a concentration of 1-100 wt%. The dropping rate of the ethylenediamine solution is 5% to 100% of its own mass per hour. The reaction temperature is 30-200 °C (oil bath temperature), and the reaction time is 2-20 hours (including the dropping time). The molar ratio of 2-chloroethylamine hydrochloride to ethylenediamine is 2:1 to 40:1. This invention is the first to propose a direct synthesis of triethylenetetramine from the bulk chemicals 2-chloroethylamine hydrochloride and ethylenediamine. Compared with the previously reported dichloroethane amination method and the nucleophilic substitution method between dichloroethane and ethylenediamine, this method offers milder reaction conditions, simpler operation, and higher selectivity, making it suitable for industrial production.

The invention belongs to the technical field of polysulfide sealants, and relates to a bi-component modified polysulfide sealant for a binding surface as well as a preparation method and application of the bi-component modified polysulfide sealant. The bi-component modified polysulfide sealant for the binding surface is prepared from a component A and a component B according to the mass ratio of 100: (8-12), the component A comprises modified polysulfide rubber, a functional filler, a coupling agent, an adhesive and a regulator; the modified polysulfide rubber is prepared from polysulfide rubber and a modifier; the modifying agent is one of bis (2-chloroethyl) ether, 1, 2-dichloroethane and bis (chloromethyl) dimethylsilane; and the component B comprises a metal oxide, a plasticizer, an accelerant and a regulator. According to the modified polysulfide sealant formed by two components, the elongation at break of the polysulfide sealant is improved in an extreme environment, the sealant has excellent deformation resistance, cracking, shrinkage and bonding failure of a sealant layer are avoided, and the sealing performance of a binding surface is improved.

The utility model relates to the technical field of synthetic reaction devices of 2, 6-difluorobenzamide, in particular to a synthetic reaction device of 2, 6-difluorobenzamide, which comprises a stirring mechanism, the stirring mechanism comprises a supporting frame, a fixed bearing is fixedly arranged at the bottom end of the supporting frame, a stirring rod is fixedly arranged at the bottom end of the fixed bearing, a metal fixing sleeve is fixedly arranged on one side of the stirring rod, and a stirring paddle is fixedly arranged on one side of the metal fixing sleeve. And a supporting rotating platform is fixedly arranged at the bottom end of the stirring rod. Production materials are fed into the reaction kettle mechanism through the convenient feeding nozzle, then the stirring paddle is started by controlling the electric driving mechanism, and the stirring rod is controlled by the driving motor to rotate, so that the stirring paddle on one side of the stirring rod is driven to rotate and stir, the mixing of the coating is promoted, and the mixed 2, 4-dichloroethane is added into the reaction kettle mechanism. And 2, 6-difluorobenzamide is discharged through a discharge valve at the bottom of the reaction kettle mechanism and is conveyed to the next process.

The present application relates to the field of chemical synthesis, in particular to a synthesis method of N-oxobutane acetamide and derivatives thereof.The synthesis method comprises the following steps: reacting a phenone compound with a nitrile compound, an acid and a reaction solvent to obtain the N-oxobutane acetamide and derivatives thereof; the phenone compound is p-bromophenone, p-fluorophenone, p-chlorophenone, p-iodophenone, p-cyanophenone, 3,4-dimethylphenone or 2-naphthaldehyde; the nitrile compound is acetonitrile, 3-chloropropionitrile, dichloroacetonitrile or deuterated acetonitrile; the acid is CF3SO3H or BF3; and the reaction solvent is acetonitrile or dichloroethane.The present application directly constructs the N-oxobutane acetamide and derivatives thereof in one step with the nitrile compound as the only nitrogen source, and has the advantages of cheap and easily available raw materials, mild conditions, high yield and easy scale-up production.

The invention relates to a green synthesis method of triphenylphosphine, which belongs to the technical field of organic synthesis, and comprises the following steps: Step 1: adding a solvent, benzene and a catalyst aluminum trichloride into a reaction flask, heating to 25-30 DEG C, dropwise adding phosphorus oxychloride, after addition, carrying out heat preservation reaction, and after the reaction is finished, cooling to room temperature to obtain a reaction product; the heat preservation temperature is 25-30 DEG C, and the heat preservation time is 3-4 hours; 2, after the reaction is finished, water is added for washing and layering, an organic phase is concentrated, the solvent is recycled, and triphenylphosphine oxide is obtained; 3, reducing the triphenylphosphine oxide in a solvent through a reducing agent to obtain triphenylphosphine, wherein the reducing agent is a triethyl silane / oxine copper reduction system; and Step 4, after the reaction is finished, cooling to room temperature, adding water for washing and layering, concentrating an organic phase, and recovering the solvent to obtain the triphenylphosphine. The synthesis method is safer and more environment-friendly, the greenization of the process is embodied, the safety and environmental protection pressure is greatly relieved, the technological process is simple, the yield is high, and the synthesis method is suitable for industrial large-scale production.

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane, which comprises the following steps: by taking aromatic aldehyde, [1.1. 1] propeller alkane and 4-alkyl substituted Hanss ester synthesized by aldehyde as initial raw materials and dichloroethane and the like as a solvent, carrying out a reaction under the protection of inert gas to obtain 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane, and separating the 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane from the 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane. A three-component free radical coupling reaction is carried out under the illumination condition, and a 1-benzyl alcohol-3-alkyl bicyclo [1.1. 1] pentane product is synthesized in one step. The method has the advantages of mild reaction conditions, high reaction efficiency, low cost, simplicity and convenience in operation and the like, and a new method is provided for later structural modification of diaryl methanol drug molecules.

The present invention discloses a preparation method of mesotrione, and the method steps are as follows: S1: Under the protection of an inert gas, 3-chloro-2-methylbenzenemethanethiol, phosphorus oxychloride, a composite catalyst and an organic solvent are mixed and reacted. After the reaction is completed, 2-chloro-3-methyl-4-methylthiophenylaldehyde is obtained through separation and vacuum distillation; 2-chloro-3-methyl-4-methylthiophenylaldehyde is mixed with sodium tungstate dihydrate and methanol, and hydrogen peroxide is added for reaction. After the reaction, 2-chloro-3-methyl-4-methylsulfonylbenzoic acid is obtained through filtration; S2: Preparation of 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid; S3: 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid is mixed and reacted with thionyl chloride and dichloroethane, and the reaction product is further reacted with 1,3-cyclohexanedione, triethylamine and samarium trichloride to prepare mesotrione. The present invention simplifies the preparation route of mesotrione, the preparation process is more green and safe, and the yield of mesotrione is higher.

The invention discloses a high-boiling-point styryl liquid cross-linking agent, a preparation method thereof and organic medium slurry of a high-frequency and high-speed copper-clad plate. The preparation method of the high-boiling-point styryl liquid cross-linking agent comprises the following steps: carrying out Friedel-Crafts reaction on toluene and dichloroethane to obtain 1, 2-bis (methyl benzene) ethane; the preparation method comprises the following steps: carrying out Friedel-Crafts reaction on dimethyl phenylethane and acetyl chloride to obtain 1, 2-bis (methyl acetyl benzene) ethane; the preparation method comprises the following steps: carrying out reduction reaction on 1, 2-bis (methyl acetyl benzene) ethane and sodium borohydride to obtain 1, 2-bis (methyl alpha hydroxyethyl benzene) ethane; and carrying out dehydration to obtain the 1, 2-bis (methyl vinyl benzene) ethane cross-linking agent. The 1, 2-bis (methyl vinyl benzene) ethane is in a liquid state at normal temperature, has high solubility for SEBS and other film-forming resins, can reduce the solvent amount for copper-clad plate manufacturing, is a high-boiling-point cross-linking agent, and has wide application prospects.