769 results about "Addition reaction" patented technology

The invention relates to the technical field of organic polymer adhesives, and particularly discloses a modified castor oil-based polyurethane adhesive as well as a preparation method and application thereof. The adhesive comprises two components, and the component A comprises the following components in parts by weight: 30.0-50.0 parts of modified castor oil and 0.0-30.0 parts of refined castor oil; the component B is prepared from the following components in parts by weight: 30.0 to 50.0 parts of polyisocyanate or a polyisocyanate modifier and 0.00 to 0.05 part of a dewatering agent; the modified castor oil is prepared from refined castor oil and cysteamine through a sulfydryl-alkene addition reaction. Amido of the modified castor oil is alkalescent, and the reaction speed of the modified castor oil and isocyanate groups is high; hydrogen bonds are easily generated between urea bonds generated by the reaction of amino groups and isocyanate groups, so that the adhesive is endowed with thixotropy and high strength. The adhesive disclosed by the invention is simple in composition, high in reaction speed and good in thixotropy and bonding strength.

The invention relates to the technical field of PC resin flexibilizers, and discloses a shell-core structure styrene-acrylic resin modified organic silicon elastomer flexibilizer as well as a preparation method and application thereof in order to solve the problems that an organic silicon material and PC resin are poor in intersolubility, a traditional flexibilizer is poor in low-temperature toughening performance and the like. Comprising the following steps: uniformly mixing hydrogen-containing silicone oil, vinyl silicone oil, a third alkenyl functional component and a catalyst, and pre-emulsifying under the action of a surfactant and a thickener to obtain an organic silicon pre-emulsion SiE; uniformly mixing an alkenyl phenyl compound, acrylate and / or a cross-linking agent, adding a molecular weight regulator and an oil-soluble initiator, and pre-emulsifying under the action of a surfactant and water to obtain a styrene-acrylic pre-emulsion SAE; the preparation method comprises the following steps: firstly, preparing an organic silicon pre-emulsion, then heating the organic silicon pre-emulsion to carry out a water-phase hydrosilylation addition reaction, then dropwise adding the styrene-acrylic pre-emulsion to carry out suspension emulsion copolymerization, and then demulsifying and drying to obtain the styrene-acrylic resin modified organic silicon elastomer toughening agent with the core-shell structure.

The invention discloses a method for synthesizing a dichloroacetyl compound, which comprises the following steps: tetrachloroethylene and an acid are subjected to an addition reaction at 100-200 DEG C to obtain an adduct, then the adduct is subjected to an acidolysis, hydrolysis or alcoholysis reaction to obtain the dichloroacetyl compound, the acid for the addition reaction is at least one of sulfuric acid, trifluoromethanesulfonic acid, methanesulfonic acid and phosphoric acid, and the acid for the alcoholysis reaction is at least one of sulfuric acid, trifluoromethanesulfonic acid, methanesulfonic acid and phosphoric acid. The molar ratio of the tetrachloroethylene to the acid is 1: (1-10). By controlling the types of acids and increasing the temperature of the addition reaction, the addition reaction of tetrachloroethylene and acids in the absence of a catalyst is realized. Double bonds of tetrachloroethylene and hydrogen protons are subjected to an addition reaction in a strong acid environment to form a cationic intermediate, then the cationic intermediate is combined with acid radical anions to form an adduct, and the adduct intermediate is high in activity, unstable and free of separation and can be directly subjected to a hydrolysis reaction, an acidolysis reaction or an alcoholysis reaction with another substrate (such as water, acid or alcohol) respectively. The synthesis of dichloroacetyl series compounds is realized, and the route has universality and diversity.

The invention discloses a high-strength and high-resilience TPE (thermoplastic elastomer) and a preparation method thereof in the technical field of high polymer materials, and the elastomer is prepared by taking a hydrogenated styrene block copolymer as a matrix and matching with a polyolefin rigid phase, plasticizing oil and a specific additive. The method is characterized in that two self-made reaction type modifiers are introduced, wherein one self-made reaction type modifier is a core-shell nano reinforcing agent containing an epoxy functional group and polyhedral oligomeric siloxane, and the other self-made reaction type modifier is a furan maleimide bifunctional dynamic cross-linking agent. The nano reinforcing agent is prepared through silane hydrolysis and amination reaction, and can react with a matrix for grafting, so that the strength and creep resistance of the material are remarkably improved; the dynamic cross-linking agent is synthesized through step-by-step isocyanate addition reaction, a cross-linked network can be reversibly formed in the processing process, and the material is endowed with extremely high rebound resilience and low permanent deformation. The obtained product has high strength, high resilience and excellent processability, and is especially suitable for high-end fitness equipment.

The invention discloses a preparation method and application of a catalyst based on pyridine ionic liquid, and belongs to the technical field of catalyst preparation. According to the invention, a hydrolysis reaction of a silane coupling agent is utilized to prepare a silicon oxide nanotube containing a pyridine unit, and then a quaternization reaction is carried out to obtain the catalyst based on the pyridine ionic liquid. The catalyst has a high specific surface area and a rich pore channel structure, exposure of active sites and contact of the active sites and reactants are facilitated, and the catalytic rate is increased. Meanwhile, the silicon oxide nanotube contains hydroxyl, and can cooperate with a pyridine ionic liquid site to catalyze a carbon dioxide cycloaddition reaction. The obtained catalyst can catalyze the reaction of carbon dioxide and an epoxy compound to prepare cyclic carbonate under solvent-free and metal-free conditions, and the catalyst is easy to recover and simple in product purification, and has a good application prospect.

The invention belongs to the field of adhesives, and relates to an acrylate-siloxane modified polyurethane adhesive as well as a preparation method and application thereof. The acrylate-siloxane modified polyurethane adhesive contains a silane modified polyurethane prepolymer, an acrylate compound, a photoinitiator and an optional rheology modifier, wherein the silane modified polyurethane prepolymer, the acrylate compound, the photoinitiator and the optional rheology modifier are used as raw materials; the silane modified polyurethane prepolymer is prepared by the following steps: firstly, carrying out addition polymerization reaction on a polyisocyanate compound and a low-viscosity polyol compound, and then carrying out addition reaction on the obtained polyurethane prepolymer and a silane coupling agent containing reactive hydrogen. The low-viscosity polyol compound has a glass transition temperature of 0 DEG C or less and a melting point of 40 DEG C or less; the functionality of at least a portion of the acrylate compound is bifunctional or less, and the glass transition temperature is 20 DEG C or more. The acrylate-siloxane modified polyurethane adhesive provided by the invention has the characteristics of low viscosity, no bubble and high curing speed.

The invention relates to the technical field of organic-inorganic hybrid materials, in particular to an antifouling organic-inorganic hybrid material, a preparation method, a photocuring antifouling material and a product. The organic-inorganic hybrid material is prepared by carrying out a ring-opening addition reaction on an epoxy group of epoxy polyhedral oligomeric silsesquioxane and polydimethylsiloxane with an amino group or perfluoropolyether with a carboxyl group. According to the scheme provided by the invention, the coating has high thermal stability and structural rigidity endowed by epoxy polyhedral oligomeric silsesquioxane and excellent low surface energy antifouling property endowed by amino-containing polydimethylsiloxane or carboxyl-containing perfluoropolyether, and the defect that a pure epoxy polyhedral oligomeric silsesquioxane coating does not have antifouling property is effectively overcome.

The invention belongs to the technical field of epoxy resin, and particularly relates to double-dynamic-bond synergistic exchange epoxy resin as well as a preparation method and application thereof. The preparation method of the double dynamic bond synergistic exchange epoxy resin comprises the following steps: adding aromatic dialdehyde and amino-containing disulfide into a solvent for condensation reaction, and filtering and drying to obtain a double dynamic bond curing agent; the preparation method comprises the following steps: adding the double-dynamic-bond curing agent into epoxy resin, carrying out ring-opening addition reaction, carrying out gradient heating curing, and cooling to room temperature, the aromatic dialdehyde is terephthalaldehyde, isophthalaldehyde or o-phthalaldehyde, and the amino-containing disulfide is 2, 2 '-diaminodiphenyl disulfide or 4, 4'-diaminodiphenyl disulfide. The invention designs and synthesizes a double-dynamic covalent bond curing agent containing an imine bond and a disulfide bond, and is used for constructing a novel degradable and self-healing epoxy resin. The material maintains good thermal stability and insulation performance, and realizes degradation and self-healing functions at the same time.

The present application belongs to the technical field of the synthesis of chiral boron compounds, and in particular relates to an MOF-Cu(II) / CMC composite material, and a preparation method therefor and the use thereof. The preparation method for an MOF-Cu(II) / CMC composite material of the present application comprises: dropwise adding an aqueous solution of sodium carboxymethyl cellulose to an aqueous solution of a bivalent copper salt, performing solid-liquid separation, mixing obtained composite microspheres with an organic solution of trimesic acid, heating the resulting mixture, and subjecting same to solid-liquid separation, so as to obtain an MOF-Cu(II) / CMC composite material. The MOF-Cu(II) / CMC composite material is used in an asymmetric chiral boron addition reaction. The reaction is performed at room temperature, involves mild conditions, is applicable to a wide range of substrates and has a high yield and enantioselectivity. Moreover, the method can achieve the synthesis of a chiral organic boride in a solvent having simple components, providing an efficient new method for the preparation of drug molecules and active intermediates, and also broadening the range of substrates used for the preparation of chiral organic borides.

The invention discloses a Janus membrane as well as a preparation method and application thereof and an emulsion treatment device, and relates to the technical field of membrane filtration, the Janus membrane comprises a polyvinylidene fluoride base membrane and a copolymerization crosslinking product grafted on the surface of one side of the polyvinylidene fluoride base membrane, the copolymerization crosslinking product comprises a product formed by tannic acid and gelatin through a Michael addition reaction. Wherein the copolymerization crosslinking product is grafted on the surface of one side of the polyvinylidene fluoride base membrane, the contact angle of the side is reduced, the contact angle of the surface of the other side of the polyvinylidene fluoride base membrane is still high, and the contact angles of the surfaces of the two sides form a difference value, so that the hydrophilicity of one side of the polyvinylidene fluoride base membrane is high, the hydrophobicity of the other side of the polyvinylidene fluoride base membrane is high, and the Janus membrane is formed. The Janus membrane is suitable for efficient separation of emulsion.

The invention relates to an epoxy resin adhesive composition and a preparation method thereof, and belongs to the technical field of high-performance polymer material modification and electronic packaging materials, and the epoxy resin adhesive composition comprises the following components by weight: 100 parts of basic epoxy resin; 5-30 parts of a hyperbranched liquid crystal modifier; adding the curing agent according to a stoichiometric ratio; 100 to 600 parts of a heat-conducting filler; 0.1-5 parts of an accelerant and an auxiliary agent; the hyperbranched liquid crystal modifier has a core-shell structure and is prepared from a hydrogen-containing hyperbranched polysiloxane core and an alkenyl-terminated liquid crystal epoxy monomer through a hydrosilylation reaction under the action of a catalyst, the hyperbranched polysiloxane core is introduced, the friction resistance among high-concentration fillers is reduced by utilizing the torispherical structure of the hyperbranched polysiloxane core, and the hyperbranched liquid crystal modifier has the advantages that the friction resistance is reduced; under the condition that 350 parts of heat-conducting filler is filled, the modifier is added, so that the high-filling system still has excellent flowability and leveling property while keeping high heat-conducting property, and is suitable for high-precision micro-encapsulation scenes; the heat conductivity of the scheme is obviously superior to that of a system which does not use the modifier or does not adopt a stepped heating process.

The invention relates to high-heat-resistance polypropylene and a preparation method thereof, and belongs to the technical field of high polymer materials. The preparation method comprises the following steps: carrying out Michael addition reaction on 2-sulfydryl-1, 3-propylene glycol and vinyl dibutyl borate to prepare dihydric alcohol containing thioether and phosphate, and carrying out polymerization reaction on 1, 12-dodecanediol, boric acid ester dihydric alcohol and dimethyldichlorosilane to obtain the flame retardant. A polymer containing a borate group, a thioether group, organic silicon and a dodecane glycol ester group is prepared, the polymer is used as a heat-resistant toughening additive of polypropylene, the borate group and the organic silicon can improve the heat resistance and flame retardance of the polypropylene, and the thioether group and the dodecane glycol ester group can provide flexibility; therefore, the polypropylene is ensured to have good mechanical strength, heat resistance and flame retardance at the same time.

This invention discloses a method for synthesizing dialkylphosphinates, belonging to the field of organic synthesis technology. The method uses hypophosphite and haloalkanes as starting materials. First, a hypophosphite is generated through a heated and pressurized reaction under the action of a phase transfer catalyst. The obtained hypophosphite does not require complex purification; it is directly reacted with an olefin under heated and pressurized conditions in the presence of a free radical initiator to obtain the target product, dialkylphosphinate. The method of this invention uses inexpensive and readily available raw materials, has a simple process route, includes only two core reactions, operates under mild conditions, is safe and convenient, produces few and easily treatable byproducts, has a high product yield, and is simple to purify. It is very suitable for large-scale industrial production, providing an economical and efficient synthetic route for the preparation of high-performance halogen-free flame retardants.

The invention discloses a fluorocarbon grafted siloxane supercritical carbon dioxide thickening agent and a preparation method thereof, and relates to the technical field of carbon dioxide thickening. The method comprises the following steps: firstly, carrying out hydrosilylation reaction on tetramethyl tetravinyl cyclotetrasiloxane, tetramethyl cyclotetrasiloxane and multi-arm unsaturated acrylate to prepare a siloxane intermediate, and then carrying out free radical polymerization on the siloxane intermediate and fluoroacrylate to prepare the thickening agent. According to the prepared supercritical carbon dioxide fracturing fluid thickening agent, the contained carbon dioxide-philic groups can interact with carbon dioxide, so that the dissolving property of the thickening agent in supercritical carbon dioxide is enhanced; the thickening agent contains rich multi-branched siloxane groups, a spatial network structure can be further formed, and the supercritical carbon dioxide is effectively thickened through the synergistic effect of all the components.

The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing cyclopentane compounds through [3 + 2] cycloaddition reaction of aryl cyclopropane and olefin under the synergistic catalysis of bromide ions / visible light. The method comprises the following steps: in a nitrogen atmosphere, sequentially adding aryl cyclopropane, a benzyl malononitrile derivative, pyridine tribromide and a photocatalyst into a reaction solvent to obtain a mixture, stirring the mixture at the temperature of 40 DEG C under the irradiation of a 12W blue light LED lamp until the reaction is complete, and performing concentration and column chromatography purification to obtain the cyclopentane compound. The method has the advantages of mild reaction conditions, simple operation, simple and easily available raw materials and low cost.

The application relates to the technical field of catalysts, and discloses a limited type iodine-based homogeneous immobilized catalyst as well as a preparation method and application thereof. The catalyst comprises a carrier and iodine ions, magnesium ions and quaternary ammonium ions loaded on the carrier, wherein the molar ratio of the magnesium ions, the quaternary ammonium ions, the iodine ions and the carrier is 0.01-1:4-15:1-30:1. The limited type iodine-based homogeneous immobilized catalyst disclosed by the application enhances the electrostatic interaction between iodine ions and quaternary ammonium ions through the molecular sieve limiting effect to construct a limited type structure. The catalyst has significantly enhanced CO2 adsorption and activation capacity, can activate an epoxide compound, and accelerates the ring opening of the epoxide compound. In a cycloaddition reaction catalyzed by the catalyst under the conditions of no solvent and no auxiliary agent, the conversion rate of propylene oxide can reach more than 73%, and the propylene carbonate selectivity can reach more than 85%.

The invention belongs to the technical field of catalytic synthesis, particularly relates to a method for preparing a nitrogen-containing fused ring compound through quantum dot catalyzed [4 + 2] cycloaddition, and aims to solve the problems of limited product structure and complex reaction system in the existing synthesis method. The synthesis method disclosed by the invention comprises the following steps: in an inert atmosphere, adding 1-phenylpyrrole and fumarate as reaction raw materials, quantum dots as a photocatalyst and an organic solvent into a reaction container, carrying out [4 + 2] cycloaddition reaction under visible light irradiation, and then filtering, concentrating, separating and purifying to obtain the nitrogen-containing fused ring compound. The reaction condition is mild, and the method can be realized by irradiating the quantum dot catalyst with a visible light source at normal temperature and pressure; a reaction system is simple, strong oxidants and additives are not needed, operation steps are convenient, and atom economy is achieved.

The invention discloses a preparation method of an arfamarana key intermediate, which comprises the following steps: carrying out nucleophilic addition reaction on a compound I and 1-[3-chloro-5-(trifluoromethyl) phenyl]-2, 2, 2-trifluoroethanone under the action of an organic solvent A and alkali to obtain a compound II; dissolving the compound II in an organic solvent B, adding concentrated sulfuric acid, carrying out intramolecular dehydration and cyanogen hydrolysis, and after the reaction is finished, cooling to room temperature for crystal growing to obtain a compound III; dissolving the compound III in an organic solvent C, carrying out intramolecular cyclization and ester hydrolysis reaction on the compound III and hydroxylamine hydrochloride under the action of a certain amount of sodium hydroxide aqueous solution, and after the reaction is finished, collecting a water phase and adjusting the pH value of the water phase, so as to obtain the key intermediate of arfampanaga. The reaction in each step has a high conversion rate, the purity of the prepared arfamarin intermediate is high, and powerful support and guarantee are provided for preparation of high-purity arfamarin.

The invention relates to the technical field of food processing safety and environmental pollution control, in particular to a natural compound preparation with a synergistic formaldehyde removal function and a preparation method and application thereof. The natural compound preparation is prepared from the following raw materials in percentage by mass: 5%-10% of carnosine, 0.5%-2% of epigallocatechin gallate, 0.05%-0.2% of edible essence, 10%-20% of a surfactant and the balance of a solvent, and the total percentage is 100%. The invention aims to reduce the exposure risk of specific groups such as chefs and guarantee the health level of the specific groups, the main component carnosine is dipeptide which can be used as a food additive and has good antioxidant activity, and amino in the structure of the carnosine can be subjected to Michael addition reaction with carbonyl of aldehydes. The epigallocatechin gallate is a common polyphenol substance, and phenolic hydroxyl groups in the epigallocatechin gallate can be reacted with aldehydes to capture and remove the aldehydes.

The invention discloses a synthesis method of piperonone, and relates to the technical field of flavors, fragrances and chemical engineering, and the synthesis method comprises the following steps: taking acrylate as a raw material, and carrying out Michael addition reaction with isobutene under the action of Lewis acid to obtain 5-methyl-5-hexenoic acid ethyl ester; the preparation method comprises the following steps: carrying out nucleophilic substitution reaction on ethyl 5-methyl-5-hexenoate and bromoisopropane under the action of a basic catalyst to obtain ethyl 5-methyl-2-isopropyl-5-hexenoate; carrying out self Friedel-Crafts acylation reaction on the 5-methyl-2-isopropyl-5-hexenoic acid ethyl ester under the action of Lewis acid, so as to obtain 5-methyl-2-isopropyl-5-chloro cyclohexanone; and carrying out elimination reaction on the 5-methyl-2-isopropyl-5-chlorocyclohexanone under the action of alkali to obtain the product piperonone. According to the synthetic route, conventional chemical reagents are used as raw materials, reaction conditions are mild, emission of three wastes is reduced to a great extent, and the synthetic route is more environmentally friendly and suitable for continuous industrial production.

The application discloses a low-viscosity nitrogen-modified flame-retardant and smoke-suppressing silicone oil and a preparation method thereof, relates to the technical field of modified silicone oil, and the flame-retardant and smoke-suppressing silicone oil is obtained by ring-opening addition reaction of double-end epoxy silicone oil and methyl urea. The nitrogen-containing group is introduced into the polysiloxane molecule in a reactive form by adopting the chemical modification of methyl urea on the end epoxy silicone oil, so that the flame-retardant and smoke-suppressing performance and the thermal stability of the silicone oil are improved without significantly sacrificing the material fluidity. The obtained low-viscosity nitrogen-modified flame-retardant and smoke-suppressing silicone oil still maintains a good flow state at normal temperature, and is convenient to use in the modification of high polymer materials, the blending of composite systems and subsequent processing applications.

The application discloses a cross-linked polyaryl piperidine anion exchange membrane and a preparation method and application thereof, and relates to the technical field of anion exchange membranes. The anion exchange membrane takes polyaryl piperidine as a skeleton, introduces crown ether structure and a cross-linked network, and solves the technical problem that the balance between the hydroxyl ion conductivity and the dimensional stability is difficult in the existing anion exchange membrane. The anion exchange membrane comprises a specific structure of a repeating unit, is prepared through Friedel-Crafts superacid catalytic polymerization, Menshutkin reaction functionalization and Michael addition reaction cross-linking, and has excellent hydroxyl ion conductivity, dimensional stability, chemical stability and mechanical strength. The preparation method is simple in operation, fast in polymerization rate, and high in conversion rate, does not need to strictly control the temperature and oxygen of a reaction environment, is suitable for the field of water electrolysis hydrogen production, especially suitable for an anion exchange membrane water electrolysis system, and has a wide industrial application prospect.

The invention belongs to the technical field of membrane separation, and discloses a composite membrane formed by compounding a loose nanofiltration layer on an ultrafiltration layer and a preparation method and application of the composite membrane. Polyphenol covalent bonds and non-covalent bonds (hydrogen bonds, pi-pi accumulation) are adsorbed on an ultrafiltration membrane matrix to form functional active sites, and then a low-activity aldehyde group substance and polyphenol are subjected to a Schiff base reaction to form a covalent anchoring network; then a flexible long-chain amido substance is introduced to slowly permeate into the network to carry out Michael addition reaction or Schiff base reaction, supplementary crosslinking is carried out with residual functional groups, and finally, the flexible long-chain amido substance reacts with a low-concentration aldehyde solution for a short time to carry out secondary surface crosslinking to form a stable and loose nanofiltration layer network structure. Through step-by-step and interface regulation and control design, the process is simple, the condition is mild, stable and repeated preparation can be realized, and an innovative high-performance technical solution is provided for the practical application of the membrane material for deep treatment and resource recycling of dye wastewater.

The invention discloses a surfactant with a branched structure as well as a preparation method and application of the surfactant. The preparation method comprises the following steps: carrying out Michael addition reaction on an amphiphilic branched polymer and polyfluorinated organic amine in an organic solvent in the presence of a catalyst to obtain the surfactant with the branched structure, the amphiphilic branched polymer has a hydrophilic chain segment and a hydrophobic chain segment, and the tail end of a branched molecular chain has double bonds. The amphiphilic branched polymer is obtained by copolymerization of polyethylene glycol di (methyl) acrylate and polypropylene glycol di (methyl) acrylate through active free radicals, or is prepared by Michael addition polymerization of a di (methyl) acrylate compound and a dimercapto compound or a diamine compound in an organic solvent in the presence of a catalyst. The surfactant can quickly reduce the surface tension and prolong the retention time of pesticide liquid, and is green, environment-friendly and degradable.

The application relates to the technical field of organic synthesis, and discloses a synthesis method of benzthiazuron, which comprises the following steps: step 1, addition reaction of alpha-methyl styrene and hydrogen chloride gas, and degassing to obtain a first reaction liquid; step 2, substitution reaction of the first reaction liquid and cyanate in the presence of a zinc chloride catalyst, and filtration to obtain a second reaction liquid containing isocyanate; and step 3, construction of an inorganic salt aqueous solution system with a density of 1.05-1.10 g / ml and a pH of 9-10, dropwise addition of the second reaction liquid into the system for condensation reaction with o-chlorobenzylamine, and post-treatment and refinement to obtain a target product. The non-phosgene route of chloro-isocyanate substitution is adopted, and the use of the toxic phosgene is completely avoided; the salting-out effect and interface control generated by the specific high-density salt solution effectively inhibit the isocyanate hydrolysis side reaction, and the reaction yield and product purity are obviously improved.

The application relates to the technical field of organic silicon synthesis, and particularly discloses a high-selectivity platinum catalyst and a vinyl double-seal head synthesis method. The high-selectivity platinum catalyst comprises a carrier and a platinum active component loaded on the carrier, the platinum active component is obtained by reducing and activating a platinum precursor and a ligand under a hydrogen atmosphere at 250-350 DEG C after coordination modification, and the molar ratio of the ligand to the platinum element in the platinum precursor is 2-3:1. In the application, the platinum active component is obtained by reducing and activating the platinum precursor and the ligand after coordination modification, and the ligand and the platinum element form a specific coordination structure of the platinum active center, guide the direct silicon-hydrogen addition reaction of acetylene and a hydrogen-containing double-seal head, thus the dimethyl chlorosilane intermediate is not needed, the process flow is simplified, and the effects of improving the reaction yield, environmental protection and process economy are achieved.

The invention relates to the field of organic synthesis, in particular to a synthesis method of gamma-aminophosphine oxide compounds and derivatives thereof. According to the synthesis method disclosed by the invention, alpha, beta-unsaturated amide, diaryl phosphine oxide or phosphite ester is taken as raw materials, and under the action of acid, the gamma-aminophosphine oxide compound can be rapidly and efficiently synthesized by a one-pot method. The preparation method comprises the following steps of: generating conjugated nitrile positive ions or imine salt intermediates with strong electrophilicity from alpha, beta-unsaturated amide under the activation of acid, converting diaryl phosphine oxide or phosphite ester into strong nucleophilic three-coordination phosphorus species under the action of alkali, and further performing phosphorus-doped Michael addition reaction on the conjugated intermediates to finally generate the gamma-aminophosphine oxide compounds. According to the method disclosed by the invention, diaryl phosphine oxide or phosphite which is cheap, easy to obtain and stable in structural property is used as a phosphorus source, the substrate applicability is wide, and the economic cost is relatively low; in addition, the method realizes synthesis of a target product without participation of a metal catalyst, and is rapid and efficient.

The application provides a preparation method of a hydrophobic photocatalyst H-g-C3N4 and belongs to the technical field of new materials and photocatalytic wastewater treatment. ‑1 The method comprises the following steps: base material preparation: under an inert or air atmosphere, melamine is heated at a rate of 3-8°C·min ‑1 to 520-580°C and kept for 2-5 h, and after cooling, g-C3N4 powder is obtained by grinding; surface hydrophobic modification: g-C3N4 is dispersed in an inert organic solvent containing 3-aminopropyl triethoxysilane and a fluorine-containing olefin monomer to obtain a dispersion liquid; in the presence of a free radical initiator, amine-olefin Michael addition reaction is carried out, and after filtration, washing and drying, the hydrophobic photocatalyst H-g-C3N4 covalently grafted with organosilane-fluorine-containing olefin is obtained. The method has the advantages of simple preparation, low cost of raw materials and mild conditions, and the obtained material has high hydrophobicity, high stain resistance and high activity, and has a wide application prospect in photocatalytic treatment of wastewater containing antibiotic refractory organic matter, and in particular, has high efficiency and interference resistance in degradation of SMX under visible light.

The invention discloses a preparation method of a thermal insulation coating based on high temperature tolerance, and relates to the technical field of coatings, the thermal insulation coating comprises an organic silicon resin matrix, a thermal insulation filler, an interface coupling system and a catalyst system; a molecular chain of the organic silicon resin matrix contains a silicon-hydrogen bond; the heat insulation filler comprises a mica functional filler; the interface coupling system is prepared from vinyl functional alkoxy silane; an alkoxy group of the vinyl functional alkoxy silane and a hydroxyl group on the surface of the heat insulation filler are subjected to a condensation reaction, and a vinyl group of the vinyl functional alkoxy silane and a silicon-hydrogen bond of the organic silicon resin matrix are subjected to an addition reaction. An inorganic and organic network interpenetrating interface layer is constructed on the surface of the heat insulation filler through an interface coupling system, chemical bonding connection of the filler and a matrix is achieved, stress is effectively transmitted, heat flow diffusion is hindered, and the coating keeps excellent adhesive force retention rate and heat conductivity coefficient stability after high-temperature heat treatment.

The invention relates to a preparation method of 3-ethoxy isoamyl propionate, and belongs to the technical field of organic solvent synthesis. The preparation method of the 3-ethoxy isoamyl propionate comprises the following steps: S1, adding ethanol, a polymerization inhibitor and a catalyst A into a reaction kettle, heating to 40-55 DEG C, then dropwise adding ethyl acrylate, preserving heat, and carrying out addition reaction for 1-3 hours to obtain a reaction mixture; s2, adding an acidic material for neutralization, and carrying out vacuum rectification to obtain ethyl 3-ethoxypropionate; s3, adding ethyl 3-ethoxypropionate and a catalyst B into a reaction kettle, heating to 100-120 DEG C, introducing isoamyl alcohol, controlling the reaction temperature to 100-115 DEG C, and carrying out transesterification for 2.5-4 hours to obtain a crude product; and S4, cooling to stop the reaction, separating to remove the catalyst B, and carrying out reduced pressure rectification on the obtained crude product to obtain the 3-ethoxypropionic acid isoamyl ester. The method has the effects of mild process, high conversion rate and high product yield.