27 results about "Allyl bromide" patented technology

The invention discloses a catalyst for preparing ultrahigh molecular weight polyoxyethylene as well as a preparation method and application thereof, and relates to the technical field of catalyst preparation. The preparation method of the catalyst comprises the following steps: S1, carrying out a reaction on 6-hexamethylenediamine and allyl acrylate to generate an intermediate 1, S2, carrying out a reaction on the intermediate 1 and diphenylphosphine to generate an intermediate 2, S3, carrying out a reaction on the intermediate 2 and allyl bromide to generate an intermediate 3, and S4, carrying out a reaction on the intermediate 3 and 9-boron bicyclo [3.3. 1] nonane. The prepared catalyst is high in catalytic activity, ultrahigh molecular weight polyoxyethylene can be prepared, and the molecular weight distribution of the prepared ultrahigh molecular weight polyoxyethylene is narrow.

The present invention discloses an N-aryl-N-alkyl-O-allylhydroxylamine compound and its synthesis method. The general structural formula is as follows: The synthesis method includes the following steps: Using cheap and easily available aldehydes or ketones as starting materials, reacting with hydroxylamine hydrochloride to form oximes, and then preparing N-alkylhydroxylamines under the action of a supported metal catalyst; N-alkylhydroxylamines react with (R4-substituted) allyl bromide, etc. in the presence of a weak base to prepare N-alkyl-N-allylhydroxylamines; N-alkyl-N-allylhydroxylamines react with aryl alkyne precursors under the action of an initiator fluoride at room temperature to prepare N-aryl-N-alkyl-O-allylhydroxylamine compounds. The method of the present invention can effectively avoid the use of toxic, harmful, and explosive strong oxidants, and at the same time solve the problems of limited raw material sources, high prices, harsh reaction conditions, and low reaction selectivity in the existing synthesis methods.

This invention discloses a low-functionality photocurable resin and its preparation method, comprising: dissolving polybenzimidazole in a polar aprotic solvent in an inert gas atmosphere to obtain a polybenzimidazole solution; adding sodium hydride in a molar amount equal to 0.8–1.2 times the molar amount of the polybenzimidazole resin to the polybenzimidazole solution, reacting the mixture, then adding allyl bromide in a molar amount equal to 0.8–1.2 times the molar amount of the polybenzimidazole resin, reacting again to obtain a polybenzimidazole prepolymer; dissolving the polybenzimidazole prepolymer in a polar aprotic solvent, adding a crosslinking agent and a photoinitiator, and mixing to obtain a photocurable resin solution; irradiating the photocurable resin solution with ultraviolet light, and drying to obtain a photocurable resin with a functionality of 20%–44%. This invention features a low allyl content, allowing for the curing of aromatic resins with less crosslinking agent, and the cured resin exhibits excellent heat resistance and ultra-high mechanical strength.

The invention provides a novel method for preparing an intermediate compound of aromatic sesquiterpenes Commiphoranes C-D. The method comprises the following steps: substituting the ortho-position of a compound 1 with iodine through n-butyllithium and diiodoethane to obtain a compound 2; removing methoxyl by using boron tribromide to obtain a compound 3; performing nucleophilic substitution on 3-allyl bromide and potassium carbonate to synthesize a compound 4; carrying out Grignard reaction to obtain a compound 5; oxidizing into a compound 6 through a Dess-Martin oxidizing agent; finally, (CH3Si) 3SiH and triethyl boron are subjected to intramolecular free radical series cyclization, so that synthesis of an aromatic sesquiterpene Commiphoranes C-D intermediate compound is successfully completed, sufficient preparation is made for follow-up total synthesis of the natural product, key intramolecular free radical series cyclization has the capacity of efficiently constructing a polycyclic system, and the synthesis process is simple and convenient. According to the preparation method, the defects of expensive reagents, long 14-step linear synthesis route, low yield and the like in the existing synthesis route are overcome; the popularization potential is high.

The present invention provides a quantum dot surface organic ligand composition and a preparation method thereof. The organic ligand composition is synthesized by azeotropic concentration of pentaethylene glycol monoallyl ether and 3-mercaptopropanol under the action of a stabilizer. There are three synthesis methods for pentaethylene glycol monoallyl ether, namely synthesis method 1, synthesis method 2 and synthesis method 3. Among them, synthesis method 1 uses methanesulfonyl chloride and allyloxyethanol as raw materials, reaction formula 2 uses pentaethylene glycol and allyl bromide as raw materials, and reaction formula 3 uses 4-toluenesulfonyl chloride and allyloxyethanol as raw materials. In the process of synthesizing the organic ligand composition of the present invention, a stabilizer is added, which improves the purity stability and viscosity stability of the organic ligand composition, and also greatly improves the binding force and oxidation stability with the quantum dot material. The azeotropic concentration method can remove fine moisture and completely control the gelation phenomenon caused by moisture, and has low viscosity reproducibility.

The application belongs to the technical field of materials, and provides a bio-based bismaleimide resin and a preparation method and application thereof, the resin being prepared by copolymerization of curcumin allyl ether and N,N'-4,4'-diphenylmethane bismaleimide. The curcumin allyl ether has a beta-diketone conjugated system, and is prepared by nucleophilic substitution reaction of curcumin and allyl bromide in a potassium carbonate acetone system; when prepared, the two are cured in stages at 150-240 DEG C to form a high crosslinking network, and a vacuum degassing and curing process is combined. The bio-based bismaleimide resin provided in the application has a curing peak temperature that is 20-30 DEG C lower than that of a traditional BD resin, a Tg that is nearly 90 DEG C higher than that of the BD resin, a carbon residue rate at 800 DEG C that is greater than or equal to 42%, an LOI that is greater than or equal to 37%, reaches a UL-94 V-0 level, a THR that is as low as 12.4 kJ / g, less flammable volatile matter at high temperatures, and a high degree of carbonization of residual carbon.

The invention belongs to the field of high polymer materials, and relates to a clean construction method of a halogen-free phosphorus-free flame-retardant epoxy polymerization system. The preparation method comprises the following steps: preparing an intermediate I from 2, 2 '-diallyl bisphenol and allyl bromide under the action of potassium carbonate; carrying out rearrangement reaction on the intermediate I to prepare an intermediate II; and carrying out etherification and ring-closure reaction on the intermediate II and epoxy chloropropane under the action of a catalyst and sodium hydroxide to obtain the epoxy resin monomer III. The halogen-free phosphorus-free flame-retardant epoxy resin polymer is obtained by mixing an epoxy resin monomer with a curing agent, melting, performing injection molding and curing. The halogen-free and phosphorus-free flame retardant polymer obtained by the invention can reach the flame retardant grade of UL94-V0 grade.

The invention relates to the technical field of fabrics, in particular to a light-weight down-proof knitted fabric for down jackets. The invention relates to a light down-proof knitted fabric for down jackets. The preparation method comprises the following steps: preparing a composite shell-core hybrid emulsion, preparing modified aramid nanofibers, and preparing the down-proof knitted fabric. The core-shell emulsion is prepared from allyl bromide modified silicon dioxide and is uniformly dispersed to prevent down penetration; modified aramid fibers are prepared from camphor, so that double heat insulation barriers are formed, and light weight is achieved. Hexagonal jacquard weave is adopted for weaving to enhance the stability, and an environment-friendly TPU hot film is coated to form a double-barrier, waterproof, anti-corrosion and protective coating, so that the downproof validity period is prolonged, and the strength and the heat preservation property of the fabric are improved.

The invention discloses a washing product based on a seaweed extract and a preparation method, and belongs to the technical field of daily cosmetics, the product takes two modified seaweed active ingredients as a core, and comprises a fucoic acid derivative modified by diallylation and quaternization, a sodium alginate copolymer modified by carboxymethylation and chitosan grafting, a sodium alginate copolymer modified by sodium alginate and chitosan grafting, and a sodium alginate copolymer modified by sodium alginate and chitosan grafting. A seaweed extract, a basic surfactant, an ampholytic surfactant, a humectant, a pH regulator and a preservative are used as auxiliary materials for compounding to form a washing product. Wherein the diallylation fucoic acid derivative is prepared through quaternization after reaction of fucoic acid and allyl bromide, and the chitosan grafted copolymer is prepared through cross-linking and grafting of sodium alginate and chitosan after carboxymethylation. Through the synergistic effect of the modified seaweed component and the natural extract, the cleaning, moisturizing and mild properties of the washing product are improved, and the natural and efficient requirements are met.

The application provides a branched halogenated butyl rubber preparation method, compared with the prior art, the branched butyl rubber synthesized by the application has a bimodal distribution of molecular weight, the molecular weight distribution is widened, and the mechanical properties such as tensile strength are obviously improved, so that the processing performance of the butyl rubber is effectively improved; the branched butyl rubber halogenation method provided by the application improves the neutralization efficiency, reduces the possibility of incomplete neutralization, effectively inhibits the conversion of the secondary allyl bromine substitution product into the primary allyl bromine substitution product, the obtained brominated butyl rubber has excellent indexes, and the structure is more stable; meanwhile, the preparation method provided by the application is simple in operation, easy in condition control and low in cost, and has a wide application prospect.

The present invention relates to the field of epoxy resin materials, and in particular to a preparation method of a multifunctional epoxy resin and its application in conductive adhesives. The preparation method includes: introducing multiple propenyl groups on the dipentaerythritol molecule by reacting dipentaerythritol with allyl bromide, and then introducing multiple epoxy groups by reacting the introduced propenyl groups with the alkenyl groups on the 1-allyloxy-2,3-propylene oxide molecule under the action of an initiator, thereby preparing a multifunctional epoxy resin; the multifunctional structure can increase the crosslinking density of the epoxy resin-based adhesive after curing, thereby increasing the heat-resistant temperature and strength of the adhesive; the multifunctional epoxy resin with a branched structure formed on the basis of the multi-branched structure of dipentaerythritol can further increase the crosslinking density of the epoxy resin, thereby increasing the strength and heat resistance; the introduction of nano-silica can effectively improve the mechanical properties of the epoxy resin and enhance toughness.

The invention belongs to the field of synthesis of drug intermediates, and discloses a process for industrially producing 2-allyl-3-methoxybenzaldehyde. The synthesis method comprises the following three steps: 1, alkylation reaction: reacting a raw material 3-hydroxybenzaldehyde with allyl bromide under an alkaline condition to obtain an allyl ether intermediate (3-allyl ether benzaldehyde); and 2, Claisen rearrangement reaction of the allyl ether intermediate: under a brand new flowing chemical reaction device (240 DEG C, 2MPa back pressure), dissolving the raw materials in a solvent, pumping the solvent into a microchannel, carrying out rearrangement reaction, and recrystallizing to remove an isomer, so as to obtain the intermediate 2-allyl-3-hydroxybenzaldehyde. And 3, methylation reaction: enabling the 2-allyl-3-hydroxybenzaldehyde to react with dimethyl sulfate under an alkaline condition, so as to obtain the product 2-allyl-3-methoxybenzaldehyde. The total yield of the three steps is 40%. According to the process, the raw materials are low in price and easy to obtain, the process operation is simple and convenient, and the process is suitable for industrial production of the 2-allyl-3-methoxybenzaldehyde.

The application discloses a kind of bio-based epoxy resin precursor, composite insulating material and its preparation method and application, belong to bio-based epoxy resin technical field, the bio-based epoxy resin precursor includes glycidyl ether structure and glycidyl ester structure, preparation method is as follows: (1) hydroxyl polyacid, allyl bromide occurs substitution reaction under the action of acid binding agent, and intermediate is prepared; (2) intermediate, hydrogen peroxide and acid catalyst are mixed and carried out oxidation reaction, and the bio-based epoxy resin precursor is prepared.The composite insulating material cured with the bio-based epoxy resin precursor has excellent thermodynamic performance and electrical performance, and also has the characteristics of rapid degradation under alkaline conditions and biodegradation in natural environment, suitable for the support, insulation and sealing of electrical equipment.

The present invention discloses a method for preparing an ortho-dibromide or an allyl dibromide. The method uses a conjugated diene as a raw material and, through substrate induction, a double bromination addition reaction to achieve the preparation of the ortho-dibromide or the allyl dibromide. Ortho-dibromides or allyl bromides are widely present in many natural products and drug molecules and are often used as intermediates in synthetic processes in many fields.

The invention relates to a preparation method of a carbon nanotube loaded Ru-Zn bimetallic catalyst for removing trace acetylene and ethylene impurities in electronic grade hydrogen chloride, and belongs to the technical field of catalysts. The method comprises the following steps: drying a carbon nanotube, dipping the carbon nanotube in a RuCl solution, stirring, carrying out ultrasonic treatment, and drying; dipping the Ru-loaded carbon nanotube in a zinc chloride solution, stirring, and drying to obtain a Ru / Zn intermediate; adding the Ru / Zn intermediate into a sodium hydroxide solution, adding tetraallylammonium bromide and 2, 5-dimercaptothiadiazole disodium salt, heating and stirring for reaction, and drying; placing the sample in an HCl atmosphere, and activating to obtain a nanoscale Ru-Zn bimetallic catalyst; the prepared catalyst has extremely high catalytic activity on trace acetylene and ethylene impurities in electronic-grade hydrogen chloride, can deeply remove the impurities, and meets the requirement of the electronic-grade hydrogen chloride on high purity.

The invention provides a preparation method of octabromo-ether, and belongs to the technical field of flame-retardant materials. According to the method, the tetrabromobisphenol A and the allyl bromide are subjected to the carbon-oxygen coupling reaction under the catalysis of the catalyst, no halogenated salt byproduct is generated, repeated purification is not needed, the loss of the octabromo-ether caused by aftertreatment is effectively reduced, and the yield of the octabromo-ether is increased; then hydrobromic acid and tetrabromobisphenol A diallyl ether are subjected to an addition reaction under catalytic oxidation of hydrogen peroxide to obtain octabromoether, and high-toxicity bromine does not need to be adopted; and hydrogen peroxide is adopted to generate oxygen and water in the reaction, thereby being green and environment-friendly. The result of the embodiment shows that the preparation method provided by the invention is green and environment-friendly, and the yield of the prepared octabromo-ether can reach 99.6%.

The invention provides a preparation method of octabromoS ether, and belongs to the technical field of flame-retardant materials. According to the preparation method, bisphenol S and allyl bromide are subjected to a carbon-oxygen coupling reaction under catalysis of a transition metal compound catalyst, bisphenol S diallyl ether and hydrogen bromide are obtained, hydrogen bromide can be recycled in a subsequent addition reaction, and the cost is saved; then hydrobromic acid and bisphenol S diallyl ether are subjected to an addition-electrophilic substitution reaction under catalytic oxidation of hydrogen peroxide to obtain octabromo-S ether, and high-toxicity bromine is not adopted; hydrogen peroxide is reduced into water in the reaction, so that the method is green and environment-friendly.

The invention discloses a preparation method of 3-[(3, 3-dimethoxy-2, 7-dioxa-3-silane-9-yl) oxy] propionitrile, which comprises the following steps: 1, adding 3-[(2-hydroxyethyl) oxy] propionitrile and a first organic solvent, cooling to 0-5 DEG C, adding sodium hydride in batches under the protection of nitrogen, heating to room temperature, stirring for 0.5-1 hour, controlling the temperature not to exceed 25 DEG C, dropwise adding bromopropene, reacting for 1-2 hours, cooling to 0-5 DEG C, cooling to 0-5 DEG C, cooling to 0-5 DEG C, cooling to 0-5 DEG C, cooling to 0-5 DEG C, adding sodium hydride in batches under the protection of nitrogen, heating to room temperature, stirring for 0.5-1 hour, and cooling to 0-5 DEG C to obtain a second organic solvent; after dropwise adding, filtering to remove insoluble substances, carrying out rotary evaporation to remove the solvent, and rectifying a crude product to obtain 3-{[2-(prop-2-alkenyl oxy) ethyl] oxy} propionitrile; and 2, adding 3-{[2-(propyl-2-alkenyl oxy) ethyl] oxy} propionitrile and a hydrosilylation catalyst, heating to 130-150 DEG C, dropwise adding trichlorosilane, carrying out a thermal reaction for 10-15 h after dropwise adding, dropwise adding a methanol solution dissolved with an acid-binding agent while controlling the temperature to be 10 DEG C or below, and carrying out molecular rectification treatment on a crude product after the reaction is completed to obtain a finished product. The method has the advantages that the synthesis method is simple and easy to implement, the post-treatment method is easy to operate, and the product purity is high.

The invention belongs to the technical field of materials, and provides bio-based bismaleimide resin as well as a preparation method and application thereof, and the resin is prepared by copolymerizing curcumin allyl ether and N, N '-4, 4'-diphenylmethane bismaleimide. The curcumin allyl ether has a beta-diketone conjugated system and is prepared by carrying out nucleophilic substitution reaction on curcumin and allyl bromide in a potassium carbonate acetone system; during preparation, the two components are subjected to segmented curing at 150-240 DEG C to form a high-crosslinking network, and vacuum degassing and curing processes are combined. According to the bio-based bismaleimide resin provided by the invention, in thermal performance and processability, the curing peak temperature is reduced by 20-30 DEG C compared with that of traditional BD resin, and Tg is greater than or equal to 390 DEG C and is increased by nearly 90 DEG C compared with that of the BD resin; in flame retardance and thermal stability, the carbon residue rate at 800 DEG C is greater than or equal to 42%, the LOI is greater than or equal to 37% and reaches the UL-94 V-0 level, the THR is as low as 12.4 kJ / g, the high-temperature flammable volatile matter is few, and the carbon residue graphitization degree is high.

The invention belongs to the technical field of fine chemicals, medicines and materials, and particularly relates to a preparation method of an aryl triepoxypropane compound. The preparation method comprises the following steps: 1) mixing 2, 6-diallylphenol with a first solvent, adding allyl bromide and alkali to obtain a mixture, heating and refluxing the mixture, reacting, and cooling to room temperature to obtain 1, 3-diallyl-2-allyloxybenzene as shown in a formula I; and 2) reacting the 1, 3-diallyl-2-allyloxybenzene as shown in the formula I, a metal complex catalyst and an oxidizing agent in a second solvent to obtain the aryl triepoxypropane compound as shown in a formula II. The preparation method has the advantages of cheap and easily available raw materials, simple and mild reaction, low catalyst price and high reaction yield, and can realize industrial production.

The application relates to the technical field of high polymer materials, and discloses a single-end type dihydroxyalkylamine modified polysiloxane as well as a preparation method and application thereof, and the structure is shown in formula I, wherein the value range of n is a natural number of 10-65. The preparation process is as follows: diethanolamine, hexamethyldisilazane, allyl bromide and alpha-(trimethylsilyl)-omega-dimethylsilyl polydimethylsiloxane shown in formula M1 are used as raw materials, and a single-end trimethylsilyl group and a dihydroxyalkylamine group are substituted at the other end under the catalysis of a Karstedt catalyst, the dihydroxyalkylamine modified polysiloxane has excellent stability and hydrophilicity, and the emulsion prepared by using the dihydroxyalkylamine modified polysiloxane has high hydrophilicity and good yellowing resistance when treating fabric.

The present invention discloses a solid organic acid catalyst, which comprises a strongly acidic cation exchange resin and a metal chloride; the strongly acidic cation exchange resin has a structure shown in Formula A below, where n = 60 - 180; the metal chloride is selected from one of aluminum chloride, iron chloride or chromium chloride. The strongly acidic cation exchange resin is prepared by reacting the product of the reaction of allyl bromide and N-(glycidyl)-N-phenyl-oxiranemethanamine with divinylbenzene, and then sulfonating with sodium aminosulfonate. The solid organic acid catalyst provided by the present invention has good stability, a long service life, strong catalytic ability and specific catalytic performance.

Waterborne epoxy modified naringin, carbon fiber sizing agent, sized carbon fiber and preparation method, which relate to the technical field of carbon fiber surface modification, and solve the problems of complex use method of existing water-soluble sizing agents and residual organic solvents. Preparation of waterborne epoxy modified naringin: Mix naringin, allyl bromide, anhydrous potassium carbonate, benzyltriethylammonium chloride and ethanol, heat up and react fully; Purify the product, and then react fully with m-chloroperbenzoic acid to obtain a brown-red liquid; Wash, filter and dry to obtain waterborne epoxy modified naringin. Carbon fiber sizing agent, including 0.1 part to 10 parts of waterborne epoxy modified naringin, 0.2 part to 10 parts of surfactant, 0.1 part to 5 parts of lubricant, 0.1 part to 5 parts of binder, 0.2 part to 5 parts of antistatic agent, and 100 parts of water. Preparation of sized carbon fiber: Place the prepared sizing agent in a sizing tank, impregnate the carbon fiber and complete wire drawing and sizing; Use air drying and winding.

The invention provides a preparation method of a polysaccharide corrosion inhibitor, which comprises the following steps: a) carrying out nucleophilic substitution reaction on beta-cyclodextrin and allyl bromide in an aprotic polar solvent at 0 DEG C under an alkaline condition to obtain allyl beta-cyclodextrin with double bonds; b) dissolving xanthan gum in water under an anaerobic condition, adjusting the pH value to 3-7, adding an ammonium ceric nitrate initiator, then adding the allyl beta-cyclodextrin obtained in the step a), and carrying out a free radical graft copolymerization reaction at 50-80 DEG C; and after the reaction is completed, adding a terminating agent, precipitating, filtering and drying to obtain the xanthan gum grafted beta-cyclodextrin corrosion inhibitor. The natural polysaccharide beta-cyclodextrin and xanthan gum are used as main raw materials, so that the natural polysaccharide beta-cyclodextrin and xanthan gum are wide in source, renewable and biodegradable. Any toxic and harmful heteroatom (such as N, S, P and the like) or a high-toxicity catalyst is not used or introduced in the whole preparation process, and the final product is non-toxic and pollution-free and completely conforms to the concepts of green chemistry and sustainable development.

The application discloses a preparation method of 2-pyrrolidone derivatives, which comprises the following steps: N-allyl bromoacetamide, aryl boronic acid, bis(triphenylphosphine) nickel dichloride, 3,4,7,8-tetramethyl-1,10-phenanthroline, formic acid, acetic anhydride and sodium carbonate are reacted at 80 DEG C for 16 hours; after the reaction is completed, post-treatment is performed to obtain the 2-pyrrolidone derivatives. The preparation method uses N-allyl bromoacetamide and aryl boronic acid as reactants, uses formic acid as a carbonyl source, has mild reaction conditions, simple operation, a wide functional group tolerance range of a substrate and high reaction efficiency. According to actual needs, a plurality of 2-pyrrolidone derivatives can be synthesized, the operation is convenient, and the practicability of the method is widened.

The invention belongs to the technical field of drug synthesis, and in particular to a method for preparing a milobalin intermediate (2E)-4-ethylheptyl-2,6-dienoic acid. Compound SM-1, i.e., (E)-2-hexenoic acid ester compounds, is reacted with allyl bromide as a raw material, and a target compound is obtained by post-processing. The reaction conditions of the present invention are mild, and the operating process is simple. The complex operation problems such as high temperature or long-term reaction and preparation of iminium salts in the prior art are solved, and the product has high purity and yield.

The invention discloses a preparation method of a 2-pyrrolidone derivative, which comprises the following steps: reacting N-allyl bromoacetamide, arylboronic acid, bis (triphenylphosphine) nickel dichloride, 3, 4, 7, 8-tetramethyl-1, 10-phenanthroline, formic acid, acetic anhydride and sodium carbonate at 80 DEG C for 16 hours, and after the reaction is completed, performing post-treatment to obtain the 2-pyrrolidone derivative. According to the preparation method, N-allyl bromoacetamide and arylboronic acid are taken as reactants, formic acid is taken as a carbonyl source, the reaction condition is mild, the operation is simple, the tolerance range of substrate functional groups is wide, and the reaction efficiency is high. Various 2-pyrrolidone derivatives can be synthesized according to actual needs, so that the method is convenient to operate, and the practicability of the method is widened.