23 results about "Butyl bromide" patented technology

The application discloses a synthesis method of afugan, which comprises the following steps: 1-[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroacetone and 4-acetylnaphthalene carboxylic acid are added into a solvent, a base is added, DMAP is added after complete reaction at 50-80 DEG C, acetic anhydride is added dropwise, tetrabutylammonium bromide is added after complete reaction, and an aqueous solution of sodium hydroxide and hydroxylamine hydrochloride is added, and reaction is carried out at 0-5 DEG C, so that an intermediate is obtained; the intermediate is reacted with acyl chloride under the action of DMF and dichloromethane, so that 4-(5-(3-chloro-5-(trifluoromethyl)phenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole-3-yl)-1-naphthalene carboxylic chloride is prepared; 2-amino-N-(2,2,2-trifluoroethyl)acetamide hydrochloride and a dichloromethane solution of a base are added dropwise, and reaction is carried out at 0-5 DEG C, so that afugan is obtained. The method has a short route, high yield and suitability for large-scale industrial production.

The invention belongs to the technical field of wet metallurgy extraction agents, and particularly relates to an amide extraction agent and a preparation method and application thereof. The preparation method of the amide extracting agent comprises the following steps: (1) putting n-butyl bromide and sec-butylamine into a reactor, reacting in a homogeneous reactor for 6-10 hours, washing with a saturated sodium bicarbonate solution after the reaction is finished, then separating liquid, and carrying out rotary evaporation on an organic phase to obtain N-butyl sec-butylamine; (2) dissolving N-butyl sec-butylamine in an organic solvent, dropwise adding diglycyl chloride into the solvent at-20 to 0 DEG C, reacting at room temperature for 1-5 hours after dropwise adding, filtering to remove precipitate, washing an organic phase with hydrochloric acid and secondary water in sequence, removing water with anhydrous sodium sulfate, performing rotary evaporation on the organic phase, and performing vacuum drying on a product to obtain the N, N '-di-n-butyl-N, N'-diglycyl chloride. The catalyst is N, N '-di-sec-butyl-3-oxoglutaramide.

This invention provides a method for preparing tetrabutylphosphine acetate and simultaneously producing sodium bromide, belonging to the field of organophosphine salt preparation and electrodialysis separation technology. The method provided by this invention uses sodium acetate and tetrabutylphosphine bromide as raw materials, and prepares tetrabutylphosphine acetate and simultaneously produces sodium bromide via displacement electrodialysis. This achieves efficient ion exchange between tetrabutylphosphine bromide and sodium acetate, and simultaneous recovery of sodium bromide. The preparation method is simple, avoids the use of large amounts of chemical reagents, and reduces environmental pollution.

The invention relates to the field of synthesis and preparation of hydroquinone, in particular to a synthesis method of high-purity hydroquinone. In order to solve the problem that in the existing process of preparing hydroquinone through a phenol hydrogen peroxide oxidation method, the selectivity of hydroquinone (HQ) is improved, and by-products with similar microstructures are generated synergistically and are difficult to remove, a composite catalysis synergistic inhibition system of phosphotungstic acid, tetrabutylammonium bromide and imidazole is adopted; through the synergistic effect of the main catalyst, the selectivity regulator and the byproduct inhibitor, HQ selectivity improvement and synchronous inhibition of trace byproducts are achieved under the optimized reaction condition, the total content of the trace byproducts is smaller than or equal to 45 ppm, the purity of the final hydroquinone product is larger than or equal to 99.995%, and the high-end application requirements of electronic-grade and photoresist raw materials are met. The technology is compatible with existing industrial equipment, operation is easy, and industrial production is met.

The invention relates to a multi-element thermodynamic accelerant for sealing carbon dioxide by hydrate and application of the multi-element thermodynamic accelerant, the multi-element thermodynamic accelerant comprises sodium glycinate (NaGly), octyl glucoside (OGP) serving as a surfactant, tetrabutylammonium bromide (TBAB) serving as a thermodynamic accelerant and tetrahydrofuran (THF) serving as an organic solvent, and after the sodium glycinate (NaGly), the octyl glucoside (OGP) serving as a surfactant, the tetrabutylammonium bromide (TBAB) and the tetrahydrofuran (THF) are mixed with water, the mass percent concentration of the NaGly is 0.001-1wt%, the mass percent concentration of the OGP is 0.001-1wt%, the mass percent concentration of the TBAB is 5-50wt%, and the mass percent concentration of the THF is 4-40wt%. NaGly can improve the stability of the hydrate, OGP can improve the generation rate of the hydrate, TBAB can improve the formation speed and efficiency of the hydrate, THF can promote rapid generation of the hydrate, the generation speed of the hydrate is remarkably increased through cooperation of NaGly, OGP, TBAB and THF, the generation time is shortened, and the storage efficiency of carbon dioxide is effectively improved.

The invention relates to the technical field of layered composite fabrics, in particular to a layered composite fabric based on a waterproof and weather-resistant coating, a preparation method and application. The layered composite fabric comprises an outer-layer fabric and an inner-layer fabric, the inner-layer fabric is a bamboo cotton fabric, the outer-layer fabric is a nylon fabric with a waterproof and weather-resistant coating, and the nylon fabric with the waterproof and weather-resistant coating is prepared by dipping a bio-based nylon fabric in a composite finishing agent and curing the bio-based nylon fabric. The composite finishing agent is prepared by the following steps: carrying out a reaction on diisocyanate, polyether polyol, bio-based polyester polyol and hydroxyl-terminated polydimethylsiloxane in N, N-dimethylacetamide, so as to prepare a polyurethane prepolymer solution; n-octadecyl diethanolamine is added for a chain extension reaction; n-butyl bromide is added, and quaternization reaction is carried out; and finally, adding the composite weather-resistant auxiliary agent, and stirring to obtain the composite finishing agent.

The present application provides a method for extracting a phenol compound and a pyridine compound from naphthalene oil stepwise by using a deep eutectic solvent (DES). The method comprises: step 1, mixing a naphthalene oil with an alkane and a DES and performing liquid separation on the mixture to obtain a deep eutectic extraction phase and a solvent raffinate phase; step 2, mixing the deep eutectic extraction phase with a first back-extraction agent and filtering the mixture to obtain a first back-extraction phase and a recyclable DES; step 3, distilling the first back-extraction phase to obtain a heteroatom mixture, mixing the heteroatom mixture with a hydrogen-acceptor-type deep eutectic extraction agent and an alkane, and performing liquid separation on the mixture to obtain a deep eutectic phenol compound extraction phase and a pyridine compound and alkane raffinate phase; and step 4, mixing the phenol compound extraction phase with a second back-extraction agent and filtering the mixture to obtain a phenol-containing second back-extraction solution and a hydrogen-acceptor-type extraction agent. A phenol product is recovered from a second back-extraction agent solution by distillation. The DES is tetraethylammonium chloride, tetrabutylammonium chloride, tetrabutylammonium bromide or tetrabutylphosphonium bromide, and glycolic acid, oxalic acid, citric acid, or p-toluenesulfonic acid.

The invention relates to a composite hydrate inhibitor for carbon sequestration, which comprises polyvinylpyrrolidone (PVP) serving as a kinetic inhibitor, tetrabutylammonium bromide (TBAB) serving as a thermodynamic accelerant and tetrahydrofuran (THF) serving as an organic solvent, and after the polyvinylpyrrolidone (PVP), the tetrabutylammonium bromide (TBAB) and the tetrahydrofuran (THF) are mixed with water, the concentrations of the PVP, the TBAB and the THF are respectively as follows: 0.001-1wt% of the PVP, 0-50wt% of the TBAB and 0-50wt% of the THF. The PVP, the TBAB and the THF are combined according to the proportion to form the composite hydrate inhibitor, and through the synergistic effect of the PVP, the TBAB and the THF, the generation speed of hydrates is increased, the carbon dioxide storage efficiency is improved, meanwhile, the aggregation degree of the hydrates can be reduced, and the blocking probability is reduced.

The invention relates to an ionic composite hydrate accelerant for carbon sequestration, which comprises amino acid salt: sodium glycinate NaGly, a surfactant: octyl glucoside OGP, a thermodynamic accelerant: tetrabutylammonium bromide TBAB and a dynamic accelerant: lauryl sodium sulfate SDS, and after the four components are mixed with water, the mass percent concentration of NaGly (0.001-1wt%) + OGP (0.001-1wt%) + SDS (0.001-1wt%) + TBAB (5-50wt%) is obtained. NaGly, OGP, TBAB and SDS are combined according to the proportion to form the ionic composite hydrate accelerant, the generation speed of hydrate is remarkably increased through cooperation of the four components, the generation time is shortened, and the sealing efficiency of carbon dioxide is effectively improved.

The invention discloses a modifier of a PA66 composite material, a preparation method of the modifier, the PA66 composite material and a preparation method of the PA66 composite material. The preparation method of the modifier of the PA66 composite material comprises the following steps: preparing a macromolecular functional connecting agent Epoxy-PSi-PBI-NH2; the preparation method comprises the following steps: preparing CNT-PSi-PBI-Epoxy; the CNT-PSi-PBI-Epoxy and the hydroxylated BF are added into tetrabutylammonium bromide, and the mixture is stirred for a reaction; and filtering the reaction solution, washing, and drying the filter cake in a vacuum drying oven to obtain the modifier BF-PSi-PBI-CNT of the PA66 composite material. According to the invention, the dispersibility of the BF-CNT in the PA66 matrix can be synchronously solved, the interface combination of the BF-CNT, the PA66 matrix and the matrix can be optimized, the synergistic enhancement of mechanics and functions (electric conduction / heat conduction) can be realized, and the mechanical property, the heat conduction property and the electric conduction property can be simultaneously improved.

The invention discloses a preparation method of perfluorobutyl sulfonamide, and belongs to the technical field of synthesis of perfluorobutyl sulfonamide. The preparation method comprises the following steps: adding a choline chloride-urea eutectic solvent, ammonium carbamate, triethylamine, tetrabutylammonium bromide, allyl (cyclopentadienyl) nickel and potassium carbonate into a reaction kettle, uniformly stirring, dropwise adding perfluorobutanesulfonyl chloride into the reaction kettle under constant-temperature heating, and heating to 70-75 DEG C after dropwise adding to continue reaction; and after the reaction is finished, cooling the reaction liquid to room temperature, adding water into the reaction liquid, stirring and dissolving, adjusting the pH value of the system to 7, extracting and separating out an organic phase, washing the organic phase, carrying out rotary evaporation, recrystallizing, and drying to obtain the perfluorobutyl sulfonamide. According to the method disclosed by the invention, the nucleophilic substitution reaction rate of the perfluorobutyl sulfonyl chloride and the ammonium carbamate can be remarkably increased, the yield and the purity of the perfluorobutyl sulfonamide are improved, and the environmental pollution is reduced.

The invention provides a synthesis method of etifoxacin, and relates to the technical field of organic synthesis, and the synthesis method comprises the following steps: adding triphenylmethyl phosphorus bromide into a solvent, adding potassium tert-butoxide at 0-5 DEG C to obtain a suspension, preparing a 2-aminobenzophenone solution, reacting the suspension at room temperature for 30-40 minutes, adding the 2-aminobenzophenone solution into the suspension, and reacting for 30-40 minutes at room temperature to obtain the etifoxacin. Completely reacting to obtain a compound 2; dissolving the compound 2 in dichloromethane, dropwise adding ethyl isocyanate, heating to room temperature, and reacting to obtain a compound 3; mixing the compound 3, Selectfluor and a compound A, adding acetonitrile, and reacting at room temperature for 60-70 minutes to obtain a compound 4; and reacting the compound 4 and sodium borohydride in ultra-dry dimethyl sulfoxide at room temperature under the protection of nitrogen to obtain etifusin. The compound A is selected from any one of potassium iodide, Selectfluor, tetrabutylammonium chloride and tetrabutylammonium bromide. According to the invention, synthesis of etifusin is realized by a metal-free catalysis and green chemical method, and the yield is high.

The invention belongs to the field of RAFT reagent synthesis, and particularly relates to a preparation method of a reversible addition fragmentation chain transfer reagent. Comprising the following steps: by taking dodecyl mercaptan as a starting raw material, generating thiolate under the action of alkali; and reacting the obtained thiolate with carbon disulfide (CS2) to generate trithiocarbonate. And reacting the obtained trithiocarbonate with trichloromethane and acetone under the catalysis of alkali, and finally acidifying to obtain 2-[dodecyl sulfenyl (thiocarbonyl) sulfenyl]-2-methyl propionic acid, namely the RAFT reagent. Tetrabutylammonium bromide is specifically selected as a phase transfer catalyst, and the catalyst system provided by the invention can realize higher product yield.

The invention discloses a preparation method of a fluralan N-1 intermediate, which comprises the following steps: S1, carrying out aldol reaction on 4-acetyl-2-methyl benzoic acid and 3 ', 5'-dichloro-2, 2, 2-trifluoroacetophenone under the action of alkali to obtain an intermediate 1; s2, dehydrating the intermediate 1, washing a mixed product obtained by reaction with diluted hydrochloric acid under a heating condition in a post-treatment process, and directly carrying out next-step reaction on a collected organic phase; and S3, adding the organic phase obtained in the step S2 into a mixed catalytic system of tetrabutylammonium bromide and 18-crown ether-6, and carrying out an intramolecular nucleophilic addition reaction to obtain the fluralan N-1 intermediate. According to the method, a second process route of the fluralana N-1 intermediate is optimized, the yield is increased, the cost is reduced, the process steps are reduced, and the method is a process route which is environmentally friendly, safe, economical, low in production cost and capable of achieving industrial production and has a very good prospect.

The invention discloses halogen-free flame-retardant nylon. The halogen-free flame-retardant nylon is prepared from the following raw materials: matrix resin, a heat-resistant agent, a flame retardant and a functional auxiliary agent, the heat-resistant agent is functionalized nano boron fiber, and the raw materials of the functionalized nano boron fiber comprise nano boron fiber, trichloromethylsilane and black phosphorus nanosheets; the flame retardant is gradient type hyperbranched polyol, and the hyperbranched polyol is prepared from the following raw materials: trimethylolpropane, diphenyl phosphate, epoxy chloropropane, glycidyl stearate and tetrabutylammonium bromide. The invention provides halogen-free flame-retardant nylon as well as a preparation method and application thereof. The flame retardant property, the mechanical property and the upper limit of heat resistance of the halogen-free flame-retardant nylon can be improved.

The invention relates to an anticorrosive metal primer and a preparation method thereof, and belongs to the technical field of paints.The component A of the primer comprises modified alloy powder, a Schiff base cobalt complex, barium sulfate, boron nitride, modified resin, a polycyclic carbonate diluent and the like; and the component B comprises a curing agent and an interface anchoring accelerator. The modified alloy powder is prepared by sintering Fe, Cr, Ni, Mo and W metal powder and carrying out surface modification through a titanate coupling agent. The Schiff base cobalt complex is prepared by compounding a Schiff base ligand and cobalt acetate. The modified resin is prepared from bisphenol S epoxy resin, epoxy propoxy propyl terminated polydimethylsiloxane, 3-(2, 2, 3, 3-tetrafluoropropoxy)-1, 2-propylene oxide, tetrabutylphosphonium bromide, 3-(trihydroxysilyl) propyl methyl phosphate, a poly cyclic carbonate diluent and propylene glycol monomethyl ether. The preparation method comprises the following steps: preparing the modified resin from bisphenol S epoxy resin, epoxy propoxy propyl terminated polydimethylsiloxane, 3-(2, 2, 3, 3-tetrafluoropropoxy)-1, 2-propylene oxide, tetrabutylphosphonium bromide, 3-(trihydroxysilyl) propyl methyl phosphate, a polycyclic carbonate diluent and propylene glycol monomethyl ether. The primer provided by the invention realizes the comprehensive performance of low-temperature rapid curing, high construction tolerance and wide temperature range environment tolerance.

The invention relates to a novel process for synthesizing gamma-mercaptopropyl triethoxy silane by a water phase method, which comprises the following steps: sequentially adding deionized water, sodium chloride, sodium hydrosulfide, potassium iodide, sodium carbonate, tetrabutylammonium bromide and cetyltrimethylammonium bromide into a reaction container, dropwise adding 3-chloropropyl triethoxy silane into the reaction container, keeping the temperature at 50-55 DEG C, reacting for 1-2 hours, filtering, washing and drying to obtain the gamma-mercaptopropyl triethoxy silane. The method comprises the following steps: adding 3-chloropropyltriethoxysilane into a reaction solution, reacting for 50-75 minutes, monitoring the reaction process through gas chromatography until the residual 3-chloropropyltriethoxysilane in the reaction solution is less than 0.5%, completing the reaction, cooling to room temperature, standing for 10-20 minutes until two phases are layered, washing and drying the organic phase, and carrying out reduced pressure distillation on the organic reagent to obtain gamma-mercaptopropyltriethoxysilane. Compared with the existing aqueous phase synthesis process, the method provided by the invention has the advantages that the mass transfer efficiency of the reaction can be remarkably improved, so that the reaction time is shortened, the yield is improved, the generation of by-products such as ethanol is effectively reduced, and meanwhile, the method is relatively light in smell in the reaction process, simple and convenient in process and easy to realize large-scale industrial production.

This invention relates to the field of aerosol technology, specifically disclosing a snow spray with good low-temperature solubility. The snow spray with good low-temperature solubility comprises the following components in parts by weight: Phase A 14-36 parts; Phase B 40.8-61.2 parts; Phase C 15-35 parts; Phase A is a compound of deionized water, stearic acid, acrylic resin, and a stabilizer; Phase B is a compound of deionized water, sodium benzoate, triethanolamine, hexadecyltrimethylammonium chloride, and tetrabutylammonium bromide; Phase C is liquefied petroleum gas. This invention has the advantage of shortening the storage time after the snow spray is prepared.

The invention discloses a preparation method of a functional polycarboxylic acid water reducing agent suitable for underwater non-dispersible concrete, which comprises the following steps: (1) adding tetrabutylammonium bromide into ethylene glycol monovinyl polyethylene glycol ether, uniformly stirring, sequentially adding NaOH powder and 2-chloroacetamide, and heating to react to obtain modified EPEG; (2) uniformly mixing olefine acid, thiohydracrylic acid and water to form a mixed solution I; and then adding the modified EPEG and the modified nano silicon dispersion liquid into water, heating and stirring to form an emulsion. And then dropwise adding the mixed solution I and an initiator solution into the emulsion at the same time, heating and stirring to react, cooling after the reaction is completed, and then adjusting the system to be neutral or acidic to obtain the functional polycarboxylic acid water reducing agent. The problems of rheological contradiction and pumping difficulty caused by the fact that the traditional technology purely depends on improvement of static viscosity are effectively solved.

The invention provides a synthesis method of 3-bromopropoxy trimethylsilane, and belongs to the technical field of chemical synthesis. The method comprises the following steps: a first step of reaction: trimethylchlorosilane and 3-chloropropanol are subjected to a reaction, and 3-chloropropoxy trimethylsilane is generated; 2, 2-methyltetrahydrofuran is used as a solvent, in the presence of a phase transfer catalyst tetra-n-butylammonium bromide, the obtained 3-chloropropoxy trimethylsilane and sodium bromide are subjected to a halogen exchange reaction, and after the reaction is completed, post-treatment is performed to obtain the 3-bromopropoxy trimethylsilane. The synthesis process is mild in condition, simple and convenient to operate and easy to control, remarkable progress is made in the aspects of safety, economical efficiency and product yield, and the method has great industrial application value.

The application relates to a hydrate carbon dioxide storage polythermodynamic promoter and application thereof, which comprises sodium glycinate (NaGly), a surfactant octyl glucoside (OGP), a thermodynamic promoter tetrabutylammonium bromide (TBAB) and an organic solvent tetrahydrofuran (THF), and the mass percentage concentration of the four mixed with water is as follows: NaGly: 0.001-1 wt%, OGP: 0.001-1 wt%, TBAB: 5-50 wt%, and THF: 4-40 wt%. In the application, NaGly can improve the stability of the hydrate, OGP can improve the generation rate of the hydrate, TBAB can improve the speed and efficiency of the hydrate formation, and THF can promote the rapid generation of the hydrate. The synergy of the four can significantly accelerate the generation speed of the hydrate, shorten the generation time and effectively improve the carbon dioxide storage efficiency.

The invention discloses an anionic fluorocarbon surfactant as well as a preparation method and application thereof, and belongs to the technical field of surfactants, the method specifically comprises the following steps: (1) in an argon atmosphere, dropwise adding hexafluoropropylene dimer and ethyl bromoacetate into a mixed solution of N-N dimethylacetamide, tetrabutylammonium bromide and potassium fluoride, and stirring to obtain a mixed solution; heating the reaction system at 80 DEG C for 24 hours, cooling to room temperature, and performing post-treatment to obtain a compound 1; (2) in an argon atmosphere, dissolving the compound 1 in absolute ether, dropwise adding into a Schlenk tube containing absolute ether and LiAlH4, stirring and reacting at room temperature for 3 hours, heating to 40 DEG C, stirring for 4 hours, cooling to room temperature, and post-processing to obtain a compound 2; and (3) dissolving the compound 2 and triethylamine in tetrahydrofuran, slowly dropwise adding chlorosulfonic acid, reacting for 3 hours in an ice-water bath, reacting for 6 hours at normal temperature, and performing post-treatment to obtain the sulfate anionic surfactant. The surfactant effectively solves the problems of environmental pollution and insufficient performance.

The invention discloses a preparation method of m-dibutylaminophenol, and relates to the technical field of carbocyclic compound preparation, the m-dibutylaminophenol comprises the following raw materials: 2-chlorophenol, 2, 6-di-tert-butyl-4-methylphenol, zinc chloride, tetrabutylammonium bromide, sodium amide, potassium tert-butoxide, an activated 3A molecular sieve, di-n-butylamine and triethylamine; according to the invention, 2-chlorophenol is used as a core reaction substrate, the structure arrangement of ortho-position chlorine atoms and hydroxyl is highly adaptive, hydrogen chloride can be accurately removed under the action of strong alkali to generate a benzyne intermediate, and a stable benzene ring skeleton is provided for a target product; through the synergistic effect of the activated 3A molecular sieve, the 2, 6-di-tert-butyl-4-methylphenol and the potassium tert-butoxide, the total impurity content is greatly reduced, the product purity and color are remarkably optimized, and the synchronous improvement of the reaction efficiency and the product quality is realized.