117 results about "Bromide methyl" patented technology

The invention discloses a synthesis process of vecuronium bromide. The synthesis process comprises the following steps: generating epiandrosterone sulfonyl ester (III) by carrying out esterification reaction between epiandrosterone (II) and paratoluensulfonylchloride; generating 5Alpha-androst-2-alkene-17-ketone (IV) by carrying out elimination and dehydration reaction between the (III) and 2,6-lutidines; generating 17-acetoxyl-5Alpha-androstane-2,16-diene (V) by carrying out enolization and esterification reaction between the (IV) and isopropenyl acetate; generating (2Alpha, 3Alpha, 16Alpha,17Alpha)-diepoxy-17Beta-acetyl-5Alpha-androstane (VI) by epoxy reaction of the (V) under the effect of hydrogen peroxide; generating 2Beta, 16Beta-di(1-piperidyl)-5Alpha-androstane-3Alpha-hydroxyl-17-ketone (VII) by ring-opening and addition reaction of the (VI) under the effect of hexahydropyridine; generating 2Beta, 16Beta-di(1-piperidyl)-5Alpha-androstane-3Alpha,17Beta-diol (VIII) by the (VII)under the reduction of potassium borohydride; generating 2Beta, 16Beta-di(1-piperidyl)-3Alpha, 17Beta- acetoxyl-5Alpha-androstane (IX) by carrying out esterification reaction of the (VIII) under the acetylation of acetic anhydride; and generating vecuronium bromide (I) by carrying out quaternary ammonium salt reaction between the (IX) and bromomethane. The invention has the advantages of low cost,less pollution and high yield.

The invention discloses a preparation method of trans-4-replacing cyclohexyl formaldehyde and trans-4-replacing cyclohexyl olefin, which uses trans-4-replacing cyclohexyl formic acid as raw material, and prepares the trans-4-cyclohexyl olefin by acyl chloride, silicon hydrogen alkane reduction, and reaction with methyl bromide triphenylphosphine quarter phosphonium. The preparation method of the trans-4-replacing cyclohexyl formaldehyde and the trans-4-replacing cyclohexyl olefin is simple in method, clean in using, and has wide application prospect.

The invention provides a method for preparing a sulfimide compound as shown in the formula (1): MN(SO2CF3) (SO2CF3), wherein M represents H and IA group alkali metals. The sulfimide compound utilizes bromotrifluoromethane easily obtained in industrial production as a raw material, and is prepared by the steps of sulfinatodehalogenation, bromination and ammoniation. The method can be used for organic synthesis, has high purity and yield as well as low cost, and can solve the problem that the sulfimide compound is difficult to realize large-scale application in industrial production due to high cost.

The invention relates to a trifluoromethanesulfonic acid preparation method. The method includes: taking halogenated trifluoromethane as a raw material, adding zinc powder and terahydrofuran under the environment of nitrogen protection and feeding trifluoro bromomethane gas prior to adding catalytic amount to obtain lodine; obtaining trifluoromethyl zinc halide through temperature control reaction, adding sulfur trioxide for continuous reaction to generate halogenated trifluoromethane sulfonic acid zinc; adding reaction liquid into alkali liquid for neutralization, evaporating filter liquid to dryness to obtain solid sodium trifluoromethanesulfonate salt prior to acidizing and rectifying to obtain trifluoromethanesulfonia acid. With the method, generation of accessory substances during the production is effectively reduced; the situation about higher fluorinion, chloridion and sulfate ion in trifluoromethanesulfonia acid products in a traditional technology is avoided. In addition, the purity of the trifluoromethanesulfonia acid obtained from distillation and purification can reach 99.95% above, and the yield can reach 83%.

The invention discloses a method for preparing tiotropium bromide, which comprises the following steps of: preparing scopine-2,2-dithienyl glycolate from scopine and methyl 2,2-dithienyl glycolate, reacting the scopine-2,2-dithienyl glycolate with methyl bromide to prepare a tiotropium bromide crude product, and refining the tiotropium bromide crude product to obtain a tiotropium bromide finishedproduct. The method is characterized in that: the scopine and the methyl 2,2-dithienyl glycolate undergo ester exchange reaction under the action of dimethylbenzene, and the mixed catalysts of sodiumand sodium methoxide, and after the reaction, reaction solution is post-treated to obtain the scopine-2,2-dithienyl glycolate. In the method, in the process of preparing the scopine-2,2-dithienyl glycolate, the sodium and the sodium methoxide are simultaneously taken as the catalysts, and scopine isomer content after the reaction is less than 0.1 percent which completely meets specifications in the trial standards of European pharmacopoeia; and the method solves a big problem for the conventional preparation of the tiotropium bromide and is easy to realize industrial production.

The invention provides a synthesis process of pyraclostrobin, which can be divided into five steps: (1) o-nitrotoluene and NH ₄ Cl reduction reaction occurs under the catalysis of zinc powder and alloy micronano powder; (2) acylation reaction of hydroxylamine; (3) methylation reaction; (4) N-methoxy-N -2-bromomethylphenyl methyl carbamate; (5) use DMF as a solvent to dissolve N-methoxy-N-2-bromomethyl phenyl methyl carbamate and make a solution for subsequent use, and 1-( 4‑chlorophenyl)‑pyrazolol, K ₂ CO ₃ , acetone and put them into the reactor together, after heating up and refluxing, slowly add N-methoxy-N-2-bromomethylphenyl carbamate solution in the reactor, and the product pyrazole ether is obtained after the reflux reaction is completed Strostrobin. Compared with the prior art, the preparation method of the present invention is simple, the raw materials are cheap and easy to obtain, the reaction conditions are mild, and the purity and yield of the obtained target product are high.

The invention discloses a synthesis method of eugenol methyl ether. In the method, eugenol and dimethyl carbonate (DMC) are taken as raw materials, and eugenol methyl ether is prepared through liquid-solid phase reaction under pressurization while base catalysis is performed. The green organic chemical raw material, namely DMC, is utilized for replacing traditional dimethyl sulfate, bromomethane, phosgene and other toxic and harmful methylating agents, and solid base is selected as a catalytic system. The synthesis method is a clean synthesis route of the eugenol methyl ether, is environmentally friendly, economic in preparation, convenient in post-treatment and low in corrosion to equipment. The method has great industrial application prospects.

The invention discloses a PTA (purified terephthalio acid) oxidized tail gas catalytic combustion processing method with low energy consumption. Oxidized tail gas from a high-pressure absorbing tower enters a catalytic combustion pre-heater and is heated to 295-300 DEG C, and then is mixed fully with assistant fuel methanol and fed into a combustion reactor, wherein the addition of methanol is 6.5-7.0kg/t PTA, the operation pressure of the catalyst combustor is 1.0-1.2MPa, the gas inlet temperature is 295-300 DEG C, and the normal outlet temperature is 395-405 DEG C. Through catalytic combustion reaction, a small amount of organic matter and CO in the oxidized tail gas is combusted to generate CO2 and H2O, and methyl bromide is converted to bromide and hydrogen bromide. Most part of gas from the catalyst combustor enters into a tail gas expanding machine to act to recover energy. The gas inlet temperature of the tail gas expanding machine is 395-405 DEG C, the inlet pressure is 1.0-1.2MPa, the gas outlet temperature is 105-115 DEG C and the outlet pressure is 0.1MPa. The tail gas outputted from the expanding machine is washed with alkali by a tail gas washing tower to remove HBr and Br2, and then is exhausted into air after reaching an environmental protection emission standard. Compared with an existing HPCCU technology, the mechanical consumption amount is reduced by 6.5-7.0kg/tPTA, the methanol consumption amount is reduced by about 50%, the energy consumption of the catalytic combustion system is reduced significantly, the processed tail gas reaches the environment emission standard, and the economic benefits are significant.

The invention discloses a supported catalyst with a mesoporous structure, and a preparation method and application thereof. The catalyst comprises, by weight, 0.5 to 20% of zinc oxide, 10 to 50% of zinc halide and 0.1 to 20% of a modification aid, with the balance being a modified mesoporous alumina carrier. The preparation method for the catalyst comprises the following steps: (1) preparing the modified mesoporous alumina carrier; (2) loading an active metal zinc precursor on the carrier obtained in the step (1) by using an equivalent-volume impregnation manner and carrying out drying and roasting so as to prepare a catalyst precursor; and (3) subjecting the catalyst precursor prepared in the step (2) to halogenation so as to prepare the catalyst for preparation of isobutene from halogenated methane. The catalyst is capable of obviously improving selectivity of isobutene when used for a reaction for preparation of isobutene from bromomethane.

The invention discloses a catalyst using a modified ZSM-5 molecular sieve as a carrier and a preparation method and application thereof. The preparation method of the catalyst includes the following steps that 1, a modified hydrogen type ZSM-5 molecular sieve carrier is obtained by using water vapor and an acid treated hydrogen type ZSM-5 molecular sieve having complexing properties; 2, zinc oxide and/or an additive oxide are introduced to the modified hydrogen type ZSM-5 molecular sieve carrier; 3, incomplete bromination treatment is conducted on the modified hydrogen type ZSM-5 molecular sieve carrier introduced with the zinc oxide. The catalyst prepared by adopting the method is used for methyl bromide to prepare isobutylene, and the selectivity of isobutene can be remarkably improved.

The invention relates to a novel method for synthesizing cyclopropyl bromide. The novel method comprises the following steps: carrying out a reaction between cyclopropyl carboxylic acid and carbonyl diimidazole to generate cyclopropyl acyl imidazole, then mixing the intermediate with bromo-trichloromethane, adding an oxidizing agent slowly under the condition that the temperature is kept to be 10 to 140 DEG C for a free radical deacidification bromination reaction, so as to obtain a cyclopropyl bromide crude product, and carrying out simple normal pressure rectification to obtain a product of which the purity is 99 percent or higher. The novel method has the advantages that the reaction conditions are mild; the used reagents are conventional, cheap and high in availability; mercuric oxide, which is a highly toxic product, is not used any more; the novel method is suitable for industrial scale-up production.

The present invention relates to one chiral amino acid derivative. L-amino acid as initial material is processed through four steps of esterification, carboxyl reduction, amino methylation and forming salt with bromomethane to synthesize the R-configuration chiral amino acid derivative. The derivative is used as novel chiral inclusion resolving agent and may be used in the resolving inclusion of ketoprofen as one non-steroid antiphlogistic medicine.

The invention relates to a fumigation agent methyl bromide activated carbon fiber adsorption recovery device. According to the fumigation agent methyl bromide activated carbon fiber adsorption recovery device, a plurality of ACF adsorption towers are connected to the same pipeline in parallel. The two ends of the pipeline are communicated with a fumigated base, so that a methyl bromide ACF circulation system is formed. The methyl bromide ACF circulation system is further communicated with a circulation heating system and a vacuum desorbing system. The method comprises the steps that a, methyl bromide gas in the fumigated base is introduced to the fumigation agent methyl bromide activated carbon fiber adsorption recovery device; b, a vacuum pump K1002 is started for vacuum desorbing; c, heat cycling is conduced; d, the ACF adsorption towers on which desorbing is conducted are prepared to conduct next adsorption; e, the desorbed methyl bromide gas is converted and sent to the base to be fumigated. Recycling and reusing of the fumigation agent methyl bromide are achieved after the fumigated base is fumigated, the fumigated base and a recycling and reusing device are organically combined, and recycling and reusing of the methyl bromide for fumigating of the fumigated base are achieved.

The invention discloses a process for activating A-type or X-type molecular sieve under room temperature by using chloromethane (chloroethane). The activated molecular sieve is used for refining haloalkane with low boiling point such as chloromethane (chloroethane) and methyl bromide, and the refining process comprises the following steps: an exothermic reaction between the crystals in the molecular sieve and the chloromethane (chloroethane) is processed with a chemical equation of H2O+RCL->ROH+HCL+Q, in which the generated alcohol and hydrogen chloride are absorbed by alkali liquor and the unreacted chloromethane (chloroethane) are recycled after being condensed. After being fully purged by high-purity nitrogen, the activated molecular sieve is placed into a molecular sieve tower of the haloalkane refining system and then the haloalkane with low boiling point is refined according to the processes of adding the haloalkane liquid-phase absorbent, gasifying, alkali washing and acid removing, cooling and impurity removing, drying and dewatering, removing the molecular sieve and fully condensing and liquefying so as to refine the finished products with high purity.

The invention discloses a technique of synthesizing low-substituted methyl bromide with photochemical reaction. The technique is provided with a photoreaction area and a circular condensing area. A reactor in the photoreaction area is vacuum before the reaction and can be illuminated by light and heated. The circular condensing area can be communicated with or is disconnected with the reactor, which is provided with a hydrogen bromide absorption tube and refrigerating circulation liquid. The circular condensing area is also connected with a product storage tank. When the reactor is vacuum, the reactor is filled with liquid bromine and methane. Light source is opened and the photoreaction begins. When the brownish red color of the liquid bromine in the reactor disappears, the reactor is heated at once to vaporize the reaction product completely. At the moment, the circular condensing area is communicated to exchange gas circularly for the product. The low-substituted methyl bromide is obtained in the product storage tank. The invention takes visible light as the light source. The chemical reaction principle is simple. The invention is applicable to commercial process.

The invention belongs to the technical field of chemical industry, and discloses a trans-1, 3-dichloropropene compound, a cis-1, 3-dichloropropene compound, a cis-trans-1, 3-dichloropropene compound and a rectification method thereof, the dichloropropene compound is composed of the trans-1, 3-dichloropropene and the cis-1, 3-dichloropropene or the cis-trans-1, 3-dichloropropene; the trans-1, 3-dichloropropene is mainly used for preparing chloramine, and the chloramine is used for preparing final product clethodim. The cis-trans mixed 1, 3-dichloropropene is used as a soil fumigant and a soil insecticide, radically treats underground nematodes and replaces methyl bromide in a methyl bromide project of the United Nations. The cis 1, 3-dichloropropene and a cis-trans mixed 1, 3-dichloropropene product are blended to serve as the cis-trans mixed 1, 3-dichloropropene to be still used for radically treating the underground nematodes. The dichloropropene compound can inhibit or directly killvarious nematodes and relieve nematode disease damage, the control effect reaches 98% or above, and the lasting period is 3 months or above.

The invention relates to 3-cyclic ether methyl trifluoro-potassium borate, in particular relates to a synthesis method of 3-cyclic ether methyl trifluoro-potassium borate, mainly solving the technical problems of the existing preparation method that the catalyst is expensive, the reaction condition is severe, the synthesis process is long and the like. According to the technical scheme, the synthesis method comprises the following steps: performing an addition reaction on 2-cyclic ether olefin taken as a raw material and borane; quenching with pinacol so as to obtain 3-cyclic ether-based pinacol boric acid ester; removing protons from the 3-cyclic ether-based pinacol acid ester by using a strong alkali and reacting with chlorobromomethane so as to obtain 3-cyclic ether methyl pinacol boric acid ester; and finally, performing a reaction on the 3-cyclic ether methyl pinacol boric acid ester and potassium bifluoride so as to obtain the 3-cyclic ether methyl trifluoro-potassium borate. The 3-cyclic ether methyl trifluoro-potassium borate is an important medicinal compound structure-modified micromolecule in the research field of a novel medicine.

The invention discloses a synthetic method of 1,1-dibromo-2,2-dual(chloromethyl)-cyclopropane. The method comprises the following steps that chlorine substitution reaction happens to 2-amino-2-hydroxylmethylpropane-1,3-diol to obtain (1,3-dichloro-2-(chloromethyl)propane-2-group)amino-sulfone-ketone; the (1,3-dichloro-2-(chloromethyl)propane-2-group)amino-sulfone-ketone is hydrolyzed through a concentrated sulfuric acid aqueous solution to obtain 1,3-dichloro-chloromethylpropyl-2-amine-sulfate; the 1,3-dichloro-chloromethyl-propyl-2-amine-sulfate is subjected to salt dissolution on the alkaline condition, and is subjected to cyclization to form 2,2-dual(chloromethyl)aziridine; reaction happens to 2,2-dual(chloromethyl)aziridine and sodium nitrite to form 3-chloro-2-chloromethyl-propyl-1-alkene; and the 3-chloro-2-chloromethyl-propyl-1-alkene reacts with bromoform on the alkaline condition to generate 1,1-dibromo-2,2-dual(chloromethyl)-cyclopropane. The synthetic method of 1,1-dibromo-2,2-dual(chloromethyl)-cyclopropane is simple and can be used for enlarged production.

The invention discloses waterproof paint not liable to peel off. The paint is prepared from following raw materials by weight: 2.5-3.8 parts of dibromomethane, 3.5-3.7 parts of tetrahydrofuran, 3.5-4.7 parts of nonylphenol polyoxyethylene ether, 3-7 parts of kaolin, 1.2-1.7 parts of phenylethyl naphthol polyoxyethylene ether, 2.5-5 parts of octadecanol polyoxyethylene ether, 1.2-2.2 parts of N-methyl-alkylamido taurine salt and 1.8-3.6 parts of a sorbitol-fatty acid ester. Compared with waterproof paint at present, the paint provided by the invention has high water resistance, high water proofness and high tensile strength and is healthy and environmental friendly; environment pollution is reduced and wall peeling off caused by rain wash after longtime use is avoided; the paint provided by the invention can prevent being washed by acid rain; and the paint film wound not peel off after rain wash, thus reducing the probability that rain permeates into the wall and corrodes the wall to cause losses.

The invention provides a preparation method of otilonium bromide, belonging to the technical field of medicine production. The method comprises the following steps: reacting o-octanoxy benzoic acid serving as a raw material and chloroformate to obtain a product; then, carrying out condensation on the product and p-aminobenzoic acid to obtain 4-(2-octanoxybenzoylamino)benzoic acid; reacting 4-(2-octanoxybenzoylamino)benzoic acid and diethylaminoethyl chloride to obtain N,N-diethyl-2-[4-(2-octanoxybenzoylamino)benzoyloxy]ethylamine; and reacting N,N-diethyl-2-[4-(2-octanoxybenzoylamino)benzoyloxy]ethylamine and bromomethane to generate otilonium bromide. The preparation method has the advantages of simple process, low reaction byproduct content, high yield, simplicity and convenience in operation, economical efficiency, environmental friendliness and high industrial popularization value so as to be suitable for large-scale industrial production.

The invention provides an alkaline earth metal modified supported catalyst as well as a preparation method and application thereof. The alkaline-earth metal modified supported catalyst comprises zinc oxide, zinc halide, an alkaline earth metal oxide and an alumina supporter; in percentage by weight of the catalyst, zinc oxide accounts for 0.5-20%, zinc halide accounts for10-50%, the alkaline earth metal oxide accounts for 0.1-20%, and the balance is the alumina supporter. The preparation method of the catalyst comprises the following steps: (1) loading a zinc element precursor and an alkaline earth metal precursor on the alumina supporter with a co-impregnation method, and performing drying and roasting to obtain a catalyst precursor; (2) performing halogenation treatment on the catalyst precursor obtained in the step (1), thereby preparing the alkaline-earth metal modified supported catalyst . When the alkaline-earth metal modified supported catalyst is used in reaction of preparing isobutene from methyl bromide, the selectivity of isobutene can be remarkably improved.

The invention belongs to the technical field of fuel cells, and provides a polyethyleneimine diaphragm for preparing hydrogen for a fuel cell, and a preparation method thereof. The method comprises the following steps: grafting a silicon base on polyethyleneimine, then forming a sol with polyvinyl alcohol under an acidic condition, converting the sol into a gel material, forming a film on the surface of an asbestos diaphragm, putting the film into a methyl alcohol solution containing methyl bromide, and curing to obtain the silicon dioxide modified polyethyleneimine diaphragm. Compared with atraditional method, the preparation method of the invention has the following characteristics that the silicon dioxide modified polyethyleneimine diaphragm prepared by the method has the advantages that inorganic silicon dioxide is formed by removing methyl from organic silicon, so that the hydrophilic performance of a diaphragm material is improved, the selective permeability to OH<-> is improved, the performance is stable in a use process, and the polyethyleneimine diaphragm has a wide application prospect in the field of hydrogen production by electrolyzing water.

The present invention discloses a group of adjuvants for making atmosphere heat treatment of metal material and its application. They includes four classes: (1). Any one kind of haloid element compounds of carbon tetrachloride, freon, methenyl bromide and iodomethane; (2) any one kind of metal element compounds of manganese naphthenate, nickel nitrate and ferrocene; (3) any one kind of nitrogen-containing compounds of cyanuramide, nitrobenzol, aniline and acetylamine; and (4). and any one kind of rare earth lanthanum or cerium compounds of cerous nitrate and lanthanum nitrate. They can be used in the heat treatment atmopshere-making raw materials or atmospheres of methyl alcohol, acetone, kerosene, propane and natural gas, and can raise gas yield of atmosphere raw material, can reduce carbon black formation, and can reduce the technological temp. of atmosphere chemical heat-treatment carburization.

The invention discloses a preparation method of an alkali-resistant yellow disperse dye, which comprises the following steps: reacting 2, 4-diaminotoluene with 2, 4-dinitrofluorobenzene to obtain a compound of formula (II-1); performing diazotization and coupling reaction to obtain a compound shown as a formula (III-1); and reacting with methyl bromide to obtain the compound shown in the formula (I-1). The dye prepared by the preparation method can realize short-process dyeing on polyester fiber fabrics, not only can improve the alkali resistance of alkali-resistant disperse dyes under the condition that the pH value is 10-12, but also can significantly improve the dyeing defect or non-uniform dyeing phenomenon of the polyester fabrics.

The invention discloses a method for preparing tetramethyl ammonium bromide. The method includes the steps that methyl aryl ether is subjected to demethylating reaction under the acid condition to generate gas containing methyl bromide, the gas containing methyl bromide is firstly introduced into an alkaline solution for adsorption, overflow gas then sequentially passes a particle activated carbon filler adsorption column and a particle anhydrous calcium chloride filler adsorption column, and pure dried methyl bromide gas is obtained; the methyl bromide gas is introduced into stirred absolute ethyl alcohol to obtain a methyl bromide and ethanol solution; dried trimethylamine gas is introduced into the methyl bromide and ethanol solution, and tetramethyl ammonium bromide precipitate is generated through reaction. The problem about recycle and use of the side product methyl bromide of the demethylating reaction of methyl aryl ether is solved through the simple method, the methyl bromide absorption rate is nearly 100%, the technology is simple and feasible, emission of three wastes meets requirements, methyl bromide recycle cost is low, and competitiveness is extremely good.

The invention discloses a method for preparing clodronate disodium. The method comprises the following steps of: performing methylenation, chlorination, acid hydrolysis and salification on triethyl phosphate and dibromomethane which serve as raw materials to obtain the clodronate disodium. According to the method, the clodronate disodium is produced by taking triethyl phosphite is used as the raw materials, so that the cost of the raw materials is reduced substantially, the method is easy to operate, and industrial production is easy to implement; derosination reaction of an intermediate II is performed by an acid hydrolysis method, the reaction condition is mild, the reaction time is shortened to 1 to 3 hours from 10 hours, and the production efficiency is improved greatly; the purity of the product and the clarity of a solution are high, so the clodronate disodium can be used for preparing high-quality clodronate disodium injections and clodronate disodium capsules, and the risk of clinical medication is reduced; and hydrochloric acid and other organic solvents which are used in the process can be recycled, so the method is environment-friendly.