84 results about "Halomethane" patented technology

A solid catalyst component for preparing alpha-olefin homopolymer or copolymer with high catalytic activity is prepared through reacting between C2-C4 alcohol and Mg powder under existance of halomethane to obtain Mg matches solution, reacting on inorganic carrier, drying to obtain Mg carrier, and reacting on Ti(OR)nCl4-n in inertial hydrocarbon solvent, where R is C2-C8 alkyl and n=0-4.

An oxidative halogenation process involving contacting methane, a C1 halogenated hydrocarbon, or a mixture thereof with a source of halogen and a source of oxygen, at a molar ratio of reactant hydrocarbon to source of halogen in a feed to the reactor greater than 23 / 1, and / or at a molar ratio of reactant hydrocarbon to source of oxygen in a feed to the reactor greater than about 46 / 1; in the presence of a rare earth halide or rare earth oxyhalide catalyst, to produce a halogenated C1 product having at least one more halogen as compared with the C1 reactant hydrocarbon, preferably, methyl chloride. The process can be advantageously conducted to total conversion of source of halogen and source of oxygen. The process can be advantageously conducted with essentially no halogen in the feed to the reactor, by employing a separate catalyst halogenation step in a pulse, swing or circulating bed mode. The production of methyl halide can be integrated into downstream processes for manufacture of valuable commodity chemicals.

The present invention provides a method for producing amine series with an adamantane framework, including the following steps: step 1: reacting adamantane series in a mixed liquid containing oleum and organic nitrile compounds; step 2: performing hydrolyzing treatment to a reaction liquid obtained in the step 1 to form acidamide series with the adamantane framework; step 3: performing alkali treatment to the acidamide series obtained in the step 2 to form the amine series with the adamantane framework. A method for producing quaternary ammonium salts with the adamantane framework in sequence includes the following steps: step A: reacting the amine series with the adamantane framework dissolved in a dissolvant a with aminic acid and methylene oxide or paraformaldehyde, to form dimethylamine series with the adamantane framework; step B: dissolving the dimethylamine series with the adamantane framework obtained in the step A in a dissolvant b to react with halomethane so as to form quaternary ammonium salt halogenide with the adamantane framework; step C: performing ion exchange to the quaternary ammonium salt halogenide with the adamantane framework to form quaternary ammonium salt hydroxides with the adamantane framework.

The invention relates to a method for preparing lower olefins, which mainly solves problems of the prior art, such as signal material, long process time, high production cost, etc. The invention solves the problems by using halomethane as material, contacting the material with SAPO type molecular screen catalyst in a reactor under conditions that the reaction temperature is 350-600 DEG C, the material weight hourly space velocity is 0.1-100 hour<-1>, and the reaction pressure measured by a surface pressure meter is 0-1 MPa, reacting to generate an effluent containing ethylene and propylene, then separating and obtaining ethylene and propylene, thereby, the invention is useful in industrial production of lower olefins.

The present invention relates to a method for preparing a quaternary ammonium salt containing adamantine alkyl. By means of the method of the invention, it is possible to effectively in a short time and industrially high-yield and high -purity prepare the quaternary ammonium salt containing the adamantine alkyl. The method is characterized in that it includes a step A and a step B, step A: a step of preparing 1-adamantane dimethyl amine (formula (2)) selected from a step of reacting a reactant of an adamantane hydrochloric acid and a base metal hydroxide dissolved in a solvent (a) which relative inductivity is 10.0 to 20.0 with aminic acid and methyl aldehyde or paraformaldehyde, a step of reacting 1-amidogen adamantane dissolved in the solvent (a) with aminic acid and methyl aldehyde or paraformaldehyde, and a step of reacting 1-halogeno adamantane with dimethyl amine; step B: a step of preparing a 1-adamantane trimethyl halogenation aminium salt by reacting the 1-adamantane dimethyl amine of the step A dissolved in a solvent (b) with halomethane.

The invention relates to environmentally-friendly methylating reagent methyl carbonate which replaces methylating reagents toxic to human body and endangering environment (such as dimethyl sulfate or halomethane) to synthesize environmentally-friendly methylated beta-cyclodextrin and a process of synthesizing the methylated beta-cyclodextrin with beta-cyclodextrin. The process comprises the following procedures: allowing the beta-cyclodextrin to react with the methyl carbonate in dimethyl formamide organic solvent in the presence of K2CO3, removing the K2CO3 and other insoluble substances by filtration after complete reaction, depressurizing to distill the solvent, condensing the solution; precipitating the product, filtering, soaking the crude product with absolute ethyl ether, and drying to obtain the product. The process is characterized by replacing methylated reagents toxic to human body and endangering environment (such as dimethyl sulfate or halomethane) with the environmentally-friendly methylated reagent namely methyl carbonate to react with the beta-cyclodextrin to synthesize the environmentally-friendly methylated beta-cyclodextrin. The process has the advantages of simple condition, high conversion of the beta-cyclodextrin, and high average degree of substitution of the product, and environmentally friendly characteristic.

The present invention provides a method for producing various types of arylbis(perfluoroalkylsulfonyl)methane having a bulky aryl group and an electron-accepting aryl group in which synthesis was conventionally considered to be difficult, at high efficiency; a novel arylbis(perfluoroalkylsulfonyl)methane that can be widely applied to asymmertric catalyst, various types of functional materials and the like; and a metallic salt thereof. In addition, excellent catalysts are also provided. An aryl halomethane is reacted with a sodium trifluoromethane sulfinate, the arylmethyl triflone produced thereby is reacted with a t-BuLi and the like, the lithium salt of the arylmethyl triflone obtained is reacted with a trifluoromethane sulfonic acid anhydride, and an arylbis(trifluoromethylsulfony)methane such as pentafluorophenylbis(triflyl)methane, {4-(pentafluorophenyl)-2,3,5,6-tetrafluorophenyl}bis(triflyl)methane and the like are obtained at a high yield.

The invention discloses a catalyst with a shell-core structure as well as a preparation method and an application of the catalyst. The core of the catalyst is zinc supported alumina, wherein content of alumina L acid is smaller than 0.2 mmol.g<-1>; BET specific surface area is 200-350m<2> / g; pore volume is 0.3-0.6 ml / g; the shell is alumina containing zirconium sulfate solid acid; the weight ratioof zinc supported alumina to alumina containing zirconium sulfate solid acid is 10:1-2:1; based on the weight of alumina containing zirconium sulfate solid acid as the baseline, the weight content ofzirconium sulfate solid acid is 5wt%-10wt%; based on the weight of zinc supported alumina as the baseline, content of zinc in terms of oxide is 5wt%-30wt%. The catalyst has the advantages that methane conversion rate and selectivity of halomethane as a target product are increased simultaneously, deep oxidation of halomethane is inhibited, and yield of halomethane is increased obviously.

A method for fluoromethylation of a halogenated alcohol. The method includes refluxing a halogenated alcohol with a dihalomethane under basic conditions in a first solvent to form a halomethyl ether and fluorinating the halomethyl ether in the presence of a fluorinating agent.

The invention discloses a preparation method of a catalyst for methane conversion. The method comprises the following steps: zirconium sulfate solid acid, 2-methylimidazole and aluminium hydroxide slurry are mixed, and aluminium hydroxide slurry containing zirconium sulfate solid acid and 2-methylimidazole is obtained; then the aluminium hydroxide slurry containing zirconium sulfate solid acid and2-methylimidazole performs spray soaking on zinc supported alumina, and the catalyst for methane oxyhalogenation conversion is prepared after drying and roasting. The catalyst prepared with the method has the advantages that methane conversion rate and selectivity of halomethane as a target product are increased simultaneously, deep oxidation of halomethane is inhibited, and yield of halomethaneis increased obviously.

The invention discloses a preparation method of a high-selectivity methane halogenation oxidation catalyst. The preparation method comprises following steps: (1), aluminum oxide is impregnated by an acid solution of sugar and then subjected to aging, drying and roasting treatment, and modified aluminum oxide is obtained; (2), zinc is supported to modified aluminum oxide prepared in the step (1), and after drying and roasting, zinc supported aluminum oxide is prepared; (3), zirconium sulfate solid acid and aluminum hydroxide slurry are mixed, and aluminum hydroxide slurry containing zirconium sulfate solid acid is obtained; (4), zinc supported aluminum oxide is subjected to spray soaking by the aluminum hydroxide slurry containing zirconium sulfate solid acid and prepared in the step (3), and after drying and roasting, the methane halogenation oxidation catalyst is prepared. According to the catalyst prepared with the method, conversion rate of methane and selectivity of a target product methyl halide can be increased simultaneously, deep oxidation of methyl halide is inhibited, and yield of methyl halide is obviously increased.

The invention provides a double-long-chain diester quaternary ammonium salt. Diester is introduced into a molecular structure, so that the degradability is enhanced greatly, and environmental friendliness is realized. The invention further provides a synthetic process of the double-long-chain diester quaternary ammonium salt. The process comprises the following steps of: mixing N-methyl diethanolamine with short-chain alkyl halide, adding an appropriate amount of solvent, and reacting under certain reaction conditions to obtain dihydroxyethyl ammonium halide serving as a reaction intermediate; mixing the dihydroxyethyl ammonium halide with long-chain alkyl acyl chloride, adding an appropriate amount of solvent, and reacting under certain reaction conditions; and performing rotary steaming at the end of the reaction and repeatedly recrystallizing to obtain a final solid product. In the synthetic process, a nonconventional quaternary ammonium salt synthesis route for quaternary amination and esterifying in sequence is adopted, so that the raw material transformation ratio is high, an intermediate product is easy to separate and purify, the reaction conditions are mild, the final product is in light color and has high active matter content, the solvent can be recycled, no three wastes is produced, and the use of the conventional toxic alkylation reagents such as dimethyl sulfate, halomethane and the like is avoided in the synthetic process.

The present invention provides a method for producing various types of arylbis(perfluoroalkylsulfonyl)methane having a bulky aryl group and an electron-accepting aryl group in which synthesis was conventionally considered to be difficult, at high efficiency; a novel arylbis(perfluoroalkylsulfonyl)methane that can be widely applied to asymmertric catalyst, various types of functional materials and the like; and a metallic salt thereof. In addition, excellent catalysts are also provided. An aryl halomethane is reacted with a sodium trifluoromethane sulfinate, the arylmethyl triflone produced thereby is reacted with a t-BuLi and the like, the lithium salt of the arylmethyl triflone obtained is reacted with a trifluoromethane sulfonic acid anhydride, and an arylbis (trifluoromethylsulfony)methane such as pentafluorophenylbis(triflyl)methane, {4-(pentafluorophenyl)-2,3,5,6-tetrafluorophenyl}bis(triflyl)methane and the like are obtained at a high yield.

The invention discloses a chrysanthemum ester molecularly imprinted polymer preparing method and relates to a molecularly imprinted polymer preparing method. The chrysanthemum ester molecularly imprinted polymer preparing method includes the following steps that firstly, chrysanthemum ester type template molecules, styrene, halomethane, a cross-linking agent, a stabilizing agent and an initiating agent are evenly mixed and are stirred at the temperature of 50-80 DEG C after nitrogen leading and aerating; secondly, after a reaction is over, standing and layering are conducted, supernatant is removed, a lower-layer solid is eluted through a carboxylic acid and alcohol mixing solution, and chrysanthemum ester molecularly imprinted polymer powder is obtained. The preparing chrysanthemum ester molecularly imprinted polymer is in a powder form, powder-form polymers are in a microsphere shape, surface hole forming is obvious, the powder-form polymers can be directly used for extracting chrysanthemum ester pesticide residues from food media without being ground, and the recovery rate can reach more than 90 percent. According to the chrysanthemum ester molecularly imprinted polymer preparing method, processing does not need to be conducted again, the preparing process is simple, the technology is stable, and the preparing cost is low.

The invention relates to the field of fine chemical engineering, and particularly relates to a preparation method of 3-substituted dimethyl pentodiate and pentene diester. According to the preparationmethod of 3-substituted dimethyl pentodiate and pentene diester, malonic ester and halomethane are used as raw materials, substitution reaction is performed under an alkaline action, then decarboxylation and esterification reaction are performed so as to prepare 3-substituted dimethyl pentodiate or pentene diester, a structural formula of 3-substituted dimethyl pentodiate is as shown in a compound (V), and a structural formula of pentene diester is as shown in a compound (IX). The preparation method of 3-substituted dimethyl pentodiate and pentene diester is mild in reaction conditions, is easy to operate and is safe. The formula is shown in the description.

The invention discloses a preparation method of a high-activity methane halogen oxidation catalyst. The preparation method comprises following steps: (1), aluminum oxide is subjected to co-impregnation by a mixed solution containing gallium and nickel and then is dried and subjected to high-temperature roasting treatment, and modified aluminum oxide is obtained; (2), zinc is supported to modifiedaluminum oxide prepared in the step (1), and after drying and roasting, zinc supported aluminum oxide is prepared; (3), zirconium sulfate solid acid and aluminum hydroxide slurry are mixed, and aluminum hydroxide slurry containing zirconium sulfate solid acid is obtained; (4), zinc supported aluminum oxide is subjected to spray soaking by the aluminum hydroxide slurry containing zirconium sulfatesolid acid and prepared in the step (3), and after drying and roasting, the methane halogen oxidation catalyst is prepared. According to the catalyst prepared with the method, conversion rate of methane and selectivity of a target product methyl halide can be increased simultaneously, deep oxidation of methyl halide is inhibited, and yield of methyl halide is obviously increased.

The invention provides a method for preparing sodium methyl taurate. According to the method, sodium methyl taurate is synthesized in one step by taking halomethane and sodium taurate as raw materials, an immobilized catalyst quaternary ammonium salt as a catalyst, and water as a solvent. The method has the advantages of high atom utilization rate, thorough reaction, no tedious separation process in the current process, low energy consumption and easiness in operation. The method has the advantages of mild reaction conditions, easily met reaction conditions under catalysis, low equipment requirements, good controllability, easy separation and high product purity, and is a green and environment-friendly preparation method.

An oxidative halogenation process involving contacting methane, a C1 halogenated hydrocarbon, or a mixture thereof with a source of halogen and a source of oxygen, at a molar ratio of reactant hydrocarbon to source of halogen in a feed to the reactor greater than 23 / 1, and / or at a molar ratio of reactant hydrocarbon to source of oxygen in a feed to the reactor greater than about 46 / 1; in the presence of a rare earth halide or rare earth oxyhalide catalyst, to produce a halogenated C1 product having at least one more halogen as compared with the C1 reactant hydrocarbon, preferably, methyl chloride. The process can be advantageously conducted to total conversion of source of halogen and source of oxygen. The process can be advantageously conducted with essentially no halogen in the feed to the reactor, by employing a separate catalyst halogenation step in a pulse, swing or circulating bed mode. The production of methyl halide can be integrated into downstream processes for manufacture of valuable commodity chemicals.

The invention discloses a catalyst for preparation of halomethane as well as a preparation method and an application of the catalyst. The catalyst has a core-shell structure, wherein the core is zinc-containing silicon oxide, the shell is aluminum oxide containing zirconium sulfate solid acid and a molecular sieve, the molecular sieve is at least one of a 5A molecular sieve, a 13X molecular sieveand mordenite, and the weight ratio of the zinc-containing silicon oxide to the aluminum oxide containing zirconium sulfate solid acid and the molecular sieve is (10:1)-(2:1); on the basis of the weight of aluminum oxide containing zirconium sulfate solid acid and the molecular sieve, the weight content of zirconium sulfate solid acid is 5wt%-10wt%, and the content of the molecular sieve is 1wt%-10wt%; on the basis of the weight of the zinc-containing silicon oxide, the content of zinc is 5wt%-30wt% based on oxide. The catalyst can increase the conversion rate of methane and the selectivity ofthe target product halomethane, inhibit deep oxidation of halomethane and further remarkably increase the yield of halomethane.

The invention discloses a catalyst for methane oxyhalogenation conversion as well as a preparation method and an application of the catalyst. The catalyst is of a core-shell structure, wherein the core is zinc-containing silicon oxide, and the shell is alumina containing zirconium sulfate solid acid; the weight ratio of zinc-containing silicon oxide to alumina containing zirconium sulfate solid acid is 10:1-2:1; based on the weight of alumina containing zirconium sulfate solid acid as the baseline, the weight content of zirconium sulfate solid acid is 5wt%-10wt%; based on the weight of zinc-containing silicon oxide as the baseline, content of zinc in terms of oxide is 5wt%-30wt%. The catalyst has the advantages that methane conversion rate and selectivity of halomethane as a target productare increased simultaneously, deep oxidation of halomethane is inhibited, and yield of halomethane is increased obviously.

The invention discloses a preparation method of clobazam, and belongs to the field of organic synthesis. The method comprises the following steps: (1) adding 2-nitro-5-chlorodiphenylamine into a lower alcohol and water mixed solvent, adding a Pd-C catalyst, and introducing hydrogen to synthesize N-phenyl-5-chloro-1,2-phenylenediamine; (2) adding the N-phenyl-5-chloro-1,2-phenylenediamine obtained in step (1) into a THF solvent, and adding malonyl chloride in batches to obtain 1-phenyl-8-chloro-1,2,4,5-tetrahydro-1,5-benzodiazepine-2,4-dione; and (3) reacting the 1-phenyl-8-chloro-1,2,4,5-tetrahydro-1,5-benzodiazepine-2,4-dione obtained in step 2 with halomethane or dimethyl sulfate to obtain the target product clobazam. The preparation method is a simple and highly-efficient clobazam synthesis method.

The present invention provides a method for producing various types of arylbis(perfluoroalkylsulfonyl)methane having a bulky aryl group and an electron-accepting aryl group in which synthesis was conventionally considered to be difficult, at high efficiency; a novel arylbis(perfluoroalkylsulfonyl)methane that can be widely applied to asymmertric catalyst, various types of functional materials and the like; and a metallic salt thereof. In addition, excellent catalysts are also provided. An aryl halomethane is reacted with a sodium trifluoromethane sulfinate, the arylmethyl triflone produced thereby is reacted with a t-BuLi and the like, the lithium salt of the arylmethyl triflone obtained is reacted with a trifluoromethane sulfonic acid anhydride, and an arylbis(trifluoromethylsulfony)methane such as pentafluorophenylbis(triflyl)methane, {4-(pentafluorophenyl)-2,3,5,6-tetrafluorophenyl}bis(triflyl)methane and the like are obtained at a high yield.

The invention relates to a preparation method of a carbamyl amino pyrazol derived compound, belongs to the technical field of drug intermediates and aims to solve the problem that an existing synthetic route is complicated and is uneasy to operate. The preparation method of the carbamyl amino pyrazol derived compound comprises the steps that in the presence of an acid-binding agent, a compound shown in a formula II and triphenyl halomethane perform condensation reaction in an organic solvent to obtain an intermediate product compound shown in a formula III; then, in the presence of inorganic base, the compound shown in the formula III is subjected to ester hydrolysis reaction, and a compound shown in a formula IV is obtained; the compound and trinitride perform Curtius rearrangement reaction to obtain a compound shown in a formula V; the compound shown in the formula V and BoxEDA perform condensation reaction to obtain the carbamyl amino pyrazol derived compound. The preparation methodhas the advantages that raw materials are easy to obtain, a reaction route operation is simple, and the product yield and purity are high.

The invention discloses side chain type water-soluble polyquaternium shown as a formula and a preparation method thereof. After ethanolamine and long-chain chloralkane are subjected to substitution reaction under an alkaline condition; a reaction solution is not treated and is subjected to the substitution reaction with 3-p-toluenesulfonyloxymethyl-3-ethyl-oxetane to generate a monomer containinga tertiary amine group; the monomer and a hydrophilic monomer are subjected to cationic ring-opening copolymerization under the action of an initiator and a co-initiator, and are treated through halomethane to obtain the side chain type water-soluble polyquaternium. The polyquaternium is novel in structure and low in toxicity and has good water solubility and a relatively strong bacterium-inhibition and antibacterial function; no bubbles are generated in a utilization process; the polyquaternium has a wide application prospect in the fields of industrial circulating water treatment, personal care products, papermaking, coating, metal processing, textiles and the like.

The invention discloses a catalyst for methane conversion as well as a preparation method and an application of the catalyst. Zinc is taken as an active component of the catalyst, one or more of cobalt, manganese and cerium is / are taken as auxiliaries, and silicon oxide is taken as a support; in terms of weight content of the final catalyst, the content of the active component in terms of oxide is5wt%-30wt%, and preferably 10wt%-25wt%; the content of the auxiliaries in terms of oxide is 1wt%-8wt%, and preferably 3wt%-5wt%. The catalyst has the advantages that methane conversion rate and selectivity of halomethane as a target product are increased simultaneously, deep oxidation of halomethane is inhibited, and yield of halomethane is increased obviously.

The invention discloses an application of pseudolarix lactone H in pseudolarix seeds in preparation of functional foods and medicines for treating diabetes. The pseudolarix lactone H is prepared by the following methods: grinding the pseudolarix seeds, extracting by using a solvent A, extracting the filter residue by using a solvent B, concentrating and drying the extracting solution extracted twice, and merging to obtain a total crude extract; dispersing the total crude extract in an aqueous solution of low alcohols, extracting and degreasing by using petroleum ether, removing the petroleum ether phase, concentrating and drying the raffinate, and thus obtaining a triterpene extract of the pseudolarix seeds; and further taking a mixed solution of halomethane and acetone as a solvent, recrystallizing the triterpene extract, and thus obtaining the pseudolarix lactone H. The preparation method is simple in process, convenient in operation and low in energy consumption and is suitable for extracting and producing the pseudolarix lactone H from the pseudolarix seeds in a large scale.

The invention discloses a catalyst for methane oxyhalogenation as well as a preparation method and an application of the catalyst. The core of the catalyst is zinc supported alumina, wherein content of alumina L acid is smaller than 0.2 mmol.g<-1>; BET specific surface area is 200-350m<2> / g; pore volume is 0.3-0.6 ml / g; the shell is alumina containing zirconium sulfate solid acid and a molecular sieve, and the molecular sieve is at least one of a 5A molecular sieve, a 13X molecular sieve and a mordenite molecular sieve; the weight ratio of zinc supported alumina to alumina containing zirconiumsulfate solid acid and the molecular sieve is 10:1-2:1; based on the weight of alumina containing zirconium sulfate solid acid and the molecular sieve as the baseline, the weight content of zirconiumsulfate solid acid is 8wt%-15wt%, and the content of the molecular sieve is 3wt%-7wt%; based on the weight of zinc supported alumina as the baseline, content of zinc in terms of oxide is 5wt%-30wt%.The catalyst has the advantages that methane conversion rate and selectivity of halomethane as a target product are increased simultaneously, deep oxidation of halomethane is inhibited, and yield of halomethane is increased obviously.

The invention provides a continuous production process of dicamba methyl ester. The process comprises the following steps: A) 5-bromo-3,6-dichlorosalicylic acid is subjected to a reaction under an alkaline condition and under the action of metal powder to remove bromine atoms in para-positions of hydroxyl, and 3,6-dichlorosalicylic acid is obtained; B) 3,6-dichlorosalycylic acid and halomethane are subjected to an etherification reaction in a mixed solvent of water and methanol, and methyl 3,6-dichloro-2-methoxybenzoate is obtained; C) methanol is removed by distillation; D) a system after distillation is left to stand for laying, an organic phase is distilled, and dicamba methyl ester is obtained. By means of the preparation process, continuous production can be realized, workers are notrequired to make direct contact with materials, the control degree is high, the production operation environment is greatly improved and safer, the process route and equipment are simple, the production cost is low, besides, the product yield and purity are greatly improved, and a superior route suitable for mass industrial production is provided.