778 results about "Cyanation" patented technology

The invention discloses a synthetic method for loxoprofen sodium, which is prepared by taking methyl acetophenone as an initial raw material through reduction, acylation or halogen substituent, cyanation, hydrolysis, bromination, condensation, decarboxylation and salifying. The method has the advantages of easily obtained raw material, unique technology, simple and stable operation, and high productive rate in each step of reaction; and all solvents used in the synthesis process can be recycled, so the production cost is reduced greatly. Tests show that the obtained product has reliable quality and stable performance, and can be further used for making preparation of non-steroidal anti-inflammatory drugs such as the loxoprofen sodium.

The invention provides a radiation-curable alkoxy silanized hyperbranched polyester acrylate, characterized in that the radiation-curable alkoxy silanized hyperbranched polyester acrylate is produced by using a hyperbranched molecule with at least 16 functionalities as a core; acrylating or methacrylating a portion of the terminal groups of the hyperbranched molecule; and terminating a portion of the end groups of the hyperbranched molecule with an isocyanated silane coupling agent. The acrylate of the invention can be formed into a coating on polar substrates, such as glass or metal, or used as an adhesive.

The invention discloses a prolinol derivative induced chiral MOFs material with asymmetric catalysis, which belongs to the technical field of a chiral catalytic material. L-BCIP or D-BCIP is used as a chiral source; 5,5'-methylene diiso-phthalic acid, 4,4'-biphenyl acid, 3,3',4,4'-biphenyltetrazole acid or 4,4'-sulfonyl terephthalic acid is used as a connecting ligand; Ln3+ is used as a node; a three-dimensional hole channel structure is constructed by a hydrothermal method; the general formula is as follows: Ln<3+>+L+L-BCIP or D BCIP->Ln-L, wherein Ln<3+> is a rare earth metal ion; L is a connecting ligand; L-BCIP is L-N-tert-butoxycarbonyl-2-imidazole-1-pyrrolidine; and D-BCIP is D-N tert-butoxycarbonyl-2-imidazole-1-pyrrolidine. The material can be used as a heterogeneous catalyst used for an asymmetric silicon cyanation reaction; therefore, the catalyst can be recycled with a yield of 100% and ee value of 99%; and the chiral MOFs material has good application prospect in the aspects of synthesis of pure enantiomer compounds, synthesis of medical intermediates and the like. The material can be recycled after proper treatment.

These disclosures relate to preparing nickel metal (Ni(0)) suited for use in catalyst systems, such as nickel complexes with phosphorus-containing ligands, useful to catalyze the hydrocyanation of ethylenically unsaturated compounds. The methods described herein can include use of steam during reduction of nickel.

The invention discloses a diamine monomer containing a carbazole structure and having a high planarity, a synthetic method and an application thereof. In the method, the diamine is directly prepared from dihalogenated carbazole through ammoniation by liquid ammonia; or is directly prepared through a Suzuki reaction; or is directly prepared by performing cyanidation, hydrolysis and acylating chlorination to the dihalogenated carbazole to synthesize diacyl chlorocarbazole and then performing a reaction to the diacyl chlorocarbazole with a hydroxyl group or an amino group to form an ester bond or an amido bond; or is prepared by performing a Ullmann coupling reaction with the halogen atoms in the dihalogenated carbazole to form an ether bond, secondary amine or the like and finally reducing the dinitro group. The diamine synthetic process is simple, is simple in purification and is suitable for industrial production. A minimum energy state 3D molecular structure of the diamine monomer is high in planarity so that the diamine monomer can be used for preparing a high barrier polymer which is strong in interaction force among molecular chains and is small in free volume. The diamine monomer can be used for preparing high-performance and functionalized polyamides, polyimides, polyamideimides, polyesterimides and such polymers.

The invention provides a synthetic system of 3-cyanomethylbenzoic acid methyl ester and a method thereof. The system comprises an acylation reaction vessel used for preparation of m-Toluoyl chloride;a liquid chlorine feeding unit used for storing and conveying liquid chlorine; a chlorination reaction unit which is connected with the acylation reaction vessel and used as a chlorination reaction chamber of m-Toluoyl chloride; a micro-interface generator which is respectively connected with the liquid chlorine feeding unit and the chlorination reaction unit and used for receiving liquid chlorineconveyed by the liquid chlorine feeding unit, crushing the liquid chlorine into micro-droplets with the diameter being micron level and conveying the micro-droplets to the chlorination reaction unitafter the crushing; and an esterification and cyanation reaction unit which is connected with the chlorination reaction unit. In the prior art, m-Toluoyl chloride and liquid chlorine cannot be fully mixed when m-Toluoyl chloride and liquid chlorine react such that yield of 3-cyanomethylbenzoic acid methyl ester is reduced. The above problem is solved by the synthetic system and the method of the invention.

The invention belongs to the technical field of medicine, and relates to a method for synthesizing 2-(3-cyano-4-isobutoxy phenyl)-4-methyl-5-thiazole formic acid. The method comprises that: 4-hydroxyl cyanobenzene is used as a raw material, and subjected to iodination, hydrocarbylation and cyanation to obtain an intermediate of 4-isobutoxy-1,3-benzene dinitrile, the intermediate reacts with sodium bisulfide and anhydrous magnesium chloride to obtain a key intermediate of 3-cyano-4-isobutoxy phenyl thioformamide, and the 3-cyano group-4-isobutoxy phenyl thioformamide is subjected to cyclization and hydrolysis reaction to obtain the 2-(3-cyano-4-isobutoxy phenyl)-4-methyl-5-thiazole formic acid. The method has the advantages of easily obtained materials, simple and convenient operation, high yield, low cost and suitability for industrialized production.

The invention discloses a reinforced leaching method of fine-grained encapsulated gold, which comprises the following steps: adding cyanation slag, calcined pyrite, pyrite cinder, auriferous sulfide ore roasted product or any other auriferous material, a gold leaching agent, a pH regulator, an oxidizer, a dispersing agent and the like into a water-base solvent, carrying out ball milling leaching to obtain extra-fine ground leaching slurry, transferring the extra-fine ground leaching slurry into a high-pressure reaction kettle, supplementing the gold leaching agent, oxidizer and water-base solvent, introducing air or oxygen-enriched air, carrying out pressure leaching, filtering and separating to obtain an auriferous pregnant solution and leaching slag. The method is simple in and convenient to operate, and can implement high-efficiency leaching of the fine-grained encapsulated gold; the obtained pregnant solution can be subjected to the existing technique composed of activated carbon adsorption, desorption, electrolysis, zinc powder (wire) reduction and the like to recover gold; and the method has high applicability and obvious economic benefits.

The invention discloses a lead-zinc floating recycling method from gold ore cyanation tailings, which comprises the following steps: (1) predisposing: adding water in the cyanation tailings; stirring to form ore paste; adding active carbon, Y0 agent, FeSO4+ammonium persulphate in the ore paste; (2) asynchronous mixing-selecting: sending the predisposed ore paste to the floater group I to proceed first roughing separation; adding Y0 agent, limestone, butyl airpotato yam to float galena; sending the tailings in the first roughing separation to floater group II; adding Y0 agent, limestone, cupric sulfate, butyl airpotato yam to float zincblende; (3) recycling and purifying tailing water: adding chlorinated lime in the tailing water to decompose CN- less than 0.5 mg per L; recycling the tailing water.

The invention discloses a preparation method for a silver and graphene composite coating of a cyanide-free system. Due to the fact that common problems that cyanide silver plating pollution is serious, the human body will be harmed, and meanwhile a silver coating has some defects exist, the preparation method is characterized in that dispersed grapheme is added in the cyanide-free system, and composite plating is carried out on a copper substrate. The preparation method comprises the basic steps that (1) a substrate is subject to oil removing and polishing, and silver soaking treatment is carried out; (2) sodium thiosulfate, potassium metabisulfite and silver nitrate are prepared into silver plating liquid, graphene powder, a certain amount of deionized water and a certain number of dispersing agent are mixed to be added into the silver plating liquid, and ultrasonic dispersion is carried out; and (3) a silver plate serves as an anode, the substrate serves as a cathode, the silver plate and the substrate are placed into the silver plating liquid to be subject to electroplating, and the silver-graphene composite coating is obtained. Compared with the prior art, the method is simple in process, good in controllability and wide in application scope; and the prepared silver-graphene composite coating is good in resistance to high temperature oxidation, high in resistance to sulfur, high in mechanical property and high in resistance to corrosion.

The invention discloses a terpolymer containing polyester chain links and polycarbonate chain links and a synthetic method thereof. The synthetic method comprises the following steps: mixing zinc-cobalt double metal cyanide complex catalyst, cyclohexene oxide and dicarboxylic anhydride in a solvent, introducing CO2 under the temperature of 30 to 150 DEG C till the pressure of CO2 is 0.5 to 10.0MPa, carrying out copolyreaction for 0.5 to 48 hours so as to obtain a crude product, and preparing the terpolymer which contains polyester chain links and polycarbonate chain links and has excellent thermal property and easy decomposition after purification. The molar percentage content of the polyester chain links, the polycarbonate chain links and polyether chain links of the terpolymer containing polyester chain links and polycarbonate chain links in the main chain are respectively 5 to 70 percent, 23 to 90 percent and 0.5 to 7 percent.

The invention relates to a method and equipment for production of adiponitrile from adipic acid, and mainly solves the problem of unstable product quality in the prior art for production of adiponitrile from adipic acid. The method employs materials of fusing adipic acid, ammonia, phosphate and a diluent. The production method is as below: mixing phosphoric acid with the diluent in a pipeline mixer; conducting neutralization of adipic acid and ammonia in a cyanation reactor; sending reaction products into the bottom of a separation tower for separation; recovering gas phase of light components from an outlet; sending the diluent recovered by a gas lifting plate into the pipeline mixer, mixing the diluent with phosphoric acid in the pipeline mixer, and sending the mixture into the cyanation reactor to dilute adipic acid; and sending a liquid phase to a scraper type evaporator. The employed equipment includes an adipic acid storage tank, an ammonia compressor, a cyanation reactor, a pipeline mixer, a separation tower, a tail gas removal tower, a phosphoric acid storage tank and a scraper type evaporator. The invention has the advantage of a good quality of the produced adiponitrile product.

The invention relates to a preparation method of a fluorescent molecular probe for detecting fluoride ions in aqueous solutions through fluorescence enhancement and an application of the fluorescent molecular probe to detecting fluoride ions. The fluorescent molecular probe is prepared by protecting 1,4-diethyl-1,2,3,4-tetrahydro-7-hydroxyquinoxaline-6-aldehyde taken as a raw material with silane and then condensing the raw material and malononitrile. The fluorescent molecular probe is simple and convenient to synthesize, and reaction conditions are mild. The fluorescent molecular probe has the specific characteristics that the probe molecule has stable optical properties and higher synthetic yield; the probe molecule has high sensitivity of detection of fluoride ions in the aqueous solutions and low lower limit of detection, and the limit of detection is 5.4mu M; the response range is 0-1mM and the detection range is wide; the probe molecule has good selectivity and has no responses to anions, such as chloride ions, bromide ions, iodide ions, tetrabutylammonium cyanide, nitrates radicals, hydrosulfate radicals, perchlorate radicals, acetate radicals, thiocyanate radicals, azide radicals, cysteine, bovine serum albumin, carbonate radicals, sulfate radicals and reduced glutathione; the fluorescent molecular probe has practical application values in the fields of biochemistry, environmental sciences and the like.

The invention discloses a synthetic process of berberine. The synthetic process comprises the following synthetic route: pyrocatechol and dichloromethane are taken as raw materials and dimethyl sulphoxide is taken as a solvent to synthesize 1,3-benzodioxole; 1,3-benzodioxole is subjected to ViLsmeiar formylation to synthesize heliotropin; heliotropin undergoes nitration through a Henry reaction to generate beta-nitro-3,4-dioxomethenyl styrene; beta-nitro-3,4-dioxomethenyl styrene is subjected to Clemmensen reduction to generate 3,4-(methylenedioxyphenyl)ethylamine; and 3,4-(methylenedioxyphenyl)ethylamine and 2,3-dimethoxy benzaldehyde condense, and the obtained product is reduced to generate N-2,3-dimethoxybenzyl [3,4-(methylenedioxy)phenyl]ethylamine hydrochloride. N-2,3-dimethoxybenzyl [3,4-(methylenedioxy)phenyl]ethylamine hydrochloride is cyclized in a condition of glyoxal, formic acid and copper sulphate to generate berberine hydrochloride. According to the synthetic route, cyanation is avoided and toxicity is reduced. Zinc amalgam is adopted to replace H2Ni and LiAlH4, so that the cost is greatly reduced, the process difficulty is reduced, and the product yield is increased.

The invention relates to a method for preparing progesterone. According to the method, 4-androstenedione is used as raw materials, and hydroxyl cyanation, dehydration, protection, hydrogenation and addition hydrolysis reaction are carried out in sequence, and the progesterone is obtained. The 4-androstenedione which has the price advantage is used as the raw materials, the reaction condition is easy to control, post-processing is easy, and yield is high.

The invention relates to steel band continuous copper plating VI which adopts a cyanation copper plating technique to perform electroplating. The steel band continuous copper plating VI mainly comprises a pretreatment process and a copper electroplating process, wherein the pretreatment process mainly comprises the steps of ultrasonic oil removal, electrolytic oil removal, water washing, activating, water washing and the like; and the electroplating process mainly comprises the steps of copper plating, recycling, water washing and the like. A technical tank in the steel band continuous copper plating adopts a closed transparent simultaneous-gas-discharge isosceles trapezoid tank with openable view windows, wherein the upper part of the tank body is designed as an isosceles trapezoid; three transparent automatic-opening view windows are respectively designed at two slope parts of the tank; a plating solution in the plating tank in steel band continuous copper plating is circulated and filtered by double mother tanks; a pretreatment waste liquid and an electroplating waste liquid in the steel band continuous copper plating are circulated and filtered by three mother tanks, and sodium carbonate is treated on line; a funnel and a filter screen are arranged below a conducting roller for steel band continuous copper plating, and the residual plating solution on the steel band is recovered in an atomization spray mode; and a steel band outlet end of the steel band continuous copper plating is provided with a vacant tank which is about 100mm long, and the residual plating solution on the steel band is recovered in an atomization spray mode.

The invention discloses a preparation method for long carbon chain nylon PA1313. The preparation method comprises the following steps: taking 1,13-tridecanedioic acid as a raw material; preparing 1,13-tridecylamine through cyanation and amination; preparing PA1313 salt by taking 1,13-tridecylamine and 1,13-tridecanedioic acid as raw materials and water as a solvent; putting PA1313 salt and water at a certain ratio into a polymerizing kettle; performing melt polymerization, thereby acquiring PA1313 with a certain molecular weight. In the cyanation step of the method, an ammonia gas recycling technique is adopted, so that the use ratio of ammonia gas is greatly increased and the emission of wastewater and exhaust gas is reduced; in the salt forming and polymerizing process, water is used forreplacing ethyl alcohol as a reaction medium, so that the safety of industrial production is promoted, the safety level of equipment is reduced, the investment in equipment is reduced and the recycling cost of solvent is lowered.

The invention relates to a preparation method of adiponitrile. The preparation method comprises the following steps: firstly performing a reaction on adipic acid and ammonia at 155-200 DEG C to produce diammonium adipate, and then dehydrating under a catalytic reaction of phosphoric acid or ammonium phosphate to produce adiponitrile; a product can be further separated in a separation tower. The reaction is performed on the adipic acid and the ammonia gas at the low temperature of 155-200 DEG C to produce H4NOOC(CH2)4COONH4 first, and then high-temperature cyanation is performed, so that the opportunity of producing a by-product and a coke from the adipic acid at high temperature is effectively avoided, not only the yield is increased by 3-5%, but also the operation cycle of a production device is prolonged by 30-60 days, and the production per unit time is increased. Liquid phosphoric acid is used as a catalyst, firstly ammonium salt of the phosphoric acid is produced, and the ammoniumphosphate can be mixed with ammonium salt of the adipic acid very well, so that the catalytic performance is improved better and the selectivity of the adiponitrile is increased by more than 2%.

The invention discloses a method for synthesizing apalutamide. The method includes carrying out condensation on N-methyl-2-fluorine-4-halogenated-benzamide compounds 1 and amino-1-cyclobutanecarboxylic acid hydrochloride 2 by means of Ullmann reaction to obtain to obtain intermediate compounds 3 and esterifying the intermediate compounds 3 to obtain intermediate compounds 4; carrying out cyclization by means of reaction on the intermediate compounds 4 and thiocyanide to obtain compounds 5; carrying out condensation by means of coupling the compounds 5 to obtain the apalutamide. The N-methyl-2-fluorine-4-halogenated-benzamide compounds 1 and the amino-1-cyclobutanecarboxylic acid hydrochloride 2 are used as starting materials. A path is shown, an R in the path represents alkyl, includes butis not limited to methyl or ethyl. The method has the advantages that route steps can be shortened to a great extent, the route efficiency can be improved, precious metal catalysts are omitted, and accordingly the process cost can be lowered; byproduct generation can be reduced, and accordingly the method is favorable for improving the purity of ultimate products.

The invention relates to the field of organic synthesis, in particular to a topramezone intermediate and a topramezone preparation method. The topramezone preparation method comprises the following steps: 3-[3-halogen-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole and cyanide are subjected to a substitution reaction to obtain 3-[3-cyano-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole; hydrolysis reaction is performed on 3-[3-cyano-2-methyl-6-(methylsulfonyl)phenyl]-4, 5-dihydroisoxazole under the action of acid or alkali to obtain 2-methyl-3-(4, 5-dihydroisoxazole-3-yl)-4-methylsulfonyl benzoic acid; and 2-methyl-3-(4, 5-dihydroisoxazole-3-yl)-4-methylsulfonyl benzoic acid and 1-methyl-5-hydroxypyrazole are condensed and rearranged to generate topramezone. According to the topramezone intermediate and the topramezone preparation method provided by the invention, the use of an expensive palladium catalyst and a dangerous butyl lithium reagent is avoided, the yield isrelatively high, the cost is reduced, the process is simplified, the defects in the prior art are overcome, and the industrial value is achieved.

The invention discloses a method for enriching platinum and palladium from a pressurized cyanating solution, and belongs to a process for extracting platinum and palladium from a basic cyanating solution. The method comprises the steps as follows: enriching [Pt(CN)4]2- and [Pd(CN)4]2- from the pressurized cyanating solution of a platine group metal concentrate by cocoanut active charcoal; using a basic ethanol solution as a stripping solution for stripping the [Pt(CN)4]2- and the [Pd(CN)4]2- adsorbed on the surface of the cocoanut active charcoal; adsorbing and stripping for multiple times; burning the cocoanut active charcoal free of adsorption capacity; dissolving by acid; recovering platinum and palladium; and combining with platinum and palladium in the stripping solution. The method is easy and convenient to operate; the cocoanut active charcoal can be purchased in the market and is repeatedly utilized when in use; and the recovery rates of platinum and palladium are larger than 99%.