259results about How to "The reaction conditions are mild and easy to control" patented technology

The invention relates to a novel method for modifying the surface of a polysulfone ultrafiltration membrane, used for improving the pollution resistance of a separation membrane. In the invention, by using polysulfone as a surface modification basement membrane, a living radical is generated on the membrane surface with an ultraviolet initiator or a thermal initiator to further graft a hydrophilic monomer on the surface of the membrane, thereby finishing grafting modification to a polysulfone ultrafiltration membrane. The method is convenient to operate, efficiently inhibits generation of polysulfone main chain fracture and also keeps the interception performance of the ultrafiltration membrane. In the prepared ultrafiltration membrane, the hydrophilicity is obviously improved, and the pollution resistance is remarkably enhanced.

The invention provides a preparation method of a phenolic resin matrix nano activated carbon fiber material. The preparation method is characterized in that the method specifically comprises the steps of: dissolving benzoxazine monomers and curing catalysts in solvent, adding blending polymers for electrostatic spinning, putting the obtained benzoxazine composite nano fiber membrane in a drying oven for curing, placing the cured benzoxazine composite nano fiber membrane in potassium hydroxide solution for soaking, taking out the benzoxazine composite nano fiber membrane and drying the benzoxazine composite nano fiber membrane in a drying oven to obtain the pretreated benzoxazine composite nano fiber membrane; and placing the pretreated benzoxazine composite nano fiber membrane in a vacuum tube furnace, heating for carbonization under the protection of nitrogen, cooling to room temperature after the carbonization process is ended, acidizing and drying to obtain the phenolic resin matrix nano activated carbon fiber material. The preparation method has a wide application prospect in fields such as activated adsorption, high-temperature catalysis, energy storage and hydrogen storage.

The invention relates to the medicine chemical synthesis field, and especially discloses a preparation method of a Ticagrelor intermediate. The preparation method comprises the following steps: 1) taking 3,4-difluorobenzaldehyde (I) as an initial raw material, reacting with a phosphorus ylide material liquid to obtain (E)-3-(3,4-difluorophenyl)-2-acrylic acid ester (II); 2) performing a Simons-Smith asymmetric cyproteronethe reaction on the (E)-3-(3,4-difluorophenyl)-2-acrylic acid ester (II) to obtain trans-(1R,2R)-2-(3,4-difluorophenyl) cyclopropanecarboxylic acid ester (III); 3) performing aminolysis on the trans-(1R,2R)-2-(3,4-difluorophenyl) cyclopropanecarboxylic acid ester to obtain trans-(1R,2R)-2-(3,4-difluorophenyl)cyclopropanecarboxamide (IV); and 4) performing a Huffman rearrangement reaction on the trans-(1R,2R)-2-(3,4-difluorophenyl)cyclopropanecarboxamide (IV) to obatain the Ticagrelor intermediate (V). The method of the invention has the advantages of simple process, convenient operation, mild reaction condition and easy control, low cost and easy acquisition of raw material, high product yield and product purity, and is adapted to large scale industrial production.

The invention relates to a polymerization method of an (ammonium) sulfate connexon polymer. The polymerization method comprises a step of subjecting a hydroxyl-containing monomer or an amino-containing monomer and a sulfuryl fluoride monomer to condensation polymerization on through a one-pot process under alkaline conditions. Compared with a traditional polyester synthesis method, the method is cost-saving; reaction conditions are mild and easy to control; reaction flow is simple, and operation is easy; and a post-treatment process is simple, environmental pollution is small, and industrial production is facilitated. In addition, a bisphenol type polysulfate compound synthesized in the invention has excellent mechanical properties, dielectric properties, tolerance and wear resistance.

The invention relates to a method for preparing isopentenol from 3-methyl-3-butenol, which performs isomerization reaction on a raw material of 3-methyl-3-butenol to generate the isopentenol in the presence of a catalyst in an atmosphere containing hydrogen, wherein the reaction pressure is normal pressure, the reaction temperature is between 50 and 90 DEG C, the reaction time is between 25 and 40 minutes, the catalyst uses Al2O3 as a carrier, a load active component is metal Pd, the content of the Pd in the catalyst in percentage by weight is between 0.1 and 2.0 percent, the particle size of the catalyst is between 80 and 200 meshes, and the weight ratio of the raw material to the catalyst is 30-100:1. Compared with the prior art, the method has obvious improvement, the catalyst is simpler, and the content of the active component is lower, thus the preparation is easier and the cost is lower; the reaction condition is mild; and on the premise of ensuring the selectivity and the product yield of a perfect product, the reaction time is greatly shortened. The reduction of the preparation cost of the catalyst and shortening of the reaction time finally reduce the overall production cost greatly.

The invention provides a method for preparing a magnetic benzoxazinyl carbon nanofiber material. The method is characterized by comprising the following specific steps of: dissolving a benzoxazinyl monomer and a solid catalyst in a solvent to obtain a benzoxazinyl solution; adding a blending polymer and an iron-containing compound; carrying out electrostatic spinning and solidification treatment, placing the solidified benzoxazinyl composite nanometer fiber membrane in a potassium hydroxide solution to soak, taking out the solid benzoxazinyl composite nanometer fiber membrane and drying in a vacuum drying box to obtain a pretreated solid benzoxazinyl composite nanometer fiber membrane; placing the pretreated solid benzoxazinyl composite nanometer fiber membrane in a vacuum tube type furnace, heating to carry out carbonization treatment under the protection of nitrogen, cooling down to room temperature after finishing a carbonization process, carrying out acidizing treatment, and drying in the vacuum drying box, thereby obtaining the magnetic benzoxazinyl carbon nanofiber material. According to the method for preparing the magnetic benzoxazinyl carbon nanofiber material, magnetism is endowed to the material based on excellent performances of a carbon fiber so that the method has wider application prospect in the fields, such as solvent recovery, water treatment, gasoline trapping and the like.

The invention discloses a preparation method of moxifloxacin hydrochloride, comprising the steps of: reacting the 1-cyclopropyl-6,7-difluoro-8-methoxy-4-oxo-1,4-dihydro-3-quinoline carboxylic acid and the S,S-2,8-diazabicyclo[4.3.0]nonane to prepare the moxifloxacin in the presence of organic base in organic solvent under the reaction temperature of 60 to 85 DEG C; separating the moxifloxacin, processing the moxifloxacin by concentrated hydrochloric acid in organic solvent under the reaction temperature of 60 to 85 DEG C to obtain the moxifloxacin hydrochloride.

The invention belongs to the nano titanium dioxide catalyst technical field, concretely relates to a bismuth and silicon doped nano titanium dioxide photocatalyst, its preparation and its application. The doping amount of bismuth in the catalyst by mole fraction is 0.2-1.1%, the doping amount of silicon is 4.8-15.6%. The bismuth and silicon doped nano titanium dioxide photocatalyst has the advantages of pure crystalline phase, high specific surface, multiple surface acidity points, visible light response and organic pollutant adsorption. The catalyst of the invention can be rapidly degraded by using visible light and sunshine, so that the catalyst keeps high visible photodegradation efficiency and high photocatalytic activity.

The invention discloses a preparation method and an application of nano zinc oxide photocatalyst. The method takes zinc acetate dihydrate and diethylene glycol as raw materials and synthesizes the nano zinc oxide (ZnO) photocatalyst by hydrolysis in one step optionally under the presence of water. The method is short in synthetic route, mild in conditions and simple in operations. The prepared nano ZnO photocatalyst has good photocatalytic performance within the range of ultraviolet and visible wavelengths, and has good application prospects particularly in dye sewage treatment.

The invention discloses a citric acid and chitosan modified biocompatible polyurethane and a preparation method thereof. A main chain of the polyurethane disclosed by the invention is a polyurethane long chain, the two ends of the long chain are respectively an anticoagulative citric acid structure covalently grafted with the long chain, and a chitosan structure is selectively grafted on the citric acid structure. The preparation method comprises the following steps: firstly, adding isocyanate, polyethylene glycol and a catalyst into a reactor, and carrying out stirring reaction for 2-5 h in the presence of nitrogen; then, adding a citric acid, and heating for reacting for 12-18 h, so that a citric acid modified polyurethane is obtained; and activating the citric acid modified polyurethane by using carbodiimide, and soaking the obtained object into a chitosan-acetic acid solution to carry out acid-amide condensation reaction, so that the modified biocompatible polyurethane is obtained. According to the citric acid and chitosan modified biocompatible polyurethane disclosed by the invention, the citric acid structures with biocompatibility and the chitosan structure are covalently bonded in the polyurethane long chain, so that the polyurethane has good chemical stability and biocompatibility, and can be used as a biomedical material; and the preparation method has the advantages of simple and easily-controlled process, low cost, and the like.

The invention discloses a method for preparing ticagrelor intermediate trans-(1R,2S)-2-(3,4-difluorophenyl) cyclopropylamine (intermediate B). The method comprises the following steps of: carrying out condensation reaction between 3,4-difluorobenzaldehyde and nitromethane to obtain trans-beta-(3,4-difluorobenzene)nitroethylene (II); carrying ou cyclopropanation reaction of the compound (II), with zinc iodide and diethyl zinc under catalytic action of chiral ligand, thus generating trans-2-(3,4-difluorophenyl)nitrocyclopropylamine (III), and finally, carrying out nitroreduction reaction of the compound (III), thus obtaining the intermediate B. The preparation method provided by the invention is simple and convenient, economical and environment-friendly, and advantageous for industrial production of the drug; besides, the preparation method is also capable of promoting the development of the economic technology of the crude drug.

The invention discloses a method for preparing magnesium hydroxide utilizing light-burned dolomite powder. The method comprises the following steps: adding the light-burned dolomite powder to enough water for digestion; introducing a carbon dioxide gas to obtained light-burned dolomite emulsion until the pH value of the reaction product is 6.7-7.0, and filtering the product; adding absolute ethanol to filtrate, heating and controlling the temperature to 50-80 DEG C, and after reaction, filtering, wherein the amount of absolute ethanol is controlled to be 30-40% of the volume of the filtrate; adding hydrochloric acid to obtained solid magnesium bicarbonate until bubbles disappear; adding a base liquid to an obtained magnesium chloride solution; and adding polyvinylpyrrolidone or ethylenediamine to obtained magnesium hydroxide slurry, wherein the amount of polyvinylpyrrolidone or ethylenediamine is equal to 2-6% the volume of the slurry; and then adding the slurry into an autoclave, controlling the temperature at 80-200 DEG C and stirring under constant temperature condition for 10-20 hours. Magnesium hydroxide precipitate prepared by the method disclosed by the invention is in a fibrous or flaky crystal shape and has high purity; and the preparation method is simple to operate, and the reaction conditions are mild and easy to control.

The invention discloses a thiosemicarbazone 7-umbelliferone-8-aldehyde probe reagent which is prepared by enabling 7-hydroxyl-8-aldehyde coumarin and thiosemicarbazone to react. By adopting a probe disclosed by the invention, selective recognition of metal ions and anion can be achieved simultaneously, specific ions can be rapidly detected through visual colorimetric, the probe can be also applied to specific ion imaging detection in living cells, has double-mode detection with fluorescence enhancement and proportioning absorption, is relatively excellent in detection sensitivity and accuracy, has the advantages of high sensitivity, high selectivity, high yield and the like, and moreover is beneficial to quantitative and qualitative analysis on complex micro systems.

The invention provides a surface treatment method for improving adhesive performance of fluorine-containing resin film, and relates to the field of surface ultraviolet grafting for the fluorine-containing resin film. In the surface treatment method, reacting liquid containing monomers, photo initiators and solvent is uniformly coated on the surface of the fluorine-containing resin film by the coating quantity of 5-20g/m<2>, then the fluorine-containing resin film is subjected to surface modification under irradiation of an ultraviolet source for 20 seconds to 10 minutes, wherein the irradiation strength of the ultraviolet source is controlled within a scope of 4000-12000 microwatt per square centimeter by referring to the standard of the wavelength lambda equal to 254nm, and the monomers are mixtures of trimethylolpropane triacrylate and n-butyl acrylate. By the surface treatment method, the lamination adhesive performance of the fluorine-containing resin film and EVA (ethylene vinyl acetate) film can be improved, and accordingly problems of low peeling strength and poor durability after adhering of the fluorine-containing resin film and the EVA film are solved. The surface treatment method has a good modification effect to surfaces of the films only and cannot affect performance of the bodies of the films severely, and has the advantages of mild reaction condition, control easiness, simplicity and capability of realizing continuously industrial treatment.

The invention discloses a treatment method of organic waste water. In the treatment method, a supported catalyst made of carbonyl metal is used, so that the chemical oxygen demands (COD) of various high-concentration organic waste waters can be effectively reduced under the mild condition; and the catalyst is convenient for separation and can be recycled, reaction condition is mild, and the treatment method is easy to operate.

The invention discloses a method for preparing an intermediate prenyl-3-methylbutyl-2-alkenyl ester. The prior methods have high control requirement on the concentration of a phosphoric acid catalyst, which have large difficulty and poor stability, and are hard to carry out in production; and other methods have low yield and conversion ratio. The method has the following steps: feeding 3-methylbutyl-2-olefine aldehyde di-prenyl acetal from a reaction kettle; performing a catalytical elimination reaction in a gas-phase fixed-bed reactor after vaporization to obtain mixed gas; introducing the mixed gas into a rectification tower; recovering the mixture at the top of the rectification tower to obtain 3-methyl-2-butenol; and discharging the material from one side of the rectification tower to obtain the prenyl-3-methylbutyl-2-alkenyl ester, wherein the unreacted raw material 3-methylbutyl-2-olefine aldehyde di-prenyl acetal at the bottom of the rectification tower is refilled into the reaction kettle for vaporization and continuous reaction, and the reaction kettle is replenished with new raw materials continuously. The catalyst used in the method has smaller destructive effect, reduces the quantity of leftover materials after the elimination reaction, and has high selectivity.

The invention discloses a method for preparing a medical material, namely Alpha-keto-phenylalanine calcium. In the conventional methods, some methods are complicate in operation and has low yield, and oxydol is used in the oxidizing process, which is not favorable for safety production; and some methods have long reaction time, harsh conditions and low hydrolysis yield. The preparation method includes the following steps: glycine, benzaldehyde, acetic anhydride and organic base catalyst are taken as raw materials, and 4-benzal-2-methyl dihydride oxazolone is obtained by adopting one-pot method for catalytic cyclization reaction; and 4-benzal-2-methyl dihydride oxazolone and calcium hydroxide conduct ring-opening and hydrolysis reaction in a pressure kettle to obtain Alpha-keto-phenylalanine calcium. The cyclization reaction adopting the one-pot method has low equipment investment and operating cost; organic amine catalyst is easy for reclamation and indiscriminate use; no waste water generates; and the hydrolysis reaction adopting pressurizing reaction has low possibility of side reaction, and the reaction conditions are mild and are easy to control, so that the reaction yield is improved.

The invention discloses a lenvatinib synthesizing method.The method includes the steps that 4-amino-3-chlorophenol and benzyl chloroformate are subjected to amidation reaction, the obtained 4-(carbobenzoxy)amino-3-chlorophenol and 4-chlorine-7-methoxyquinoline-6-formamide are subjected to condensation reaction, the obtained 4-[3-chlorine-4-(carbobenzoxy)aminophenoxy]-7-methoxyquinoline-6-formamide and cyclopropylamine are subjected to amidation reaction, and the finished product lenvatinib is obtained.The method is short in process route step, operation is simplified, cost is low, and the method is environmentally friendly and suitable for industrial production.

The invention belongs to the technical field of nano composite materials, and discloses a preparation method and application of a 1D Sb2S3 nanorod/3D ZnIn2S4 composite structure. The method is as follows: firstly hydrothermally synthesizing 1D Sb2S3 nanorods, then dispersing the 1D Sb2S3 nanorods into deionized water to form a suspension, and finally, using in-situ hydrothermal method to prepare the 1D Sb2S3 nanorod/3D ZnIn2S4 composite structure. The composite structure prepared by the method can be applied to catalytically degrade 2-thiol benzothiazole under visible light or decompose waterto produce hydrogen under sunlight. The method has rich raw materials, simple operation process and mild reaction conditions, and belongs to a green synthesis method. The 1D Sb2S3 nanorods are combined with 3D ZnIn2S4 nanostructures to make full use of the in-situ growth characteristics, and close contact between the 1D Sb2S3 nanorods and the 3D ZnIn2S4 nanostructures is formed to achieve efficient transmission and separation of photogenerated electrons, improve the electron transport capability in the composite, and broaden the light absorption range of a single photocatalyst, so that the overall photocatalytic activity is enhanced, and the 1D Sb2S3 nanorod/3D ZnIn2S4 composite structure has important and broad application prospects in environmental management and energy conversion.

The invention discloses a high-strength and wear-resisting liteglow glass product and a preparation method thereof. The glass product is prepared from the following components: silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, graphene, titanium dioxide, diboron trioxide, sodium silicate, potassium oxide, antimony oxide, arsenic oxide and noctilucent powder. The preparation method comprises the following steps: firstly, carrying out mixed melting on all the components to obtain a molten mass; secondly, raising the temperature of the molten mass to 1400 to 1500DEG C and performing thermal insulation for 12 to 14 hours; thirdly, feeding a glass molten mass into a forming machine to obtain glass products with different shapes and sizes; fourthly, carrying out annealing treatment on the glass products to obtain a finished product. The glass product prepared by the preparation method disclosed by the invention has better strength and wear resistance; the fragile degree of the product can be greatly reduced, the service life of the product is prolonged, and the use cost of the product is reduced.

The invention discloses a polysiloxane organo-phosphines toxic sensitive material, which regards polysiloxane as the skeleton and is an organic material with oxybenzene as the functional group. The process for preparation comprises the following procedures: (1) charging hydrogenous silicon oil and platinum catalyst in toluene, mixing uniformly; (2) dropping allyl phenol in the mixed solution of the procedure (1) slowly; (3) heating and reacting, heating the mixed solution of procedure (2) to 80-120 DEG C and mixing 2-6 hours in the temperature; (4) filtering, filtering the reacting liquid of the procedure (3) with activated carbon in order to remove the platinum complex charged in the procedure (1); (5) evaporating, removing toluene of the filtering liquid of the procedure (4) with vacuum distillation. The material responses quickly for the organo-phosphines toxic, and has good selectivity and reversibility, reduces the toxic owing to the material and the intermediate product without halogen, which has simple preparing method, mild and easy control reaction condition, easy operation, few reaction procedures and low cost, and is a nerve toxic sensitive material with good appliance future.