31results about How to "Reduced overall reaction time" patented technology

The invention relates to a 11-alpha hydroxylation reaction preparation method of a steride hormone substance important intermediate. The reaction preparation method comprises the following steps of: inputting a steride substrate I into a fermentation medium containing mold seeds to ferment, carrying out the hydroxylation reaction under the effect of the mold and a catalyst, and modifying 11 sites and 21 sites of the steride substrate I to obtain the steride hormone substance important intermediate II with 11-alpha-hydroxy and 21 hydroxy. According to the reaction preparation method, a borate catalyst is used, so that the reaction speed is improved, the reaction time is saved, the consumption of air in a fermentation process is reduced, and simultaneously, the conversion rate is improved by about 5%; and the synthetic medium is used for replacing a natural medium, so that the cost is reduced, and the section pressure of subsequent separation is relieved.

The invention discloses a production device and a production method of liquid sodium dimethyl dithiocarbamate. The production device comprises a reaction kettle, wherein the upper part of the reaction kettle is respectively communicated with a dimethylamine head tank, a sulfur dioxide head tank and a sodium hydroxide head tank by pipelines; the lower part of the reaction kettle is connected with a reaction kettle dump valve; and the reaction kettle dump valve is sequentially communicated with a filter, a finished product allocation tank and a finished product storage tank sequentially by pipelines. The production method comprises the following steps of: measuring carbon bisulfide, a 30% sodium hydroxide solution and 40% dimethylamine at a mass ratio, placing a dimethylamine solution into the reaction kettle, mixing, supplying a cooling medium to a reaction kettle jacket and an internal cooling coil tube, pressing carbon bisulfide into a synthetic kettle when the temperature of the kettle drops to 10-20 DEG C, then pressing the 30% sodium hydroxide solution into the synthetic kettle, slowly opening a synthetic kettle dump valve, and pressing a material in the reaction kettle into the filter and then into the finished product allocation tank.

The invention discloses a growing method of nanometer carbon pipe, which comprises the following steps: providing base; preparing nanometer catalyst solution with certain viscosity; dripping nanometer catalyst solution on the base surface through injecting device of micrometer-grade injecting needle array; forming catalyst layer; growing nanometer carbon pipe on the base surface; making catalyst drip as micrometer grade.

The invention discloses a preparation technology of aluminum nitride. The preparation technology comprises the following two stages of 1, using aluminum oxide and carbon as raw materials, performing carbon thermal reduction reaction under the vacuum and high temperature conditions, and forming a solid product mainly containing aluminum carbide and aluminum oxycarbide; 2, using the product in the stage 1 as a raw material, grinding, putting into a carbon crucible or mixing with a small amount of carbon raw material, and performing high-temperature nitridation reaction under the nitrogen atmosphere, so as to obtain the aluminum nitride. The preparation technology has the advantages that the required temperature is lower, the reaction time is shorter, the carbon content in the obtained aluminum nitride powder is low, and the subsequent carbon step can be shortened or avoided; besides carbon monoxide, the other waste gases are not produced; the industrializing is easily realized.

The invention relates to a method for synthesizing a persantine intermediate 2,4,6,8-tetrahydroxy pyrimido[5,4-d] pyrimidine, comprising the following steps of: (1) adding nitro orotic acid in an alkali liquid, then hydrogenating with Ni / H2, and filtering to obtain an amino orotic acid solution which is directly used for next reaction without separation; (2) adjusting pH of the amino orotic acid solution with concentrated hydrochloric acid to 3, adding sodium cyanate for temperature control reaction to obtain the urea derivatives of the amino orotic acid; then dropping a 30% sodium hydroxide solution to adjust pH to 13, heating for cyclization, dropping a 50-60% sulfuric acid solution to adjust pH to 3; (3) cooling to room temperature, filtering, washing to neutrality and drying to obtainthe product. The intermediate of step (1) is not needed to separate, thereby saving a lot of time and labor, reducing about 50% of total reaction time with mild reaction condition and maximum reaction temperature reduced to 95 DEG C so that the device is less required and more durable.

The invention discloses a growing method of nanometer carbon pipe, which comprises the following steps: providing base; preparing nanometer catalyst solution with certain viscosity; dripping nanometer catalyst solution on the base surface through injecting device of micrometer-grade injecting needle array; forming catalyst layer; growing nanometer carbon pipe on the base surface; making catalyst drip as micrometer grade.

The invention discloses a synthetic method for 2-formamide cyclohexanone with low emission and low consumption, and belongs to the technical field of medicinal chemistry and organic synthesis. According to the method, a non-oxide proton acid or salt thereof is used as a catalyst, arene is used as a solvent and a water-carrying agent, and cyclohexanone and urea are used as raw materials, so that the 2-formamide cyclohexanone can be prepared through a one-pot reaction. The screw ring synthetized through the technology provided by the invention is not needed to be cooled and separated, so that a great amount of scouring water is eliminated; besides, condensation generated water saturated by cyclohexanone, evaporated water generated during the screw ring hydrolysis and aqueous phase mother solution generated after the product is separated out are used for preparing hydrolyzing diluted acid to realize cyclic utilization, so that the loss caused by the cyclohexanone dissolution in water is eliminated, the use ratio of cyclohexanone is increased and the zero release of sewage is realized; the method is simple and convenient to operate and is suitable for industrial application.

The invention provides a bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation device and method. The bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation device comprises a feeding kettle, a diaphragm pump, a reaction kettle, a filter press, a distillation still and a vacuum pump. The feeding kettle, the diaphragm pump, the reaction kettle, the filter press, the distillation still and the vacuum pump are sequentially connected. The bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation method includes the following steps of inflation, feeding, pressurizing, mixing, reacting, heat preserving, discharging, and decompressing and drying. The bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation device and method solve the technical problems that a bis(2,4,5-trichloro-6-carbopentoxyphenyl)oxalate preparation method in the prior art is slow in reaction and low in yield.

The invention provides a method for preparing bleeding stopping oxidized celluloses in ramie oxidation degumming procedures. The method includes smashing raw ramie to obtain short fibers and soaking the short fibers to sufficiently moisten the short fibers and allow the short fibers to sufficiently swell; mixing the pretreated raw ramie short fibers and degumming solution with one another to obtain mixtures, heating the mixtures, then preserving heat, sufficiently removing colloid in the raw ramie by the aid of oxidability of specific oxidizing agents and simultaneously oxidizing celluloses with active hydroxyl to obtain oxidized celluloses with a large quantity of carboxyl; soaking oxidized and treated fibers by the aid of organic solvent aqueous solution and removing the unreacted oxidizing agents; separating the oxidized celluloses from water and carrying out drying treatment on the oxidized celluloses to ultimately obtain the powdery bleeding stopping oxidized celluloses. The method has the advantages that processes are simple, the original two working procedures are combined into a single working procedure, accordingly, the total reaction time can be shortened, medicines and the cost can be saved, and the efficiency can be greatly improved; the bleeding stopping oxidized celluloses which are products prepared by the aid of the method are high in bleeding stopping speed and bleeding stopping efficiency and can be widely applied to quickly stopping bleeding under conditions of war wound, trauma and the like, and stable effects can be realized.

The invention discloses a production process of diethylenetriaminepentamethylenephosphonic acid. The specific operation steps include: (1) Add the measured hydrochloric acid, diethylenetriamine and phosphorous acid into the reaction kettle in sequence, and the reaction kettle is continuously stirred to keep the temperature ≤ 50°C; (2) Raise the temperature to a certain temperature, and add dropwise at different flow rates Part of the formaldehyde solution, after the dropwise addition, keep warm, concentrate; (3) add hydrochloric acid and raise the temperature to 110~120°C, add the remaining formaldehyde solution dropwise, after the dropwise addition, keep warm for reaction, steam externally, dilute, cool down, adjust Sour qualified finished product. The invention accelerates the reaction rate, not only effectively suppresses the production of the by-product hydroxymethylphosphonic acid, improves the conversion rate and product yield of the effective active component diethylenetriaminepentamethylenephosphonic acid, but also shortens the total reaction time. time, reducing production costs. The process method is simple, safe and easy to operate, and is beneficial to industrialized production.

The present invention provides the synthetic method of 1,3-dinitrohalobenzene compound, comprises the following steps: A) halobenzene compound, and the mixed acid of nitric acid, sulfuric acid, carry out the first nitration reaction in one-stage continuous flow microreactor , through oil-water separation, to obtain a nitrohalobenzene compound and the first waste acid; B) diverting the mononitrohalobenzene compound into the secondary continuous flow microreactor, and carrying out the second nitration reaction with the mixed acid of nitric acid and sulfuric acid , the nitration mixture generated is quenched and filtered at the outlet of the secondary continuous flow microreactor to obtain 1,3-dinitrohalobenzene compound and the second waste acid; C) the second waste acid is recycled to the first-level continuous flow In the microreactor, carry out the third nitration reaction with the halobenzene compound, and separate the oil and water to obtain the mononitrohalobenzene compound and the third waste acid; repeat steps B), C); the halobenzene compound has the formula I structure. Short reaction time and less waste acid realize continuous production.

The invention provides a preparation method of an Avanafil intermediate. The preparation method comprises the following steps: dissolving 4-hydroxy-2-methylthio-ethyl 5-pyrimidinecarboxylate and potassium carbonate in DMF to obtain a mixed solution, adding methanesulfonyl chloride into the mixed solution under the stirring condition, continuously stirring after addition until a reaction is ended, adding water and ethyl acetate into a reaction solution, carrying out extraction and liquid separation, carrying out vacuum concentration on an organic phase to prepare 4-methanesulfonic sulfonic ester-2-methylthio-ethyl 5-pyrimidinecarboxylate; dissolving the obtained 4-methanesulfonic sulfonic ester-2-methylthio-ethyl 5-pyrimidinecarboxylate into DMF, adding a (3-chloro-4-methoxy)Benzylamine hydrochloride to obtain mixed liquor, adding triethylamine into the mixed liquor under the stirring condition, continuously stirring after addition until a reaction is ended, adding water and ethyl acetate, carrying out extraction and liquid separation, carrying out vacuum concentration on an organic phase, and recrystallizing to prepare 4-(3-chloro-4-methoxybenzylamino)-5- ethyloxycarbonyl-2-methylthiopyrimidine. The invention has advantages of less environmental pollution, high product yield, safe post-processing and simple operation.

The invention discloses a treatment method of selenium-containing wastewater. The treatment method comprises the following steps: regulating the pH of the selenium-containing wastewater to 8-10, and carrying out ozonation in an ozone reactor to oxidize a selenite ion (SeO3<2->) into a selenate radical ion (SeO4<2->); carrying out aerobic biological treatment, regulating the pH to 3-5, and carrying out chitosan (CTS) adsorption; finally feeding the product into a flocculation sedimentation tank, adding a flocculant, stirring, and carrying out solid-liquid separation, so as to obtain wastewater without selenium. The treatment method has the beneficial effects that the removal rate of the selenium in the wastewater is high, the application range is wide, and the operation is easy and convenient.