94results about How to "Fewer post-processing steps" patented technology

The invention relates to a method for synthesizing adefovir dipivoxil intermediate, namely 9-[2-(diethylphosphono methoxyl)ethyl]adenine. The synthesis method comprises the following steps: (1) under the condition of alkali catalysis, adding ethylene carbonate and adenine into a solvent to perform reaction until the reaction is complete; (2) adding p-benzenesulfonyloxymethyl phosphoric acid diethylester and alkali into reaction liquid obtained in step (1) to perform reaction until the reaction is complete; and (3) performing post treatment on reaction liquid obtained in step (2) to obtain the 9-[2-(diethylphosphono methoxyl)ethyl]adenine. The synthesis method has few reaction steps, simplified operation, easy amplification and environmental protection, improves yield and greatly reduces cost.

The invention relates to the technical field of hydrofluoroester production and particularly relates to a clean production method for hydrofluoroester. The method is as follows: adding fluorine-containing sodium alkoxide catalyst into fluorine-containing alcohol liquor, adding fluorinated olefin, heating and stirring for reacting to obtain mixed liquor; carrying out after-treatment onto the mixed liquor to obtain hydrofluoroester, wherein the fluorine-containing sodium alkoxide catalyst is sodium trifluoroalkoxide, and the corresponding fluorine-containing alcohol is trifluoroalcohol or pentafluoroalcohol. The catalyst used by the method is fluorine-containing alkanol liquor of the fluorine-containing sodium alkoxide, and the fluorine-containing sodium alkoxide is one of reaction materials, so that any other solvent is not needed to be added, and therefore, separation of the solvent and reaction products is avoided, after-treatment steps are reduced, production cost is saved, reaction yield is high, product purity is high, and economic benefits are very high.

The invention discloses preparation and application of 4-chlorine-3-ethyl-1-methyl-N'-(2-substituted phenoxy acetyl)-1H-pyrazol-5-carbohydrazide compounds. The preparation comprises the following steps: carrying out backflow reaction on thionyl chloride and N-methyl-3-ethyl-4-chloride pyrazole carboxylic acid for 1h to obtain a compound (II), putting the mixed liquor of a compound (III), an organic solvent and an acid-binding agent in a round-bottom flask, dropwise adding the compound (II) at 20-30 DEG C while stirring, then heating up to backflow reaction, carrying out TLC tracing until the raw materials are completely reacted, stopping the reaction, respectively extracting by using 50ml of water twice, drying the organic layer by anhydrous NaSO4, evaporating out the solvent under reduced pressure, and carrying out recrystallization to obtain the target compound shown in the formula (I). According to the preparation and the application, the reaction conditions are mild, the postprocessing is convenient and the total yield of the reaction is as high as 81%; and the compound has a herbicidal activity, thus laying a foundation for the research and development of new pesticides.

The invention discloses a preparation method of a high-frequency wave-transparent sandwich structure composite material 5G antenna housing. The antenna housing consists of an outer covering skin and acore layer material, wherein the skin adopts a glass fiber-reinforced cyanate ester modified epoxy resin composite material, and the core layer selects an aramid fiber honeycomb core. By adopting a hot-pressing tank secondary forming process, the compactness of the composite material is ensured, the porosity of an antenna housing product is reduced, the antenna housing also has high strength, high temperature resistance, low dielectric constant and a high wave transparent rate while meeting high frequency, the production efficiency is high, the assembling procedures are reduced, the cost is low, the quality is stable, and the mass production requirement and the performance requirement of the civil antenna housing product can be met.

The invention provides a preparation method of a lanthanide fluoride two-dimensional porous nanosheet, and belongs to the field of novel materials. The method comprises the following steps: mixing water-soluble lanthanide metal salt with a sodium acetate aqueous solution in a nitrogen atmosphere to obtain a mixed solution; adding the aqueous solution of fluorine-containing salts to the mixed solution for precipitation reaction to obtain the lanthanide fluoride two-dimensional porous nanosheet. Additional surfactants or template agents are not needed to be added in the preparation process, pollution of the surfactants on the surface of a preparation material is prevented, the complicated template agent post-treatment step is reduced, large-scale production can be performed, and one-step large-scale preparation of the lanthanide fluoride two-dimensional porous nanosheet constructed by nanoparticles is realized; other organic solvents are not needed, and environmental pollution caused bythe preparation process is prevented.

The invention discloses a method for preparing a hierarchical pore carbonic oxide microsphere material. The method comprises the following steps: A, impregnating PU foam with a PAA solution, and drying for 6-20 hours at 50-90 DEG C in vacuum; B, heating the PU foam after impregnating and drying in an inert gas atmosphere, namely heating for 0.5-3 hours at 80-120 DEG C, increasing the temperature to 170-230 DEG C and heating for 0.5-3 hours, and increasing the temperature to 270-330 DEG C and heating for 0.5-3 hours; and C, roasting for 1-6 hours at 500-800 DEG C in the inert gas atmosphere after the heating treatment in the step B is completed, and cooling to room temperature. The method is simple, has low cost and short reaction time, and is suitable for industrial production; and the prepared carbonic oxide microsphere material has an ideal flower-like spherical shape, a micropore-mesopore-macropore hierarchical porous structure, a large specific surface area, high nitrogen content and excellent electrochemical performance, and has huge application prospects in the field of super-capacitors.

The invention provides a method for synthesizing a metal-organic framework MIL-101-Cr with carboxylate as organic ligand and a purifying method for the MIL-101-Cr. The method comprises the following steps: preparation of terephthalate; synthesis of a sample; purification of the sample; etc. According to the invention, terephthalate is used for replacing terephthalic acid as organic ligand for hydro-thermal synthesis of the MIL-101-Cr, so the problem of obstruction of microchannels caused by difficulty in dissolving terephthalic acid in water can be overcome; nitrogen adsorption, XRD, TEM and other methods are employed for characterization of MIL-101-Cr synthesized with carboxylate as the organic ligand. Results show that an unpurified MIL-101-Cr product has a clear microporous structure and has a BET specific surface area of 2600 m<2> / g. The product has uniform particle sizes and is a crystal with a small particle size of 60 nm, which is far less than the particle size of a product prepared by using a traditional hydrothermal method. The MIL-101-Cr synthesized with carboxylate as the organic ligand has high purity without complex subsequent purification, and the yield of the MIL-101-Cr reaches 70%.

The invention relates to a nuclear staining cell counting method based on deep learning of an incomplete label, computer equipment and a storage medium, and the method comprises the following steps: (1) making label data: loading a pathological image to label software, and obtaining sub-mask image data pairs of all sub-images and positive cells; (2) model training: training a convolutional neural network model to respectively obtain a trained positive cell convolutional neural network model and a trained negative cell convolutional neural network model; (3) reasoning stage: inputting pathological images to be detected into the trained convolutional neural network model to obtain real mask images; and (4) post-treatment stage: calculating the number of positive cells and negative cells, and calculating to obtain the proportion p of the positive cells in all the cells. The method does not need extra parameters, is high in universality, greatly reduces manual adjustment, and effectively improves the recognition accuracy and robustness. The method is faster, more accurate and more effective in data marking.

The invention provides a method for processing microalgae. The processing method includes placing microalgae liquid in an environment with a normal temperature and pressure, increasing the temperature and pressure of the environment of the microalgae liquid, continuously subjecting the microalgae liquid to the environment after the temperature and pressure are increased, and directly transferring the microalgae liquid to a vacuum environment from the environment. The invention further provides a device for preparing the microalgae, which includes a microalgae liquid storage tank used for storing the microalgae liquid at the normal temperature and under the normal pressure, a high-pressure pump used for pressurizing the microalgae liquid storage tank, a heater used for heating the microalgae liquid storage tank, a vacuum container with a vacuum pump, which is empty inside and used for containing the microalgae liquid obtained from the microalgae liquid storage tank, and a buffer tank used for containing water discharged from the vacuum container. According to the method and the device for processing microalgae, the collecting, wall-breaking and drying of the microalgae are achieved simultaneously or performed by one step and the extraction rate of microalgae oil after wall-breaking can be reached above 90%. The method and the device for processing microalgae have the advantages of simple process, high wall-breaking efficiency, low energy consumption, and the like.

The invention relates to a preparation process of neopentyl polyol oleate. The preparation process comprises the following steps: by aiming at different batches of purchased neopentyl polyol and oleic acid, firstly determining a theoretical molar ratio required by a complete esterification reaction between neopentyl polyol and oleic acid according to the number of hydroxide radicals in molecules of utilized neopentyl polyol or mixed neopentyl polyol, or carrying out multiple small experiments according to a previous experience molar ratio of neopentyl polyol or mixed neopentyl polyol to oleic acid, ending the experiment when the acid value of a small experiment sample is less than or equal to 1.5mgKOH / g and synthetic liquid and water is well separated, and producing by taking the raw material batch and raw material ratio of the last small experiment as the raw material ratio for large-scale production. The preparation process has the advantages that the raw materials can be adequately utilized, and troubles in after-treatment of products are reduced.

The invention discloses a preparation method of ciprofloxacin hydrochloride. The existing synthesis method generally uses isoamyl alcohol and the like as solvent, thus having the problems of strong smell, difficult biodegradation and higher environmental pollution. If the solvent such as the isoamyl alcohol and the like is used, more alkali insoluble substances and acidic insoluble substances are generated in recovery after the reaction, so that the insoluble substances are needed to be treated by purification through the steps such as alkali-dissolving heat-filtering call-back throw filter, acidic-dissolving heat-filtering call-back throw filter, salifying decoloration heat-filtering and the like, the process route is longer, and the product yield is lower. The preparation method of the ciprofloxacin hydrochloride selects the proper solvent as reaction medium, firstly leads cyclopropane carboxylic acid and piperazine to have piperazine reduction reaction and then leads the reaction product to be salified together with hydrochloric acid. In the reaction process, less alkali insoluble substances and acidic insoluble substances are generated in the reaction process, and the ciprofloxacin hydrochloride can be obtained by salifying decoloration heat-filtering, separation by crystallization, throw filter, rinsing and drying after being directly cooled and leached, so that the time for occupying equipment and the time of working procedures are shortened, and the production efficiency of a workshop is improved.

The present invention discloses a ketone oxime ester photoinitiator green synthetic method. According to the method, diphenyl sulfide as a raw material is condensed with caprylyl chloride under the effect of a zirconium catalyst, and then a ketone oxime ester photoinitiator can be obtained by oximation and esterification. The method does not relate to high temperature and high pressure reaction, and is mild in reaction conditions, and good in security. No aluminum chloride or zinc waste water is produced due to use of the zirconium catalyst during the synthesis process, produced byproducts can be recycled, no environmentally harmful solvent is used, and the ketone oxime ester photoinitiator green synthetic method is environmentally friendly, and therefore suitable for industrial production.

The invention relates to a method for liquid nitrogen assisted preparation of high quality graphene, and high quality graphene prepared through the method. According to the present invention, the graphene has characteristics of low oxygen content, few defects, high content of few-layer graphene (less than 5 layers) and high two-dimensional lamella size; the method comprises: placing worm-like graphite in liquid nitrogen, stirring at a high speed, and volatilizing the liquid nitrogen after completing the stirring to obtain the graphene powder; the method is fast, efficient, safe, environmentally friendly and low-cost; the obtained graphene has good quality and has the oxygen content of below 8%, wherein the peak intensity ratio of the D peak to the G peak is below 0.8, and the peak intensity ratio of the 2D peak to the G peak is more than 0.2 in the Raman spectrum of the graphene; and the method can be used for the large-scale production of high-quality graphene.

The invention discloses a micro-electromechanical structure and a manufacturing method thereof. In the invention, the micro-electromechanical structure comprises a substrate and at least one suspending microstructure which is positioned on the substrate. The suspending microstructure comprises multiple metal players, at least one dielectric layer and at last one edge metal wall, wherein the dielectric layer is clamped between the metal layers and the edge metal wall is parallel to the thickness direction of the suspending microstructure and surrounds the edge of the dielectric layer. The edge metal wall can resist etching liquid erosion of the dielectric layer in the process and the structure that the metal layers are compounded with the dielectric layer can increase the structural strength of the suspending microstructure in the thickness direction.

The invention discloses a method for preparing an amino acid derivative by using a photocatalysis micro-channel. The method comprises the following steps: (1) dissolving a cysteine derivative and a diazonium acid ester compound in a solvent to prepare a homogeneous solution; (2) pumping the homogeneous solution prepared in the step (1) into a micro-reactor in a micro-channel reaction device provided with a light source for a reaction; and (3) collecting effluent of the microreactor to obtain the amino acid derivative. The reaction involved in the invention is a novel method for synthesizing the amino acid derivative, and the method does not need a homogeneous system added with a catalyst and other additives, and has good applicability to ortho-substituted diazonium acid ester, meta-substituted diazonium acid ester and para-substituted diazonium acid ester.

The invention belongs to the field of medicine processing, and specifically relates to a synthesizing technology of a triazole derivative. The synthesizing technology provided by the invention is advantaged in that: the raw materials are easy to obtain, the time consumption is low, the condition is mild, and the yield is high. A technical scheme adopted by the invention comprises steps that: methanamide is added into a four-port flask provided with a stirrer, a constant-temperature dropping funnel, a distillation apparatus and a tail gas absorbing apparatus; methanamide is heated to a temperature of 175-190 DEG C; hydrazine hydrate is dropped into methanamide, wherein a molar ratio of methanamide to hydrazine hydrate is 1:1.1-1:2; the dropping is finished in 0.5-2.5h; emitted ammonia gas is delivered into an absorbing bottle to be absorbed, wherein the absorbing bottle contains 20-30% H2SO4; when dropping is finished, the temperature is maintained for 0.5-2.5h; the materials are cooled; when a large amount of crystals are precipitated, the materials are subject to pump filtration, such that a crude product is obtained; the crude product is washed by using ethyl acetate, such that a target product 1H-1,2,4-triazole is obtained. A yield is calculated, and a melting point is detected.

The invention discloses a surface-exposure-based multi-degree-of-freedom 3D printing method, and relates to the technical field of 3D printing. The method solves the technical problem that a support needs to be additionally arranged during workpiece manufacturing and then consumables are increased. The method comprises the following steps that firstly, a triangular patch on the surface of a printing model is partitioned, the triangular patch in the area is normalized to obtain an outer normal vector of the area face, and the area face and the corresponding outer normal vector are put into an area set; and then, the candidate substrate intersection surface and parameters of the printing model are searched, and based on the candidate substrate intersection surface and the area set, the cutting surface is found so that the printing model can carry out unsupported printing by taking the candidate substrate intersection surface and the cutting surface as the bottom. The invention further discloses a surface-exposure-based multi-degree-of-freedom 3D printing device and system. According to the printing method, device and system, support is not needed to be additionally arranged, so thatthe product quality is improved while consumables are reduced. The manufacturing direction variability improves the flexibility of the slicing direction, the number of slicing layers is increased, andthe fine degree of the model is also improved.

The invention relates to a preparation method of lenvatinib and salt thereof. The adopted method for preparing the lenvatinib has the advantages that the process is simple, the cost is low, the purity is high, the single-purity content meets the regulations, and the industrial production is easier.

The invention discloses a high-performance adsorption material and a preparation method thereof. A hierarchical-pore nitrogen doped carbon / MgO composite microsphere material is prepared by performing a high-temperature thermal treatment carbonization method on polyimide serving as a carbon and nitrogen source, polyurethane foam serving as a macroporous scaffold and metal magnesium salt serving as an additive. According to the high-performance adsorption material and the preparation method thereof, the use of an expensive template agent and a toxic raw material reagent is avoided; the prepared composite microsphere material has an ideal flower-shaped spherical appearance, is of a hierarchical-pore structure with micro holes and macro holes, has controllable surface characteristics, excellent structural stability, high nitrogen content and magnesium content, and shows high adsorption volume and excellent circulating stability when used as a CO2 adsorption material. The preparation method disclosed by the invention is simple and feasible; the process is controllable, and the reaction time is short; furthermore, no complicated experimental equipment and complicated experimental steps are needed; and the industrial large-scale production is facilitated.

The preparation process of the solid component of olefin polymerizing catalyst includes first reaction of C2-C8 alcohol and magnesium powder in the molar ratio of 2.0-4.0 in the presence of methane halide to form homogeneous magnesium ligand solution; subsequent addition of electron donor compound to form homogeneous solution and the reaction between the solution with titanium compound to form Mg-Ti ligand solution; the contact reaction between the solution with inorganic oxide carrier to prepare solid catalyst precursor; and final activation of the precursor with alkyl aluminum chloride to obtain the solid catalyst. The solid component of catalyst of the present invention is matched with alkyl aluminum for the polymerization of ethylene and has high catalytic activity and polymer prepared with very small amount of fine powder.

The present invention discloses a hemodialysis medicinal component sodium diacetate preparation method, which comprises: (1) adding a raw material drug sodium acetate to a reaction kettle, heating while stirring, and adding food grade glacial acetic acid to the reaction kettle in a dropwise manner to react, wherein a molar ratio of the medical sodium acetate to the food grade glacial acetic acid is 1:(1.1-2.0); and (2) after completing the reaction, heating to a temperature of 110-120 DEG C, carrying out reflux for 1-2 h, filtering while hot, cooling to a room temperature to obtain a crystal, and rapidly drying the crystal to obtain the medicinal sodium diacetate. According to the present invention, the prepared sodium diacetate meets the medicinal standard, the product is the solid, has characteristics of easy transportation, easy storage and risk reducing, and can be used for hemodialysis powder preparation.

A technical solution adopted by the invention relates to a preparation method for 3-chloropropionylchloride. The preparation method comprises the following steps of mixing acrylic acid and water; dropwise adding thionyl chloride at a temperature of 20 DEG C; refluxing for 3-8 h by heating until acrylic acid is reacted completely; distilling to a temperature of 120 DEG C under a normal pressure; and then distilling out a product under a reduced pressure. The preparation method has the beneficial effects that cost is greatly reduced than that of a two-step method; post treatment steps are few; and the product is high in yield and high in purity. Besides, according to the preparation method, water is added, thereby facilitating the reaction. Compared with preparation methods reported in the prior art, the preparation method has essential difference. Results of gas phase analysis and standard sample contrast analysis show that the product is 3-chloropropionylchloride. The product is used for preparing 3'-chloropropiophenone; and the product and the yield are the same.

The invention belongs to the field of herbicides and particularly relates to a synthetic method of s-metolachlor. The synthetic method of s-metolachlor comprises the steps that a cheap compound 2-methyl-6 ethyl benzene easy to obtain is used as a raw material, and finally the high-quality herbicide product s-metolachlor is obtained through condensation reaction, catalytic hydrogenation reduction reaction, chloride acetylation reaction and purification treatment. The simple water-phase s-metolachlor synthesis method easy to execute is provided, the yield of the s-metolachlor product reaches 98.5% and the purity reaches 98.2% in a kilogram-level experiment, and the environment-friendly synthesis method is suitable for industrial production. In addition, compared with a traditional organic solvent synthesis method, use of organic alkali is avoided, few post-treatment steps are adopted, the production pollution is low, the cost is low, required material types are few, the solvent use amount is small, the cost is low, and the method is suitable for large-scale popularization and use.

The invention discloses a preparation method of dapagliflozin. The preparation method comprises the following steps: (1) reacting a compound solution as shown in a formula II and an n-butyllithium solution in a first microreactor in a microchannel reaction device; (2) reacting effluent of the first microreactor with a compound as shown in a formula III in a second microreactor in the microchannel reaction device to obtain a compound as shown in a formula IV; (3) carrying out reduction reaction on the compound shown in the formula IV in a third microreactor in the microchannel reaction device to obtain a compound shown in a formula V; and (4) deprotecting the compound as shown in the formula V to obtain dapagliflozin as shown in the formula I. According to the method disclosed by the invention, benzyl-protected glucolactone is adopted as a starting raw material, so that generation and multiple derivatization of isomer impurities and ring-opening impurities are avoided, the stereoselectivity is relatively high, and post-treatment steps and waste generation are reduced; and meanwhile, the yield is high, the purity is high, the synthesis steps are few, the operation is simple and convenient, and the safety is high.

The invention provides an acidic waste gas treatment device and belongs to the technical field of gas treatment equipment. The acidic waste gas treatment device comprises a liquid storage tank, a first gas-liquid mixer and a conveying pump, wherein the first gas-liquid mixer is provided with a first mixing chamber, a first liquid inlet, a first liquid outlet and a first gas inlet for inputting the acidic waste gas; the first gas inlet, the first liquid inlet and the first liquid outlet are all communicated with the first mixing chamber; a first input hole and a first output hole are formed on the liquid storage tank; an input end of the conveying pump is connected with the first output hole; an output end of the conveying pump is connected with the first liquid inlet; the first liquid outlet is connected with the first input hole. The acidic waste gas treatment device is simple in structure, small in volume, low in use cost and capable of reducing the discharge index and processing cost of the acidic waste gas.

The invention belongs to the field of medicament processing and particularly relates to a process for synthesizing a triazole derivative. The process has the advantages that the raw materials are easily available, time consumption is low, reaction conditions are mild and yield is high. According to the technical scheme, the process comprises the following steps: adding formamide to a four-necked flask which contains a stirrer, a constant-pressure dropping funnel, a distillation device and a tail-gas absorption device; heating to a temperature of 175-190 DEG C; dropwise adding hydrazine hydrate for 0.5-2.5 hours, wherein the molar ratio of formamide to hydrazine hydrate is 1:(1.1-2); introducing the escaping ammonia into an absorption bottle filled with 20-30% H2SO4; preserving heat for 0.5-2.5 hours after finishing adding dropwise; cooling and filtering after a large amount of crystals are separated, to obtain a crude product; washing the crude product by ethyl acetate to obtain the target product which is 1H-1,2,4-triazol; calculating the yield; and measuring the melting point.

The invention relates to a preparation method of hydrofluoride ether, and particularly relates to a method for preparing 1,1,2,2-tetrachlorofluoroethyl-2,2,3,3-tetrachlorofluoropropyl ether. The method comprises the following steps: with tetrachlorofluoropropyl alcohol as an initial raw material and sodium tetrachlorofluoro-propoxide as a catalyst, reacting with a tetrafluoroethylene monomer, and carrying out after treatment on reaction products to obtain the 1,1,2,2-tetrachlorofluoroethyl-2,2,3,3-tetrachlorofluoropropyl ether. The catalyst used by the method is a tetrachlorofluoropropyl alcohol solution containing the sodium tetrachlorofluoro-propoxide, while the tetrachlorofluoropropyl alcohol is also one of the reaction raw materials, so any other solvents need not to be added so as to avoid separation of the solvent and the reaction products, reduce the after treatment steps and lower the production cost; by using the sodium tetrachlorofluoro-propoxide as the catalyst, the product yield is high and the purity is high.

The invention discloses a preparation method of hydroxymethylated lignin. The method comprises the following steps: adding certain amounts of lignin, a formaldehyde solution and a solid base into a hydrothermal reactor, performing uniform stirring, sealing the reactor, heating the reactor to a specific temperature, carrying out a reaction for a period of time, cooling the obtained reaction productto room temperature, and carrying out washing, suction filtration and drying on the product to obtain the hydroxymethylated lignin. The method for preparing the hydroxymethylated lignin by a hydrothermal process has the advantages of easiness in operation, simplicity in post-treatment, no acidification precipitation step, facilitation of further high-value utilization of the hydroxymethylated lignin, and good application prospect.

The invention discloses a synthetic method of tapentadol. The method comprises the following steps: reacting meta-substitution cinnamic acid serving as a starting material with a chiral adjuvant to obtain amide; reacting the amide with a nucleophilic reagent and an electrophilic reagent, and introducing two chiral centers to obtain a chiral product; performing reduction and deprotection on the chiral product to obtain chiral alcohol; performing an amination reaction and a substitution reaction on the chiral alcohol to obtain the tapentadol. The tapentadol is synthesized by taking cheap and readily-available (1R,2R)-psedo-ephedrine as the chiral adjuvant, forming two chiral centers by using a one-pot method and performing simper deprotection and subsequent transformation. By adopting the synthetic method, the reaction route can be simplified, post-treatment steps can be reduced, and the production cost is reduced. The synthetic method is more suitable for industrial application.