37results about How to "Synthetic mild" patented technology

The invention discloses a preparation method of an ultrathin B phase titanium dioxide nano sheet, and relates to the field of titanium dioxide. The preparation method comprises the following steps: (1) adding a titanium precursor into glycol, and stirring to obtain a glycol-titanium solution; (2) adding water into the glycol-titanium solution obtained in the step (1), stirring, carrying out reactions at a temperature of 150 to 180 DEG C, and subjecting the obtained turbid liquid to centrifugation so as to obtain white precipitate; (3) washing the white precipitate obtained in the step (2), and drying white precipitate in the air to obtain the ultrathin B phase titanium dioxide nano sheet. The preparation method has the advantages that the raw materials are cheap, little sulfuric acid is used, the output of waste byproducts is little; the reaction temperature is mild and is far lower than the boiling point of glycol; the reaction pressure is not high and thus is benefit for amplification operation; the thickness of the prepared ultrathin titanium dioxide nano sheet is less than 2 nm, the nano sheet appears typical characteristics of a two-dimensional material; the operability is strong, the reaction apparatus is simple, the synthesis and post treatment conditions are mild, the conditions during the preparation process are mild, the reaction process is clean and pollution-free, and the reaction efficiency is high.

The invention discloses a catalyst for polylactone preparation. A raw material lactone monomer undergoes ring-opening polymerization under the action of a difunctional group ionic liquid catalyst to obtain polylactone, and the catalyst is 1-(4-sulfo)butyl-3-methylpyrazinyltetrafluoroborate or 1-(4-sulfo)butyl-3-methylimidazolyltetrafluoroborate. The catalyst can catalyze lactone ring-opening polymerization to obtain polylactic acid, polyglycolic acid, poly(trimethylene carbonate) or other degradable polymers.

The invention provides a preparation method and application of uniform-size graphene quantum dots. The method adopts a strategy from top to bottom; oxidized graphene is used as raw materials; an ultrasonic auxiliary hydrothermal method is used; the ultrasonic mechanical stress is used for assisting the high oxidation effect of nitric acid for cutting carbon-carbon bonds; then, high-temperature heat treatment is performed to prepare a pure graphene quantum dot material with the uniformly distributed size. The method process is simple; the conditions are mild; the prepared graphene quantum dotshave good purity degree, small particle diameter and uniformly distributed size. Used as an electrode material of an energy storage device, the prepared graphene quantum dot material shows excellent electrical conductivity, high specific capacity, excellent rate performance, fast ion adsorption and transmission rate and long cycle service life; good application potential is realized in the field of energy storage devices.

The invention relates to copper-silicon catalysts, in particular to a preparing method of a copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate. The preparing method includes the steps that silica sol is added into water to obtain silica sol dispersion liquid; copper salt is dissolved in deionized water, ammonia water is added to form a copper-ammonia complex-ion solution, and then ammonia chloride is added to obtain a copper-ammonia complex-ion mixed solution; the silica sol dispersion liquid is added into the copper-ammonia complex-ion mixed solution to obtain a silica sol and copper-ammonia complex-ion mixed solution, the mixed solution is transferred into a closed container, the container is placed in a constant-temperature environment to obtain blue precipitate, blue powder is obtained through cleaning and then airing and dispersed into water again, and dispersion liquid of a mesoporous copper-silicon catalyst precursor is obtained after ultrasound treatment; the dispersion liquid is placed in a water bath, L-arginine and a cationic surface active agent are added into the dispersion liquid, and then tetraethoxysilane is added to obtain light blue precipitate; the light blue powder is obtained through cleaning, airing and heat treatment, and the cationic surface active agent is removed from the light blue powder to obtain the copper-silicon catalyst for preparing ethylene glycol by hydrogenating dimethyl oxalate.

The invention relates to a strontium titanate-titanium dioxide composite nanotube array film and a preparation method and application thereof. The film is obtained through direct growth on a conductive glass substrate with a three-step hydrothermal method; hydrothermal synthesis of titanium dioxide nanorods is carried out in the first step, the titanium dioxide nanorods are etched to generate titanium dioxide nanotubes in the second step of hydrothermal treatment, strontium hydroxide serves as a strontium source in the third step of hydrothermal reaction, and finally the composite film with perovskite type strontium titanate nanoparticles uniformly distributed on the surface of the titanium dioxide nanotube array is obtained, wherein the titanium dioxide nanotubes are vertically arrayed on the conductive glass substrate. The composite film can serve as an anode material of solar cells or serve as a photocatalyst for degradation treatment of photolysis water or organic matter. The three-step hydrothermal method is adopted for in-situ synthesis, the preparation process and needed equipment are simple, the controllability is high, and production is safe, free of toxin and environmentally friendly; by assembling the film into solar cells, the sunlight capturing capability of photoanodes can be improved, and the photoelectric conversion efficiency can be improved.

The invention discloses an acetylene amide mediated method for selectively synthesizing carbonyl thioesters and ordinary thioesters. The ordinary thioesters are further used for preparing amides and peptides, and the carbonyl thioesters are used for preparing thioamides and thiopeptides. An addition reaction is carried out between acetylene amide in m-xylene and thiocarboxylic acid to selectivelyobtain the carbonyl thioester and ordinary thioester of which the ratio is 3:1 under the condition of 40 DEG C below zero; the ordinary thioesters can carry out a combination reaction with amines to produce amides and peptides; and the carbonyl can carry out a combination reaction with the amines to produce thioamides and thiopeptides. The method disclosed by the invention is mild in reaction conditions, free of any metal catalyst, high in reaction speed, high in yield, simple in operation and wide in application range. With respect to chiral thiocarboxylic acid in a position alpha of carboxyl, when thioamide bonds or thiopeptide bonds are formed from the carbonyl thioesters or when amido bonds or peptide bonds are formed from the ordinary thioesters, any racemization phenomenon can be avoided.

The invention discloses a preparation method of hollow mesoporous silica nanospheres and relates to a silica nanosphere. The preparation method comprises the following steps: adding the silica nanospheres into water, performing ultrasound treatment to get dispersion liquid of the silica nanospheres, then refluxing the dispersion liquid of the silica nanospheres, further centrifugating and collecting the silica nanospheres; dispersing the silica nanospheres in the water, adding cetyltrimethylammonium bromide and stirring to get the dispersion liquid; further adding NaOH, etching, standing for cooling, collecting sediment, cleaning and airing to get white powder; and removing a cationic surfactant in the white powder to get the hollow mesoporous silica nanospheres with greater aperture.

The invention provides series cosmetics containing glycosylglycerol (aGG) and a preparing method thereof. The series cosmetics comprise moisturizing watery essence, moisturizing cream, after-sun repairing gel, moisturizing masks and brightening masks. The series cosmetics in a formula are prepared from, by mass, 0.5%-1% of glycosylglycerol (aGG), 0.01%-0.1% of oat-beta-glucan, 0.01%-0.1% of a seaweed extract, 0.01%-1% of a green tea extract, 0.01%-0.1% of sodium hyaluronate, 0.01%-1% of a mint extract amd 0.001%-0.01% of rose essential oil. The moisturizing series cosmetics have a good moisturizing effect, and are free of stimulation and toxic and side effects.

The invention discloses a preparation method of 3', 4', 7-trihydroxy isoflavone (T1) and 4', 6, 7-trihydroxy isoflavone (T2). The T1 and T2 are used in military medicine Research. The present invention uses cheap and easy-to-get chemical raw materials: resorcinol and 3,4-dimethoxyphenylacetonitrile or 3,4-dimethoxyphenol and p-hydroxybenzonitrile as starting materials, and the improved Hoesch Reaction, carbo-increasing and ring-closing reaction and three-step reactions such as removing dimethyl protection, respectively obtained 3', 4', 7-trihydroxy isoflavone (T1) and 4', 6, 7-trihydroxy isoflavone (T2 ). The method has the characteristics of economy, high efficiency, environmental protection, industrialization and the like.

The invention discloses a preparation method of poly epsilon-caprolactone. The method includes: mixing epsilon-caprolactone with an alcohol molecular weight regulator in proportion, then adding 1-(4-sulfonyl)butyl-3-methylpyrazine tetrafluoroborate or 1-(4-sulfonyl)butyl-3-methylimidazole tetrafluoroborate as the catalyst, and at a temperature of 60-180DEG C, carrying out ring opening polymerization under anhydrous and oxygen-free conditions to obtain poly epsilon-caprolactone.

The invention provides a synthesis method of pidotimod disclosed as Formula (1). The synthesis method comprises the following steps: (1) carrying out condensation reaction on thioproline and cyprolidol under the actions of a catalyst and a condensation reaction solvent to obtain an intermediate I; (2) carrying out condensation reaction on the intermediate I and pyroglutamic acid under the actions of a catalyst and a condensation reaction solvent to obtain an intermediate II; and (3) dropwisely adding an acidic material into the intermediate II, and carrying out degreasing reaction in a degreasing reaction solvent. The synthesis method avoids using thionyl chloride, pentachlorophenol and other toxic reagents, and thus, has favorable environment friendliness. The method does not need strong alkali high-temperature esterolysis, so the synthesis process is milder. The intermediate I and intermediate II can absorb ultraviolet light, so that the whole synthesis progress can be monitored conveniently. In addition, the optical purity of the pidotimod prepared by the synthesis method is higher.

The invention discloses a preparation method of glycidyl ether epoxy resins with low total chlorine content. The preparation method comprises two steps of synthesis and refining treatment, wherein in the synthesis step, a phenol or alcohol raw material, epoxy chloropropane, an aprotic polar solvent and a granular alkali metal hydroxide with a specific particle size are subjected to a one-step reaction; and in the refining step, the resin product is treated by adopting an alkaline aqueous solution with the concentration of 2-10%. According to the preparation method disclosed by the invention, the ultra-high-purity epoxy resin with the total chlorine content lower than 200 ppm can be obtained. The preparation method provided by the invention is suitable for preparing various glycidyl ether epoxy resins, and has the advantages of low total chlorine content of the product, high epoxy value and yield, mild reaction conditions and the like.

Disclosed is a method for synthesizing a novel chiral ligand, a metal chelate, a variety of non-natural amino acids, Maraviroc and a key intermediate thereof. In the invention, (R)-2-methyl proline is selected and used as a starting raw material, (S)-β3-amino acid is obtained by asymmetric resolution induced by using a nickel chelate, and Maraviroc is synthesized by using (S)-3-amino-3-phenylpropionic acid as a key intermediate with a high yield and the ee value reaching 98.2% or more. The method of the present invention has widely available materials, mild synthetic process conditions, is easy to control, and produces a product of a high optical purity.

The invention discloses a molecular weight controllable poly epsilon-caprolactone and a preparation method thereof. The method includes: mixing epsilon-caprolactone with an alcohol molecular weight regulator in proportion, adding 4-methyl-1-(4-sulfobutyl)pyridine tetrafluoro-borate or 1, 1'-(butane-1, 4-diyl)bis[3-(4-sulfobutyl)-imidazole]tetrafluoroborate to serve as the catalyst, and conducting ring opening polymerization at 60-180DEG C and under anhydrous and oxygen-free conditions, thus obtaining poly epsilon-caprolactone.

The invention relates to a silver-iron oxide composite structure film and a preparation method and application thereof. The silver-iron oxide composite structure thin film is prepared through a three-step method, firstly, silver-iron oxide composite particles are prepared through a reflux condensation method, then, the particles are dispersed in a PU adhesive to prepare slurry, then, a conductivesubstrate is coated with the slurry through a dispensing method, and finally, the silver-iron oxide composite structure thin film is obtained after calcination. The composite structure film can be used as a cathode of a photocatalytic fuel cell or a dye-sensitized solar cell, and compared with a common platinum electrode, the silver-iron oxide composite structure film is lower in cost and better in cathode dye degradation or heavy metal ion reduction effect. The preparation process and required equipment adopted by the invention are simple, high in controllability, safe in production, non-toxic and environment-friendly; and when the structure fil, is assembled into a photocatalytic fuel cell as a cathode, degradation of dye in a cathode chamber or reduction of heavy metal ions can be accelerated, and meanwhile, power generation can be realized.

The invention discloses a preparation method of a copper-silicon catalyst used for hydrogenation of dimethyl oxalate to ethylene glycol, relating to the copper-silicon catalyst. Add silica sol to water to obtain silica sol dispersion; dissolve copper salt in deionized water, add ammonia water to form copper ammonium ion solution, and then add ammonium chloride to obtain copper ammonium ion mixed solution; add silica sol dispersion to copper A mixed solution of ammonium ions to obtain a mixed solution of silica sol and copper ammonium ions, then transferred to a closed container, placed in a constant temperature environment, to obtain a blue precipitate, washed and dried to obtain a blue powder, and then dispersed in water, Obtain the dispersion of the mesoporous copper-silicon catalyst precursor after ultrasonication; then place it in a water bath, add L-arginine and cationic surfactant to the dispersion, and then add ethyl orthosilicate to obtain a light blue precipitate; After washing and drying, a light blue powder is obtained. After heat treatment, the cationic surfactant is removed from the light blue powder to obtain a copper-silicon catalyst for hydrogenation of dimethyl oxalate to ethylene glycol.

The invention discloses a laser desorption ionization mass spectrometry method. The method comprises the steps of: (1) forming a polydopamine modified layer on the surface of a solid material so as toobtain a sample carrying substrate; (2) applying a to-be-detected sample to the surface of the polydopamine modified layer of the sample carrying substrate, and then drying the to-be-detected sample;and (3) carrying out laser desorption ionization mass spectrometry on the sample carrying substrate. The polydopamine modified solid material is used as the sample carrying substrate (a target plate)for laser desorption ionization, only the one-step target plate preparing process is required, and a matrix does not need to be added; by adopting the polydopamine modified solid material to carry out spectrometry detection and spectrometry imaging, the laser desorption ionization mass spectrometry method has an excellent signal-to-noise ratio, excellent repeatability and a high spatial resolution, and can implement universal, simple, efficient, rapid and sensitive spectrometry soft ionization detection and spectrometry imaging analysis.

The invention discloses a molybdenum sulfide-zirconium phosphate catalyst for preparing allyl alcohol through glycerin hydrogenation and a preparation method and application of the catalyst. The molybdenum sulfide-zirconium phosphate catalyst is prepared in the mode that zirconium phosphate and molybdenum sulfide are mixed through a ball milling method, and the mass ratio of the zirconium phosphate to the molybdenum sulfide is (0.5-2):1. The molybdenum sulfide-zirconium phosphate catalyst is applied to a gas-phase hydrogenation allyl alcohol preparation reaction for glycerinum, the reaction temperature is controlled within 185-225 DEG C, the hydrogen pressure is controlled within 1-3 MPa, the glycerinum conversion rate after the reaction can reach 49.5-82.8%, the selectivity of the allyl alcohol can reach 40.5%, and the highest time space yield of the allyl alcohol can reach 0.25 g-allyl alcohol / g-catalyst / h.

The invention discloses a preparation method of hollow mesoporous silica nanospheres and relates to a silica nanosphere. The preparation method comprises the following steps: adding the silica nanospheres into water, performing ultrasound treatment to get dispersion liquid of the silica nanospheres, then refluxing the dispersion liquid of the silica nanospheres, further centrifugating and collecting the silica nanospheres; dispersing the silica nanospheres in the water, adding cetyltrimethylammonium bromide and stirring to get the dispersion liquid; further adding NaOH, etching, standing for cooling, collecting sediment, cleaning and airing to get white powder; and removing a cationic surfactant in the white powder to get the hollow mesoporous silica nanospheres with greater aperture.

The invention discloses a fluorescence labelled nucleotide based on a molecular glue and a use thereof in DNA sequencing. The structure formula of the fluorescence labelled nucleotide is shown in a formula (I) in the specification, wherein R1 is shown in the specification, R2 is fluorescein or shown in the specification, and dNTP is ribonucleoside triphosphote which contains four different base groups; the fluorescein is selected from one of the BODIPY, rhodamine, coumarin, xanthene, cyanin, pyrene, phthalocyanine, alexa, a squarene dye, a composition for generating energy transfer dye and the derivatives thereof. The fluorescence labelled nucleotide can be used for DNA sequencing; simultaneously the raw materials for synthesizing the fluorescence labelled nucleotide are simple and easy to obtain and the fluorescence labelled nucleotide can be used for large-scale popularization. The biological assessment result shows that all the requirements of the high-throughput sequencing biochemical reaction can be satisfied by the reversible terminal, and the reversible terminal has good practical prospect.

The invention relates to a silver-iron oxide composite structure film and its preparation method and application. It is prepared by a three-step method. First, the silver-iron oxide composite particles are prepared by a condensation reflux method, and then the particles are dispersed in a PU adhesive. A slurry is made, and then applied on a conductive substrate by a drop-coating method, and finally a silver-iron oxide composite structure film is obtained after being calcined. The composite structure film can be used as the cathode of a photocatalytic fuel cell or a dye-sensitized solar cell. Compared with the common platinum electrode, the silver-iron oxide composite structure film has a lower cost and a better effect on cathode dye degradation or heavy metal ion reduction. it is good. The preparation process and required equipment adopted in the present invention are simple, highly controllable, safe in production, non-toxic, and environmentally friendly; as a cathode, assembled into a photocatalytic fuel cell can accelerate the degradation of the dye in the cathode chamber or the reduction of heavy metal ions, and at the same time can generate electricity.

The invention discloses a method for improving thermal stability of virus-like particles (VLPs) based on metal organic framework biomimetic mineralization. According to the preparation method disclosed by the invention, VLPs is successfully encapsulated in a zeolite imidazole framework 8 (ZIF-8) under the coordination action of dimethylimidazole and zinc nitrate, so that the VLPs-ZIF-8 nanoparticles are formed. According to the invention, a frame structure formed by coordination of metal ions and organic matters is encapsulated outside the virus-like particles, so that the heat resistance of the VLPs vaccine is improved, and the problems of consumption of a large amount of manpower and material resources caused by cold chain transportation and the like are solved. The prepared ZIF-8 metal organic framework is low in cost, the method is simple, and the synthesis process is mild. The cellular immune response level of the VLPs vaccine biomimetically mineralized by the metal organic framework is obviously improved, and a new technical means is provided for improving the cellular immune level of the VLPs vaccine.

The invention provides a synthesis method of pidotimod disclosed as Formula (1). The synthesis method comprises the following steps: (1) carrying out condensation reaction on thioproline and cyprolidol under the actions of a catalyst and a condensation reaction solvent to obtain an intermediate I; (2) carrying out condensation reaction on the intermediate I and pyroglutamic acid under the actions of a catalyst and a condensation reaction solvent to obtain an intermediate II; and (3) dropwisely adding an acidic material into the intermediate II, and carrying out degreasing reaction in a degreasing reaction solvent. The synthesis method avoids using thionyl chloride, pentachlorophenol and other toxic reagents, and thus, has favorable environment friendliness. The method does not need strong alkali high-temperature esterolysis, so the synthesis process is milder. The intermediate I and intermediate II can absorb ultraviolet light, so that the whole synthesis progress can be monitored conveniently. In addition, the optical purity of the pidotimod prepared by the synthesis method is higher.

The invention provides a series of cosmetics containing glycerol glucoside (αGG) and a preparation method thereof. This series includes moisturizing essence, moisturizing cream, after-sun repair gel, moisturizing mask and brightening mask. The cosmetic formula mainly contains the following: Components by mass content: glycerol glucoside (αGG) 0.5‑1%; oat β‑glucan 0.01‑0.1%; seaweed extract 0.01‑0.1%; green tea extract 0.1‑1%; sodium hyaluronate 0.01‑0.1%; peppermint extract 0.1‑1%; rose essential oil 0.001‑0.01%. The moisturizing series cosmetics provided by the invention have good moisturizing effect and no stimulation and no toxic or side effects.

The invention discloses a synthesis method of an antibacterial agent cefoxitin acid. The method comprises the following steps: with 7-aminocephalosporanic acid as a raw material, dissolving the aminocephalosporanic acid with a weak alkaline solution; adding an etherified enzyme to the weak alkaline solution, adding a methoxide reagent, carrying out etherification reaction, and filtering out the etherified enzyme after etherification reaction is ended; adding solidified enzyme to a feed liquid for carrying out hydrolysis; after hydrolysis is ended, adding ethyl acetate to the solution, and beginning to drop a 2-thiophene acetyl reagent; after reaction is ended, dropping a benzthine cellulose acetate water solution to a reaction liquid, and separating out crystal to obtain a compound I; and reacting the compound I with an ammonia methoxyl acylation reagent, and introducing carbamyl methoxyl group to the third site of the compound I to obtain the cefoxitin acid. The synthesis method is mild in reaction condition, simple in synthesis process and easy to implement; the yield is effectively improved; the production steps are shortened; the production cost is reduced; the product purity is improved; the energy consumption is reduced; the wastewater output is reduced; the synthesis method is suitable for carrying out large-scale production.

The invention discloses a preparation method and an application of a bismuth titanium tungstate photocatalyst and belongs to the technical field of material preparation and environmental pollution control. The chemical formula of the bismuth titanium tungstate photocatalystis Bi6Ti3WO18, bismuth nitrate, tetrabutyl titanate and tungsten hexachloride are taken as initiators, a precursor is prepared through esterification complexation, and a Bi6Ti3WO18 nanosheet with photocatalytic activity is prepared through thermal treatment. The prepared photocatalyst has the characteristics of smaller particle size, large specific surface area, high visible light response and high photocatalytic performance. The preparation process is simple, convenient, low in energy consumption and cost and high in yield, meets the actual production requirement and has greater application potential.

The invention relates to a synthesis method of a dipyridyl derivative or an analogue without adding a ligand. The method comprises the steps of mixing and heating 2-halogenated pyridine, its derivative or analogue, nickel salt, zinc powder or manganese powder and halide salt in a solvent to form a coupled product. The method has the advantages that the catalyst ligand is not required to be added; particularly, the high-toxic organic phosphine ligand is not required to be added; the catalyst nickel salt is low in price and small in use amount; and the method is easy and simple to operate, mild in condition, easy to amplify, especially suitable for industrial production, wide in application scope, high in yield, low in cost and environment-friendly.