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 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 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 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 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 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 green and high-efficiency preparation method and application of graphite-phase carbon nitride nanosheets. The method uses layered graphite phase carbon nitride material as raw material, and obtains Pt / graphite phase carbon nitride by modifying Pt nanoparticles on the surface of graphite phase carbon nitride; Pt / carbon nitride is placed in a tube furnace, and Through high-temperature water vapor treatment, graphite-phase carbon nitride nanosheets can be obtained. The preparation method provided by the invention has simple process, mild and controllable conditions, and high yield of graphite-phase carbon nitride nanosheets. The specific surface area of ​​the obtained graphitic carbon nitride nanosheets is significantly increased, the charge separation is significantly improved, and it has good photocatalytic performance.

The invention discloses an in-situ generated perovskite heterojunction photocatalyst, the photocatalyst is composed of CsPbBr 3 and CsPb 2 Br 5 Two phases exist in the form of heterojunction. The catalyst of the present invention is applied to photocatalytic reduction of carbon dioxide, and the activity is pure phase CsPbBr 3 3.63 times that of perovskite quantum dots; successful construction of homoheterojunctions that retain the pure phase CsPbBr 3 The small size effect and particle confinement effect of perovskite quantum dots improve the separation efficiency of electrons and holes, and enhance the activity and stability of perovskite quantum dot materials. In situ generation of CsPbBr compared to heterojunctions reported by other patents 3 / CsPb 2 Br 5 The perovskite heterojunction photocatalyst does not introduce new elements and is formed by a one-step reaction. The synthesis is simple and the reaction conditions are mild. The invention enables the perovskite quantum dot material to have wide application prospects, and meanwhile has theoretical significance in methodological research.

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.

The invention discloses a method for selectively synthesizing thiocarbonyl esters and common thioesters mediated by alkyne amides, further using common thioesters to prepare amides and polypeptides, and using thiocarbonyl esters to prepare thioamides and thioamides peptide. Under the condition of ‑40 degrees Celsius, the addition reaction of alkyne amides and thiocarboxylic acids in m-xylene selectively yields thiocarbonyl esters and common thioesters (3:1); common thioesters can react with amines to form amides, Polypeptides; thiocarbonyl esters can react with amines to generate thioamides or thiopeptides. The invention has mild reaction conditions, no metal catalyst, fast reaction speed, high yield, simple operation and wide application range. For thiocarboxylic acids with chirality at the α position of the carboxyl group, no racemization occurs when thiocarbonyl esters form thioamide bonds or thiopeptide bonds, or ordinary thioesters form amide bonds or peptide bonds. .