185results about How to "No purification required" patented technology

The invention discloses a multifunctional urethane acrylate oligomer as well as a synthesis method and application thereof. The synthesis method comprises the following steps: synthesizing a modified glycidyl ether by adding a diglycidyl ether, a dibasic acid and a catalyst which is the triphenylphosphine into a reactor and subjecting the materials to reaction at 120-150 DEG C for 2.5-3.5 hours; synthesizing a semi-adduct by dropwise adding acrylic hydroxy ester and dibutyltin dilaurate into diisocyanate, and keeping the reaction temperature at 40-50 DEG C until the concentration of the isocyanate group is 48-52% of the initial concentration; and synthesizing a hydroxyl-group containing multifunctional urethane acrylate. In the process of synthesizing, by using the difference of raw materials and controlling the proportion of monomers for reaction, the soft and hard segments are introduced into the molecule structure so that the toughness is increased, and the brittleness of the coating film is improved. The hydroxyl groups are provided in the molecular structure design, which is helpful to the improvement of the adhesion of the coating film on the substrate in the later period.

The invention relates to a preparation method of a high-graphitized nanometer carbon material. The method comprises the following steps: (1), uniformly mixing magnetic metal or metal oxide particles with a solid organic carbon precursor material, wherein the magnetic metal or metal oxide particles in the mixture account for 10 to 80 percent of the total weight; and (2) putting the mixture in a microwave oven and processing in microwave for 3 seconds or longer under the microwave power of 300W to 3000W so as to obtain carbon-wrapped magnetic metal nanometer particles or a multi-wall carbon nanometer pipe material. The prepared carbon material has high graphitization degree, controllable grain diameter and thickness, simple technology, low preparation cost, high product purity, wide selective raw material range and easy mass preparation.

The invention provides a synthetic method of plant growth regulator trinexapac-ethyl intermediate 3-carbethoxy-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate. The synthetic method comprises the following steps: (1) carrying out annulation reaction on 2-acetonyl-1,4-diethyl succinate and organic alkaline at the temperature of 20-120 DEG C for 0.5-5 hours in a non-polarity organic solvent to obtain 3,5-cyclohexanedione-1-ethyl formate; and (2) adding organic amine and cyclopropanecarboxylic acid chloride, and carrying out acylation reaction at the temperature of minus 5-50 DEG C, so as to obtain 3-ethoxycarbonyl-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate in the presence of micromolecular alcohol, ether, ketone and nitrile the carbon atoms of which are below C8 and are used as additives. According to the method, special additives are added before acylation so that cyclopropanecarboxylic acid chloride can directly react with intermediate-state 3-ethoxycarbonyl-5-oxo-cyclohexane-1-enol sodium salt to obtain the trinexapac-ethyl precursor 3-ethoxycarbonyl-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate, thereby shortening reaction time, simplifying synthesis process and improving yield; and the product is directly rearranged without purification so as to obtain the final product trinexapac-ethyl.

The invention discloses an Al-18F mark fusion peptide and an application thereof. The Al-18F mark fusion peptide comprises glioma specific targeted polypeptides cRGDyK and A7R connected together. The preparation method comprises the following steps: (1) preparing NOTA-PEG-RGDyK-Lys-Ac-A7R; (3) preparing 18F physiological saline liquor; (3) preparing [Al18F]NOTA-PEG-RGDyK-Lys-Ac-A7R; and (4) purifying the prepared [Al18F]NOTA-PEG-RGDyK-Lys-Ac-A7R to obtain the Al-18F mark fusion peptide. The Al-18F mark fusion peptide disclosed by the invention comprises glioma specific targeted polypeptides cRGDyK and A7R connected together, and the specificity of the fusion peptide on glioma is further improved by means of different targeted biological characteristics.

The invention relates to a method for preparing asenapine shown in a general formula (11) and an intermediate shown in a general formula (8) and used for preparing asenapine. The general formulas are shown in the specification. The method comprises the following steps: obtaining a compound shown in a general formula (9) through ring-closure reaction of the compound shown in the general formula (8); obtaining a compound shown in a general formula (10) through reduction reaction of the compound shown in the general formula (9); obtaining asenapine shown in the general formula (11) through substitution reaction of the compound shown in the general formula (10), wherein in the general formula (8), R1 represents halogen, preferably chlorine or bromine.

The invention discloses a phosphorus-containing polyurethane acrylate oligomer, and a preparation method and an application thereof. The preparation method comprises the following steps: adding hydroxy acrylate and dibutyltin dilaurate to diisocyanate in a dropwise manner, controlling the reaction temperature, and monitoring the concentration change of -NCO in a system to obtain a semi-adduct of diisocyanate; dissolving polyol in toluene, adding an acylchloriration agent phosphorous oxychloride in a dropwise manner, and reacting to obtain cyclic phosphate B; and heating the cyclic phosphate B, the semi-adduct of diisocyanate and a polymerization inhibitor, adding a catalyst dissolved in acetone in a dropwise manner, and reacting to obtain phosphorus-containing annular structured polyurethane acrylate. The above product can be applied in photoimageable components. Introduction of an annular phosphate group in the design process of a molecular structure increases the adhesion of a dry film photoresistive resist on a metal substrate; and the method has the advantages of simple synthesis route, few side reactions, no pollution, and obtaining of the product with good performances without purification.

The invention relates to a method for preparing asenapine shown in a general formula (9) and an intermediate shown in a general formula (7) and used for preparing asenapine. The general formulas are shown in the specification. The method comprises the step that asenapine shown in the general formula (9) is obtained through ring-closure reaction of a compound shown in a general formula (8).

The invention discloses a method for recycling bivalent manganese in electrolytic manganese leached residues. The method comprises the following steps: using water to carry out counter-current rinsing on the electrolytic manganese leached residues through a filter press to obtain a manganese-containing feed liquid, and detecting the content of the bivalent manganese; adding precipitating agent sodium carbonate to the manganese-containing feed liquid, so as to generate precipitate; carrying out pressure filtration after precipitation to obtain filtrate and filter residue containing manganese carbonate; detecting the content of the manganese carbonate in the filter residue containing the manganese carbonate, directly using the filter residue to prepare a manganese sulphate solution when the Mn(2+) of the manganese carbonate in the filter residue is not less than 80%, and re-precipitating the filter residue when the Mn(2+) of the manganese carbonate in the filter residue is less than 80%. The method has the advantages of being simple to operate, safe, low in production cost, and being suitable for industrial production; and moreover, the Mn(2+) in the electrolytic manganese leached residue is sufficiently recycled, thereby the harm caused due to the fact that the soluble metal Mn (2+) enters the natural environment is reduced and the wastes of a manganese resource is reduced; and besides, the content of Mn(2+) in the recycled manganese carbonate is high and more than 80%, and the recycled manganese carbonate can be directly used for preparing the manganese sulphate solution.

The invention discloses a noncellular synthetic biology based preparation method of 2-phenylethanol and an application. According to the preparation method and the application, three recombinases including ARO8, ARO10 and ADH1 are utilized to constitute a co-reaction system, and a complicated metabolic process of an Ehrlich pathway requiring multi-step continuous reaction and multi-enzyme participation for synthesis of 2-phenylethanol in microorganisms is simplified to be performed in the same reaction system in vitro, so that the environmental pollution is reduced and the reaction process is shortened. Furthermore, the three recombinases are subjected to carrier-free co-immobilization with glutaraldehyde serving as a cross-linking agent, Combi-CLEAs (Combi-Cross-linked Enzyme Aggregates) are prepared, a target product is synthesized in vitro, accordingly, the enzymes are further recycled on the basis of the beneficial effects, and the production cost is reduced; the preparation method fills up the technical blank of multi-enzyme preparation of 2-phenylethanol in vitro, and important reference is provided for biological preparation of 2-phenylethanol.

The invention relates to a method for preparing high purity surface active agent used for papermaking industry. By intra-molecular structure design, the content of isooctyl alcohol in succinic acid bi-alkyl SEDSS surface active agent is controlled, thus adjusting the hydrophilicity and penetrability of the surface active agent and surface tension of coatings, meeting the need of papermaking industry and promoting the development of the papermaking industry. The preparing method has the advantages of simple preparation, no need of decompression distillation purification after esterification, no need of taking inert gas as protective gas in sulfonation reaction, no need of adding phase transfer catalyst, no time wasting or labor force wasting and that the production cost of the surface active agent is reduced; the prepared succinic acid bi-alkyl SEDSS has the advantages of high purity, less by-product, no need of purification, cheap and easily obtained materials of reaction, low toxicity and wide application prospect.

The invention embodiment provides a preparation method for graphene oxide, and relates to the technical field of material preparation. The method comprises the following steps: placing a carbon-containing carbon source which is used as an anode and an electric conductive material which is used as a cathode into electrolyte water, electrifying the anode and the cathode with a direct current for three minutes or more to obtain a graphene oxide solution, and performing drying treatment on the graphene oxide solution to obtain the graphene oxide. According to the invention, in the preparation method for the graphene oxide, the water is used as an electrolyte and free of pollution, the graphene oxide has good dispersion in the solution, impurities are less and purification is not needed, and the preparation process is simple.

The invention discloses a preparation method of a 24-epibrassinolide intermediate, and belongs to the field of chemical synthesis, and the preparation method comprises the following steps: 1) taking ergosterol as an initial raw material, carrying out methanesulfonylation under the catalysis of tetrabutylammonium hydrogen sulfate to obtain a first-step product, namely an intermediate 1, filtering afirst-step reaction solution, and directly carrying out a next-step reaction on a filtrate; 2) adding water and potassium bicarbonate into the filtrate obtained in the step 1), carrying out heating reaction, and carrying out split-phase water removal, concentration, cooling and filtration to obtain an intermediate 2; 3) reacting the intermediate 2 with benzyl halide in the presence of an acid-binding agent to generate an etherification product; 4) reacting the etherification product with tetrabutylammonium bromide and tetrabutylammonium hydrogen persulfate to obtain an intermediate 3; compared with a traditional CrO3/pyridine oxidation method, the method has the advantages that the use of an oxidizing agent containing heavy metal chromium and having serious pollution to the environment isavoided, the reaction conditions are mild, the yield is high, the post-treatment is simple, the next step of reaction can be performed without refining, and the method is suitable for industrial production.

The invention discloses a preparation method of a cuprous oxide nano material and hydrogen evolution performance of the cuprous oxide nano material, and belongs to the technical field of nanometer materials. According to the preparation method, ethylene glycol and diethylene glycol are used as reducing agents, copper hydroxide and basic copper carbonate with specific morphology are used as coppersources, and the copper hydroxide and the basic copper carbonate copper are reduced to form cuprous oxide nano material with maintained morphology under the protection of inert gas through a gas phasereduction method. The reaction steps are simple and are environmentally friendly, the obtained product does not need to be washed, and a pure cuprous oxide product can be obtained. According to the preparation method provided by the invention, the simple and rapid method is adopted for synthesizing the cuprous oxide nano material with the maintained morphology, and the prepared cuprous oxide nanomaterial has the performance of electro-catalytic hydrogen evolution.

The invention discloses a molecularly-imprinted nanoparticle for glycoprotein and a synthesis method thereof, belongs to the field of analytical chemistry, and relates to synthesis of molecularly-imprinted polymers. The synthesis method comprises the following steps: firstly, preparing a solution phase A from template glycoprotein molecules, preparing a solution phase B from a functional monomer and a cross-linking agent, and preparing solution phase C from an initiator; secondly, respectively fixing the solution phase A, the solution phase B and the solution phase C on three micro-fluidic injection pumps with adjustable flow rates, connecting and mixing the solution phase A and the solution phase B through a Y-shaped three-way valve, connecting and mixing the mixed solution and the solution phase C through another Y-shaped three-way valve, and enabling the obtained mixed solution and the solution phase C to flow into a reactor for a polymerization reaction; and finally, collecting a polymerized nanoparticle at the tail end of the reactor, and removing the glycoprotein template molecules to obtain the molecularly-imprinted nanoparticle for glycoprotein. The molecularly-imprinted nanoparticle for glycoprotein is prepared in a microfluidic mode, operation is easy, continuous production can be achieved, and the obtained molecularly-imprinted nanoparticle can be used for specific recognition of target glycoprotein molecules.

The invention discloses a method for large-scale preparation of high-efficiency red/near-infrared emission fluorescent carbon dots. The method comprises the following steps: o-phenylenediamine and aninorganic metal salt are ground into powder with uniform granules, the mixed powder of o-phenylenediamine and inorganic metal salt or a mixture of o-phenylenediamine and dilute hydrochloric acid is transferred to the lining of a reaction kettle, then packaged, and transferred to a drying oven, and the reaction temperature and reaction time are set, the temperature of the drying oven is cooled to room temperature after the reaction is completed, and the reaction kettle is taken out to obtain a product; and the product is washed and dried. Compared with the prior art, the method of the inventionhas the advantages of simple and convenient reaction, no purification, low cost, convenient mass production, good environmental stability, and convenient storage and transportation, and the preparedfluorescent carbon dots have excellent red fluorescence performance and four-photon fluorescence property, and realizes the fluorescence emission of the carbon dot in the near-infrared third window for the first time; and the carbon dot product can meet the fabrication requirements of various optoelectronic devices without complicated modification at the later stage.