39results about How to "Efficient reaction conditions" patented technology

The invention belongs to the technical field of preparation of selenium-containing polymers, and discloses a method for preparing polyselenourea / polyselenoamide through multi-component polymerizationof elemental selenium, isonitrile / alkyne and amine. The method comprises: carrying out a reaction on elemental selenium, a binary triple bond compound and a diamine in an organic solvent under an inert atmosphere, and subsequently treating to obtain a selenium-containing polymer, wherein the binary triple bond compound is binary isonitrile or binary alkyne, and the selenium-containing polymer is polyselenourea or polyselenoamide. According to the present invention, the method has characteristics of mild reaction conditions, high efficiency, energy saving, no catalyst, no by-product generation,atomic economy, green chemistry, low monomer toxicity, high atom utilization rate and high yield (more than or equal to 90%); the group has strong tolerance, and a variety of functional groups can beintroduced into the monomer; and the polyselenourea / polyselenoamide is stable, and can be degraded under specific conditions.

The invention relates to a method for synthesizing 6-hexose phosphate by employing an enzymic method. The method comprises the following steps: with hexose as a substrate, polyphosphates and / or triphosadenine salt as phosphate donors, putting a reactant into a pH buffer system; adding inorganic polyphosphoric acid hexokinase and cofactors to the buffer system; and synthesizing the 6-hexose phosphate under the catalysis action of the inorganic polyphosphoric acid hexokinase. Compared with a chemical method, the method for synthesizing the 6-hexose phosphate by employing the enzymic method is green and safe; compared with other methods for synthesizing the 6-hexose phosphate by other enzymic methods, the polyphosphates and / or triphosadenine salt can be used as phosphate donors by the inorganic polyphosphoric acid hexokinase disclosed by the invention. The triphosadenine salt with high cost is replaced with polyphosphates, so that the problem of high production cost is solved.

The invention discloses a highly-hyperbranched cationic polysaccharide derivative containing a dendritic polyamidoamine group and a preparation method of the highly-hyperbranched cationic polysaccharide derivative. The highly-hyperbranched cationic polysaccharide derivative containing the dendritic polyamidoamine group has a structural formula shown by a formula (I); and the highly-hyperbranched cationic polysaccharide derivative is synthesized by selectively coupling dendritic polyamidoamine (PAMAM D3 or D4) to a hyperbranched polysaccharide chain through an efficient nitrine-alkyne click reaction method. The preparation method disclosed by the invention is mild in reaction condition and has high reaction efficiency and selectivity at the same time. The prepared cationic polysaccharide derivative containing the dendritic polyamidoamine group has a characteristic of a highly-hyperbranched structure, can well form an electropositive nano-composite with siRNA, is favorable for carrying siRNA to enter cells, can improve the transfection efficiency of siRNA to genes, is expected to be used as a gene carrier and has a great prospect of application.

The invention belongs to the technical field of food processing and relates to sea worm seasoning and a manufacturing method thereof. The sea worm seasoning comprises, by weight parts, 70-105 parts of refined salt, 20-30 parts of natural yeast extract, 8-12 parts of clam nectar, 20-28 parts of youxiantai, 25-35 parts of white sugar, 4-6 parts of natural HVP, 0.3-0.6 part of allicin, 20-30 parts of corn starch, 12-18 parts of bonito powder, 6-12 parts of sea worm juice and 0.4-0.8 part of sodium glutamate and further comprises 60-120 parts of sauce. The sea worm seasoning is in a powder or sauce shape. The sea worm powder is formed by raw material pretreatment, enzymolysis, reaction and spray drying; and the sea worm sauce is formed by raw material pretreatment, mixing, reaction and forming. The product is free of any abnormal smell and fishy smell and is particularly outstanding in delicious taste; all natural young seafood raw materials are adopted, no chemical substance is added in the production process, and the sea worm seasoning is all natural and healthy.

The invention discloses a preparation method of an alpha, alpha-di-substituted iso-chroman compound. The alpha,alpha-di-substituted iso-chroman compound is obtained by directly synthesizing a raw material alpha-monosubstituted iso-chroman compound, which is diverse in structure and easy to synthesize, and nitromethane in one step. The method has the advantages of short reaction steps, mild reaction conditions, high efficiency and simple operation. According to the preparation method, the C-H bond on the alpha-site carbon of the alpha-mono-substituted iso-chroman compound can directly form theC-C bond, so that the use of an intermediate in a redundant synthesis step is avoided, which is consistent with the concept of green synthetic chemistry of economy and sustainable development of atomspursued at present. The prepared alpha, alpha-disubstituted iso-chroman compound can be subjected to a series of chemical conversion to generate various substituted iso-chroman derivatives; the method has great application potential in preparation of medicines and active natural products.

The invention relates to a method for preparing aromatic monomers by virtue of bi-oxidation degradation of lignin. The method comprises the following steps: suspending lignin, an oxidant and inorganicacid in a molten salt hydrate according to the mass ratio and uniformly stirring , and reacting for 0.5 to 5 hours at 90 to 150 DEG C; after a reaction solution is cooled, suction filtering, and washing for 3 to 4 times; placing the reaction solution in 20mL of hydrogen peroxide, reacting for 5 to 24 hours at 20 to 80 DEG C, after the reaction solution is cooled, extracting and degrading a product by using ethyl acetate, removing the organic solvent in a rotary evaporating manner, vacuum drying to obtain a lignin monomer compound. The method is mild in reaction condition, rapid and efficientin reaction, and capable of efficiently degrading the lignin by breaking an ether bond (beta-O-4) and a carbon-carbon bond (Calpha-Cbeta) of the lignin; and the highest yield of the lignin monomer compound can reach 80 percent.

The invention relates to non-animal-derived LMW (low molecular weight) heparin, a preparation method therefor and application of the non-animal-derived LMW heparin. The preparation method disclosed bythe invention comprises the steps of performing a one-step chemical method and a variety of enzyme catalysis methods in order: extracting an exopolysaccharide K5CPS, subjecting the exopolysaccharideK5CPS to chemical-method N-deacetylation / N-sulfation modification, and then, carrying out partial depolymerization in a buffer solution through heparinase III; and subjecting obtained LMW products toenzyme-method C-5 epimerization / 2-O-sulfation modification, 6-O-sulfation modification and 3-O-sulfation modification sequentially, thereby obtaining a product with anti-FXa and anti-FIIa activity. The invention provides a novel method for preparing the LMW product with typical structure characteristics of the heparin and remarkable anticoagulation activity. According to the method, raw materialsare non-animal-derived, the quality is controllable, the risk of contamination is low, adopted reaction conditions are mild and efficient, the obtained product is easy to separate, and large-scale preparation of the LMW heparin with good structural homogeneity and high anticoagulation activity can be achieved.

The invention belongs to the field of nitrate reduction in water, and particularly relates to a nitride catalyst for efficient photocatalytic reduction of nitrate in water and a water treatment methodthereof. The method comprises the following steps of preparing the nitride catalyst for the photocatalytic reduction of the nitrate in the water by adopting different methods; putting the prepared catalyst into nitrate-containing industrial wastewater to be treated, and conducting photocatalytic reduction of the nitrate in the water under ultraviolet light irradiation. The catalyst for the photocatalytic reduction of the nitrate in the water is a nitride type, and includes transition type nitride, covalent type nitride, nitride of different morphologies, defect nitride, nitride loaded with ametal and a metal quantum dot, a composite of nitride and a metal oxide and nitride loaded on different carriers. The method has the advantages of simple equipment, easy control, mild reaction conditions and the like; the prepared nitride catalyst can efficiently and stably remove the nitrate in sewage, and have good stability.

The invention belongs to the technical field of tissue engineering, and discloses a method for building a biological activity gel film layer on the surface of a biological material containing alkynyl.The method comprises the following steps that (1) performing reaction on a high molecular material containing alkynyl and biological active macromolecules containing azide groups to obtain a high molecular material with biological active macromolecules; (2) performing reaction on the biological active macromolecules containing alkynyl and a high molecular material bonded with biological active macromolecules to obtain a high molecular material bonded with an active layer; (3) repeating the step (1) or the steps (1) to (2) to obtain the high molecular materials bonded with active layers with different thickness on the surface; (4) performing reaction on micromolecules containing azide groups or alkynyl and the high molecular materials in the step (3) to obtain a product. The method provided by the invention is simple, flexible and efficient; the reaction conditions are mild; the thickness of the biological active layer can be controlled; no limitation exists on the material form morphological structure; the application range is wide; the combination of the biological active layer and the high molecular materials is stable and firm.

The invention discloses a bamboo sprout amino acid preparation method. Bamboo sprouts and / or other processing leftovers of the bamboo sprouts are used as raw materials of bamboo sprout amino acid. The method specifically comprises the steps that firstly, the raw materials are sliced or smashed; secondly, the raw materials are subjected to an enzymatic reaction through compound enzymes containing protease or other enzymes to promote proteolysis, wherein the dosage of the protease is 50-500 AU / g, the dosage of the other enzymes is 10-1000 AU / g, and the other enzymes are one or two kinds of amylase, lipase, beta glucanase, xylanase, mannanase, cellulose, pectase and phytase; amino acid is extracted from the raw materials which are subjected to enzyme treatment and then subjected to water immersion, filtration membrane concentration and mist spraying in sequence, and amino acid extracts contain 20%-80% of the amino acid. By means of the method, the content of free amino acid and the content of oligo-peptide matter in the raw materials are remarkably increased, and the yield and the extraction efficiency are improved. Products such as the bamboo sprout fragrance seasoning packets, tartar sauce, sauce solution and nutrition powder can be prepared with bamboo sprout amino acid as a main ingredient.

The invention belongs to the technical field of organic chemistry, and discloses a polyacetylenic compound and a preparation method thereof. The method comprises the following steps: (1) under the protection of an inert gas, mixing a diacetylene halide compound and a binary sulphonamide compound in a catalytic system and an organic solvent, reacting, and cooling to obtain a reaction mother liquid; (2) adding the reaction mother liquid into a precipitator for precipitating, collecting a precipitated, and drying to constant weight to obtain a polyacetylenic compound. The preparation method disclosed by the invention is simple; the reaction is efficient; the group tolerance is high; a plurality of functional groups can be intruded into monomers; the prepared polyacetylenic compound contains a carbon-carbon triple bond, and has important application to serving as an intermediate in a further reaction; moreover, the compound is easy to hydrolyze, and has a very promising prospect in the aspects of environmentally friendly chemistry, green chemistry and the like, such as a degradable material.

The invention belongs to the field of organic synthesis, and particularly relates to a method for synthesizing cyclic carbonate and derivatives thereof, which comprises the following step of: reactingan epoxy compound shown in a formula I with carbon dioxide under the catalysis of a catalyst shown in a formula II to obtain a target product. The product prepared by the method has the advantages ofhigh yield, high purity, low catalyst cost and mild synthesis conditions, and the obtained product has no metal residue.

The invention provides a method for preparing glycyrrhetinic acid through biological catalysis of novel glucuronidase. The method comprises the following steps of screening and expressing novel recombinant glucuronidase through a genetic engineering means; by taking glycyrrhizic acid as a substrate, performing a catalytic reaction to obtain the glycyrrhetinic acid with higher purity; incubating beta-glucuronidase and Fe3O4@Zr-2MIm in a phosphate buffer solution environment to obtain an immobilized enzyme; and carrying out a catalytic reaction on the immobilized enzyme and the glycyrrhizic acidto obtain the glycyrrhetinic acid. The beta-glucuronidase screened out in the method is high in catalytic activity; the glycyrrhizic acid can be rapidly and completely converted within 2 hours, and an intermediate product glycyrrhetinic acid monoglucuronide cannot be generated; and the high-purity glycyrrhetinic acid can be conveniently obtained. Meanwhile, the immobilized enzyme can be recycled,so that the production cost is reduced; and the process is simple, economic and very suitable for large-scale industrial production. The conversion rate of the glycyrrhizic acid by the immobilized enzyme reaches 95% or above, and the substrate glycyrrhizic acid is basically and completely converted into the glycyrrhetinic acid.

A lignin depolymerization method comprises the following steps: suspending 2 g of lignin and 0.2-1.2 g of a catalyst in 20 mL of a molten salt hydrate in a mass ratio, performing uniform stirring, andreacting the obtained mixture at 90-150 DEG C for 0.5-5 h; and cooling the obtained reaction solution, performing suction filtration, performing water washing 3-4 times, and performing vacuum dryingto obtain a degradation product. The method has the advantages of mild reaction conditions, quick and high-efficiency reacting, effective degradation of beta-O-4 bonds in lignin, and realization of cost reduction and environmental protection by resin acid and the molten salt hydrate.

The invention discloses a solid acid catalyst. Commercial TiO2 (titanium dioxide) serving as a matrix is immersed by using an ammonium persulfate solution and roasted at a high temperature, so that S2O8<2-> / TiO2 is prepared. The catalyst has a certain acid content, has high-efficiency performance for catalyzing alcoholysis ring-opening reaction styrene oxide at a room temperature; the solid acid catalyst is simple in preparation, and has reusability; a raw material is easily available. The solid acid catalyst belongs to one kind of ring-opening reaction catalysts which is environment-friendly and easy to industrialize.

The invention discloses a preparation method of a coupling aromatic compound, which comprises the following steps of taking non-functional aromatic hydrocarbon and / or halogenated aromatic hydrocarbon as a raw material, taking an oxime ether cyclopalladated complex as a catalyst, reacting for 6-48 hours in an organic solvent at a temperature of 100-160 DEG C under the inert atmosphere under the action of alkali, and post-processing reaction liquid after the end of reaction to obtain the coupling aromatic compound. The oxime ether cyclopalladated complex is a complex formed by reacting metal palladium salt with an organic nitrogen ligand in a methanol solvent at a room temperature; and the metal palladium salt is lithium tetrachloropalladate; and the organic nitrogen ligand is 4-hydroxy acetophenone oxime. The preparation method has the beneficial effects that when the oxime ether cyclopalladated complex is selected as the catalyst to replace a traditional palladium / phosphorus composite catalyst, the reaction condition can be milder and more efficient, so that the use of the ligand is greatly reduced; and the halogenated aromatic hydrocarbon which is lower in activity and cost and is easily obtained can also be used as a substrate in the reaction.

The invention discloses an alkyne-containing quinoxalin derivative and a preparation method thereof. The structure general formula of the alkyne-containing quinoxalin derivative is shown in the specifications, wherein R is aryl, alkyl, trimethylsilyl or halogen alkyl; and R' is hydrogen, halogen, aryl or alkyl. The preparation method comprises the following steps of: putting terminal alkyne and an o-phenylenediamine compound serving as raw materials and CuX serving as a catalyst into a sealed pipe; reacting with magnetic stirring to obtain a crude product; and performing silica gel column chromatography to obtain the alkyne-containing quinoxalin derivative. Compared with the prior art, the invention has the advantages: the raw materials of the product are cheap and readily-available, and the method is easy to operate and control and has mild reaction conditions, high efficiency and low environmental pollution.

The invention discloses a supported cyclometalated iridium catalyst, a preparation method thereof and application of the supported cyclometalated iridium catalyst in dehydrogenation reaction of dihydroindolines compounds; the catalyst is loaded with a pyrene-loaded cyclometalated iridium complex by taking a multiwalled carbon nanotube as a carrier; in the cyclometalated iridium complex, an iridium atom is taken as a coordination center and 4-methoxy-n-[1-(4-hydroxyphenyl)]-phenylamine and pentamethylcyclo penta dience as ligands. The catalyst disclosed by the invention is simple in preparation method and short in preparation cycle and is capable of realizing the dehydrogenation reaction of the dihydroindolines compounds in green solvent (mixed solvent of water and trifluoroethanol); the reaction condition is mild, safe, green and efficient; the catalyst disclosed by the invention can be recovered through simple centrifugal separation, and the excellent catalytic performance of the catalyst is still kept after the catalyst is reused for multiple times.

The invention discloses a dynamic and static combined stirring system. The system comprises a stirrer and further comprises a plurality of static stirring paddles parallel to a stirring shaft of the stirrer, the static stirring paddles are arranged around the stirring shaft, and stirring blades are installed at the bottom of the stirring shaft. In addition, the invention further discloses a process for preparing a chromium salt through chromite liquid phase oxidation by adopting the dynamic and static combined stirring system. The invention provides a novel process for preparing a chromium salt by using the chromite liquid phase oxidation method, the key process problems of solid-liquid separation in the chromite leaching process, separation of the chromium salt in a high-alkali medium andconversion of an intermediate product into a series of chromium salts are innovatively solved, and the method has a great industrial application prospect.

The invention discloses a catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol, and its preparation method. The preparation method comprises the following steps: adding Cr(NO3)3.9H2O, HF and terephthalic acid into deionized water, then adding into a hydrothermal reaction vessel to react for 7-9 hours at the temperature of 210 DEG C-230 DEG C; cooling to the room temperature and filtering, vacuum drying to obtain an activated organometallic framework structure material; taking the framework structure as a carrier, loading the reduction state metal Pd nano particles to obtain a catalyst for one-step preparing cyclohexanone by hydrogenation of water phase phenol; the catalyst possesses two functions of Lewis acid sites and hydrogenation active sites. The preparation method of the invention has the characteristics of environmental protection, mild reaction condition, high activity and selectivity, good stability, simple products separation and the like. Thepreparation method for the catalyst is simple, and a reaction solution and the catalyst are easy to separate.

The invention discloses a preparation method of cross-linking enzyme. The preparation method comprises the following steps: mixing polyphenol oxidase with a glutamine transaminase solution for a reaction; the cross-linked enzyme microparticles with a particle size of several micrometers to tens of micrometers and different vigor sizes can be obtained,the cross-linked glutamine transaminase prepared by the method can be separated from a solution by means of filtration, centrifugation and the like, and the prepared cross-linked glutamine transaminase is used for polyethylene glycol (PEG) modification and the like of protein drug molecules. The cross-linked glutamine transaminase is easy to recover and can be repeatedly used in the use process, no burden is caused to product separation, and the production cost is greatly reduced. According to the method, the crosslinking process is environmentally friendly, mild and efficient, the reaction is controllable, a carrier is not needed, glutamine transaminase does not need to be purified, and multiple enzymes can be crosslinked and immobilized together.

The invention discloses a preparation method of a coupling aromatic compound, which comprises the following steps of taking non-functional aromatic hydrocarbon and / or halogenated aromatic hydrocarbon as a raw material, taking an oxime ether cyclopalladated complex as a catalyst, reacting for 6-48 hours in an organic solvent at a temperature of 100-160 DEG C under the inert atmosphere under the action of alkali, and post-processing reaction liquid after the end of reaction to obtain the coupling aromatic compound. The oxime ether cyclopalladated complex is a complex formed by reacting metal palladium salt with an organic nitrogen ligand in a methanol solvent at a room temperature; and the metal palladium salt is lithium tetrachloropalladate; and the organic nitrogen ligand is 4-hydroxy acetophenone oxime. The preparation method has the beneficial effects that when the oxime ether cyclopalladated complex is selected as the catalyst to replace a traditional palladium / phosphorus composite catalyst, the reaction condition can be milder and more efficient, so that the use of the ligand is greatly reduced; and the halogenated aromatic hydrocarbon which is lower in activity and cost and is easily obtained can also be used as a substrate in the reaction.

The invention belongs to the technical field of organic chemistry, and discloses a polyacetylenic compound and a preparation method thereof. The method comprises the following steps: (1) under the protection of an inert gas, mixing a diacetylene halide compound and a binary sulphonamide compound in a catalytic system and an organic solvent, reacting, and cooling to obtain a reaction mother liquid; (2) adding the reaction mother liquid into a precipitator for precipitating, collecting a precipitated, and drying to constant weight to obtain a polyacetylenic compound. The preparation method disclosed by the invention is simple; the reaction is efficient; the group tolerance is high; a plurality of functional groups can be intruded into monomers; the prepared polyacetylenic compound contains a carbon-carbon triple bond, and has important application to serving as an intermediate in a further reaction; moreover, the compound is easy to hydrolyze, and has a very promising prospect in the aspects of environmentally friendly chemistry, green chemistry and the like, such as a degradable material.

The invention discloses a ferrocene bonding chromatographic stationary phase and a preparing method thereof. The ferrocene bonding chromatographic stationary phase is obtained in the way that under the protection of inert atmosphere in an organic solvent, azodiisobutyronitrile is added dropwise to 3-mercaptopropyl silanized inorganic matrix microspheres and vinylferrocene to serve as the initiator, reaction is conducted for 18-36 h at 80-120 DEG C, and then cooling, filtration, washing and drying are conducted. The preparing process is simple, cost is low, reaction materials are easy to obtain and have wide sources, and the ferrocene bonding chromatographic stationary phase can be directly used without any modification; the prepared ferrocene bonding chromatographic stationary phase is a universal hydrophobic interaction chromatographic stationary phase, has high separation selectivity for most compounds, and has high application value and potential.

The invention belongs to the technical field of preparation of selenium-containing polymers, and discloses a method for preparing polyselenourea / polyselenoamide through multi-component polymerizationof elemental selenium, isonitrile / alkyne and amine. The method comprises: carrying out a reaction on elemental selenium, a binary triple bond compound and a diamine in an organic solvent under an inert atmosphere, and subsequently treating to obtain a selenium-containing polymer, wherein the binary triple bond compound is binary isonitrile or binary alkyne, and the selenium-containing polymer is polyselenourea or polyselenoamide. According to the present invention, the method has characteristics of mild reaction conditions, high efficiency, energy saving, no catalyst, no by-product generation,atomic economy, green chemistry, low monomer toxicity, high atom utilization rate and high yield (more than or equal to 90%); the group has strong tolerance, and a variety of functional groups can beintroduced into the monomer; and the polyselenourea / polyselenoamide is stable, and can be degraded under specific conditions.

The invention discloses a highly-hyperbranched cationic polysaccharide derivative containing a dendritic polyamidoamine group and a preparation method of the highly-hyperbranched cationic polysaccharide derivative. The highly-hyperbranched cationic polysaccharide derivative containing the dendritic polyamidoamine group has a structural formula shown by a formula (I); and the highly-hyperbranched cationic polysaccharide derivative is synthesized by selectively coupling dendritic polyamidoamine (PAMAM D3 or D4) to a hyperbranched polysaccharide chain through an efficient nitrine-alkyne click reaction method. The preparation method disclosed by the invention is mild in reaction condition and has high reaction efficiency and selectivity at the same time. The prepared cationic polysaccharide derivative containing the dendritic polyamidoamine group has a characteristic of a highly-hyperbranched structure, can well form an electropositive nano-composite with siRNA, is favorable for carrying siRNA to enter cells, can improve the transfection efficiency of siRNA to genes, is expected to be used as a gene carrier and has a great prospect of application.

The invention discloses a method for preparing cyclic ether through diol dehydration cyclization. The method comprises the following steps: carrying out a diol dehydration reaction in a temperature range of 50-200 DEG C by using an ionic liquid as a solvent and a catalyst to prepare cyclic ether. The ionic liquid catalytic system provided by the invention has the advantages of high efficiency, simplicity, mildness (120 DEG C), no metal participation and the like, can efficiently catalyze glycol dehydration to prepare cyclic ether, and has a relatively high industrial application value.

The invention provides a green synthesis method of an isoxazole compound as shown in a formula (III). The method comprises the following steps: by taking an aldoxime compound as shown in a formula (I) as a substrate, reacting with an alkyne compound as shown in a formula (II) at room temperature for 6-16 hours in an aqueous solution of a surfactant with the mass concentration of 1wt%-5wt% under the combined action of N-chlorosuccinimide and an alkaline substance, and carrying out post-treatment on the obtained reaction liquid to obtain the isoxazole compound as shown in the formula (III). According to the invention, water is used as a reaction solvent, so the usage amount of an organic solvent is reduced, and zero emission of the solvent is realized.