890 results about "Dichloromethane" patented technology

The invention discloses a crown ether grafted polyarylether sulfone ion separation membrane as well as a preparation method and application thereof, and belongs to the technical field of ion separation membranes, collaborative optimization is realized through crown ether accurate grafting and ultrathin ordered membrane formation: a main chain of polyarylether sulfone is grafted with 4 '-aminobenzo-12-crown-4 to form an inherent channel adapted to Li, and the specific surface area of the main chain is increased; the ultrathin film is prepared by a water surface spreading method, and the ion transmission path is shortened. Finally, in a LiCl / MgCl system, Liion flux has high selectivity, high permeation-high selectivity cooperation is preliminarily realized, the chemical synthesis step can be amplified to a kilogram level, and after a DPAES-g-CE / dichloromethane solution is dropwise added to the water surface, the DPAES-g-CE / dichloromethane solution is rapidly spread to form a film without precise equipment; the raw materials are industrial-grade monomers and have no toxic residues, the membrane can be recycled and reused through dichloromethane, the equipment cost is reduced by about 90%, and industrialization is easy; the main chain of the polyaryl ether sulfone is high in rigidity and resistant to high temperature and chemical corrosion; crown ether grafting avoids molecular chain agglomeration, and the swelling rate is far lower than that of a traditional sulfonated membrane.

The invention relates to the technical field of repair materials, and particularly discloses an extracellular matrix fiber material as well as a preparation method and application thereof. The invention discloses a preparation method of an extracellular matrix fiber material. The preparation method comprises the following steps: taking animal tissues, and carrying out virus inactivation, decellularization and antigen removal, degreasing, drying, grinding and sterilization; the decellularization and antigen removal method comprises the following specific steps: sequentially soaking a sample with a surfactant solution for h; then, soaking treatment is carried out by adopting a salt-alkali solution which contains 0.05-3 mol / L of salt and has the pH value of 8-11; then carrying out soaking treatment by adopting a 0.1-1wt% enzyme solution; and in degreasing, one or more of normal hexane, trichloromethane, dichloromethane, methanol, ethanol, acetone, diethyl ether and ethyl acetate are used for soaking the sample. According to the technical scheme, the ECM powder particle material with high growth factor content is prepared.

The invention relates to the technical field of fine chemical engineering and flame retardant preparation, and discloses a preparation method of bromo-triazine capable of improving thermal stability, and the preparation method comprises the following steps: mixing phenol, water and dichloromethane, controlling the temperature, and carrying out oxidative bromination reaction to prepare an organic phase containing tribromophenol; then, under the action of an organic amine catalyst, carrying out condensation reaction on the organic phase, liquid caustic soda and cyanuric chloride; after the reaction, washing with water to remove impurities; and in the presence of process water, firstly controlling the temperature at 38-42 DEG C for azeotropic desolvation, then raising the temperature to 85-95 DEG C for high-temperature crystallization and crystal growing, and finally cooling, filtering and drying to obtain the bromo-triazine product. By utilizing the high selectivity of the organic amine catalyst and a two-stage azeotropic crystallization process, the side reaction is effectively reduced, the solvent wrapped in the crystal is eliminated, the prepared product is high in main content and extremely low in volatile component, the temperature can reach 370 DEG C or above when the thermal weight loss is 2%, and the thermal stability is remarkably improved.

The invention belongs to the technical field of lithium / sodium batteries, and particularly relates to a method for pre-embedding lithium / sodium into a battery. The preparation method comprises the following steps: firstly, preparing a lithium / sodium pre-embedded material of the lithium / sodium battery, namely putting a sodium salt of the material into an organic solvent, dropwise adding acid, stirring for reaction, extracting and drying, and evaporating the solvent to dryness; placing the product in deionized water, adding lithium salt, stirring for reaction, and evaporating the solvent to dryness; recrystallizing the solid by using ethyl acetate and dichloromethane; and drying the obtained solid powder to obtain a final material. Dissolving the prepared lithium / sodium pre-intercalation material in a battery electrolyte to realize lithium / sodium pre-intercalation of the battery; the sodium salt of the material takes organic sodium sulfinate as a skeleton, and side groups are substituted with different alkyl groups or aryl groups; the prepared lithium / sodium pre-embedded material is high in specific capacity, good in compatibility with a battery system and good in material stability; lithium / sodium pre-embedding is carried out on the battery through an electrolyte adding method, the lithium / sodium pre-embedding process is safe and convenient, the process is simple, the cost is low, and large-scale production can be realized.

The invention relates to the technical field of organic synthesis, in particular to a method for constructing Orforglipron tetrahydropyran ring chirality through enzyme catalysis, which comprises the following steps: step S1, taking SM1 as a raw material, and carrying out hydrolysis resolution in a solvent, a buffer salt system and enzyme catalysis to obtain a chiral pure intermediate INT-1; step S2; performing ring closing on the INT-1 through Grignard reaction to synthesize a lactone intermediate; s3, carrying out Diball-H reduction, quenching, dichloromethane extraction and anhydrous sodium sulfate drying on the INT-4, and then reducing the INT-4 by using triethyl silane to obtain an intermediate INT3; step S4, coupling the INT-3 in the presence of a catalyst and a ligand to obtain an intermediate INT-4; step S5, carrying out deprotection and salification on the INT-4 to obtain an intermediate INT5; s6, closing an indole ring from INT5 to obtain a compound of which the general formula is A; chirality is constructed through enzyme catalysis, isomer impurities do not need to be split and separated through SFC when the chirality is constructed, the loss is reduced, the yield is increased, and a target product is obtained with high chiral selectivity; meanwhile, the cost is relatively reduced, and the cost is saved.

The invention belongs to the technical field of organic synthesis, and provides a preparation method of a cationic lipid compound, which comprises the following steps: (1) reacting 1, 5-dihalopentane, 2-tert-butyl glycolate and alkali to obtain a product G; (2) hydrolyzing the product G under an acidic condition to obtain a product H; (3) carrying out esterification reaction on the product H, the raw material C, 4-dimethylaminopyridine and a condensing agent in dichloromethane to obtain a product J; and (4) carrying out amination reaction on the product J, the raw material L and alkali in acetonitrile to obtain the cationic lipid compound. Compared with the prior art, the method has the relatively remarkable advantages that when the first part of halogenated long-chain alkyl ester H is synthesized by the method, 1, 5-dihalopentane and 2-tert-butyl glycolate are used as raw materials, the halogenated long-chain alkyl ester J is synthesized by a simple method, the product is obtained at a higher yield in synthesis, and the method is suitable for kilogram-level production. The route synthesis only comprises four steps of chemical reactions, and is suitable for industrial production.

The invention discloses cyclodextrin alkyl ether sulfonic acid as well as a preparation method and application thereof, and relates to the technical field of oil and gas field auxiliaries. The preparation method of the cyclodextrin alkyl ether sulfonic acid comprises the following steps: adding hydroxyl alkyl sulfonic acid into dichloromethane, adding alkali and a sulfonyl chloride reagent, and reacting for 3-5 hours to obtain sulfonate; the preparation method comprises the following steps: adding sulfonate into iodide, adding acetone, reacting for 5-8 hours, and removing excessive iodide after the reaction is finished, so as to obtain iodo-hydrocarbyl sulfonic acid; the preparation method comprises the following steps: dissolving cyclodextrin in tetrahydrofuran, cooling to 0 DEG C, adding alkali under the protection of nitrogen, reacting for 0.5-2 hours, then adding iodo-alkyl sulfonic acid, reacting for 30-60 hours at room temperature, cooling to 0 DEG C, and carrying out reduced pressure distillation to obtain cyclodextrin alkyl ether sulfonic acid; the cyclodextrin alkyl ether sulfonic acid prepared by the invention is used as a cosolvent of the powder resistance-reducing agent, can effectively prevent aggregation among molecules of the powder resistance-reducing agent, improves the dispersity, reduces agglomeration and precipitation phenomena, and meanwhile, can avoid pipeline blockage in a conveying process.

The invention provides a silicon-phosphorus-containing macromolecular flame retardant, flame-retardant low-dielectric polycarbonate containing the flame retardant and a preparation method of the flame-retardant low-dielectric polycarbonate. The preparation method comprises the following steps: mixing and dissolving dichloromethane, triethylamine, bisphenol containing an R structure and bis (aminopropyl)-terminated siloxane to prepare a solution A; dissolving isophthaloyl dichloride and / or paraphthaloyl dichloride and phenylphosphoryl dichloride in dichloromethane to prepare a solution B; dropwise adding the solution B into the solution A, stirring and reacting, and then carrying out end capping treatment to obtain the silicon-phosphorus-containing macromolecular flame retardant. The flame-retardant low-dielectric polycarbonate containing the flame retardant has the advantages of high flame retardance, low dielectric constant and low loss, can meet the flame-retardant requirement of UL 94V-0 level under the condition that the thickness is 0.8-3.2 mm, and belongs to a halogen-free flame-retardant environment-friendly high polymer material.

The present invention relates to the technical field of organic synthesis, and specifically relates to a method for constructing the chirality of a pyran ring in Orforglipron by means of enzymatic catalysis, the method comprising the following steps: step S1, by using SM1 and SM2 as starting materials, carrying out a reaction under the action of a palladium catalyst and a ligand to obtain INT-1; step S2, under the catalysis of Pd / C, subjecting INT-1 to double bond hydrogenation reduction to obtain INT-2; step S3, in the presence of a solvent, a buffer salt system and enzymatic catalysis, subjecting INT-2 to hydrolysis and resolution to obtain a chirally pure intermediate INT-3; step S4, subjecting INT-3 to a Grignard reaction for cyclization, so as to synthesize a lactone intermediate INT-4; and step S5, subjecting INT-4 to reduction by means of Dibal-H, quenching same, performing extraction with dichloromethane, drying same with anhydrous sodium sulfate, and then performing reduction by means of triethylsilane to obtain a compound of general formula A. In the present invention, the chirality is constructed by means of enzymatic catalysis without the need of SFC resolution for separating isomeric impurities during the construction of the chirality, thereby reducing losses and improving yield, obtaining the target product at high yield and high chiral selectivity, and further saving expenses and reducing costs.

The invention discloses a crystal compound, a preparation method thereof and application of the crystal compound in X-ray detection, imaging and anti-counterfeiting encryption, and belongs to the technical field of crystals. The molecular formula of the crystal compound is [Cu (totp) (CH3CN) 3] [Cu2I3 (totp) (PN)]. (CH3CN), wherein totp is tris (o-tolyl) phosphine; and PN is diphenyl-2-pyridine phosphine. The crystal compound disclosed by the invention is simple in preparation method, and has the characteristics of large mass attenuation coefficient of X-ray energy, high light yield and low detection limit when being used as a material of an X-ray detector. The compound also has the characteristic of structural transformation in solvents such as methanol, ethanol, acetone, dichloromethane, tetrahydrofuran and the like, and meanwhile, the conversion of luminescence color under the excitation of 365nm ultraviolet light and X rays is accompanied. The material can be applied to the aspects of scintillator materials, room-temperature X-ray radiation indirect detection materials, radiation detection dosimeters, X-ray scintillator medical imaging, anti-counterfeiting encryption and the like.

The invention relates to the technical field of waste gas treatment, and particularly discloses waste gas treatment liquid for treating large-air-volume low-concentration waste gas through a water-based method. The waste gas treatment liquid for treating the large-air-volume low-concentration waste gas through the water-based method comprises a surfactant, a defoaming agent, a dissolution accelerant and water. Wherein the surfactant can be selected from any one or more of polyoxyethylene alkyl ether, polyoxyethylene alkyl ether and polyoxyethylene fatty acid ester; the dissolution accelerant can be selected from any one or more of ethylene glycol monobutyl ether, diethylene glycol monobutyl ether and triethylene glycol monobutyl ether; the defoaming agent is any one or more of butanol, dimethyl silicone oil, silicone and polyether modified polysiloxane. When the waste gas absorption liquid obtained in the invention is used for treating waste gas, the absorption efficiency of methanol, butanol, benzene, toluene, xylene, ethyl acetate, dichloromethane and acetone is obviously improved, and the absorption efficiency of the waste gas absorption liquid on aromatic hydrocarbon, halogenated hydrocarbon, alcohol, ketone and ester pollutants is improved.

The invention relates to the technical field of lithium / sodium ion batteries, in particular to a preparation method of a highly graphitized coated carbon material based on phenolic resin, which comprises the following steps: uniformly mixing formaldehyde, resorcinol and a basic catalyst, and then catalyzing and curing; carrying out carbonization treatment on the uncarbonized phenolic resin based on a gradient heating method; mixing ethidene diamine, dichloromethane and carbonized phenolic resin, and heating in an oil bath; and placing the cured and coated graphitized phenolic resin in a tubular furnace for highly graphitizing. According to the preparation method of the highly-graphitized coated carbon material based on the phenolic resin, high ordering of a carbon layer is achieved through gradient heating graphitization, a carbon six-membered ring plane is promoted to expand, an ABAB stacked graphite structure is formed, the conductivity is effectively improved, a CVD coating and nitrogen doping synergistic technology is combined, a CVD reaction is formed through ethanediamine and dichloromethane, and the high-graphitization coated carbon material based on the phenolic resin is obtained. Functional groups such as pyridine-N and graphite-N are introduced to the surface of the carbon layer, so that the interface bonding force between the carbon layer and the matrix is enhanced, and the conductivity of the carbon layer is further improved.

The invention discloses a preparation method of ethyl 4-chloroacetoacetate, and belongs to the technical field of compound synthesis. The method comprises the following steps: by taking diketene as a raw material, adding a polymethylsilsesquioxane polymerization inhibitor into a dichloromethane solvent, introducing chlorine at low temperature, carrying out chlorination reaction to generate 4-chloroacetoacetic acid, then esterifying the 4-chloroacetoacetic acid with absolute ethyl alcohol to obtain a crude product, and finally distilling and purifying to obtain the product. The preparation method is characterized in that a polymethylsilsesquioxane polymerization inhibitor is added before chlorination reaction, the polymerization inhibitor is prepared by grafting a functional monomer containing a 3, 5-di-tert-butyl-4-hydroxycinnamic acid structure onto surface-ethenylated polymethylsilsesquioxane microspheres, and the polymethylsilsesquioxane polymerization inhibitor has both steric hindrance and free radical capture capability. The method can effectively inhibit the self-polymerization and copolymerization tendency of diketene, intermediates and products in a reaction system, obviously reduces the generation of by-products such as dichloro and polychloro, enables the product to be high in yield and good in purity, and meets the quality requirements of high-end medical intermediates.

The invention discloses a preparation method of hippocampus oil, which comprises the following steps: 1) adding dried hippocampus powder into a dichloromethane-methanol mixed solution, uniformly stirring, and extracting for 24 hours; 2) filtering the leach liquor, adding water, fully and uniformly mixing, standing for 12 hours, and collecting a lower layer organic phase; 3, the organic phase is subjected to rotary evaporation drying.The invention further discloses application of the hippocampus oil in preparation of uric acid lowering products.The hippocampus oil is rich in omega-3 polyunsaturated fatty acid (EPA and DHA), the activity of xanthine oxidase is moderately reduced, release of inflammatory factors is inhibited, and the comprehensive effect of inhibiting generation and relieving inflammation is achieved.

The invention belongs to the technical field of hydrophobic electromagnetic shielding materials, and particularly relates to an asymmetric electromagnetic shielding composite film and a preparation method and application thereof. The PNTs are polypyrrole nanotubes, after Na2MoO4. 2H2O and CH4N2S are added and subjected to a high-temperature reaction, a MoS2 flower-shaped shell structure can grow on the PNTs, the layered structure and the high specific surface area of MoS2 contribute to enhancing scattering and absorption of electromagnetic waves, and rich defect sites can induce dielectric polarization to achieve dielectric loss. Introducing the PNTs (at) MoS2 core-shell nanowire as an electromagnetic wave absorbent into a polylactic acid / dichloromethane system, then putting the system into a culture container in which a conductive filler is pre-paved, and standing and volatilizing at room temperature by adopting an ethanol solution as a volatile agent to finally obtain a three-layer asymmetric electromagnetic shielding composite film comprising the conductive filler, the PNTs (at) MoS2 structure and a polylactic acid matrix from bottom to top. And an asymmetric conductive gradient network is constructed, and the EMI shielding performance which mainly focuses on absorption is remarkably improved, so that the secondary radiation problem of electromagnetic waves is reduced.

This invention provides a dry powder drag-reducing agent for fracturing fluids and its preparation method, belonging to the technical field of fracturing materials for drilling. The method includes the following steps: dissolving 4-bromobutyryl chloride and N-dodecylmethylamine in acetonitrile, heating and stirring to react; adding polyethylene glycol monomethyl ether acrylate and dichloromethane; stirring under a nitrogen atmosphere; purifying to obtain a double-tailed hydrophobic monomer; mixing core-shell Fe3O4 / SiO2 composite nanoparticles, ethanol aqueous solution, KH570, and ammonia solution; stirring; purifying to obtain modified SiO2 / Fe3O4; adding acrylamide, acrylic acid, sodium 2-acrylamido-2-methylpropanesulfonate, the double-tailed hydrophobic monomer, and modified SiO2 / Fe3O4 to water; adjusting the pH value; mixing and stirring with nitrogen gas; adding an azo initiator; stirring; cooling; purifying; vacuum drying; and pulverizing into powder to obtain the dry powder drag-reducing agent for fracturing fluids. This invention achieves good drag-reducing performance while also possessing certain heat resistance, making it better suited for fracturing operations in drilling processes.

The invention discloses a method for coating a Ca-Cur submicron modified material-doped PLA layer on the surface of an Ag-DCPD film layer, and relates to the technical field of biological coatings on the surfaces of medical materials. The method comprises the following steps: manufacturing an LPBF-NiTi alloy matrix by adopting a laser powder bed melting additive manufacturing technology, and carrying out pretreatment on the LPBF-NiTi alloy matrix; the pretreated LPBF-NiTi alloy matrix is subjected to electrochemical deposition in an electrolyte solution, and the LPBF-NiTi alloy matrix with the deposited Ag-DCPD film layer is obtained; the preparation method comprises the following steps: dissolving CaCl2 and curcumin in absolute ethyl alcohol, putting the solution into a closed container filled with (NH4) 2CO3, and carrying out constant-temperature reaction to obtain a Ca-Cur submicron modified material; polylactic acid is dissolved in dichloromethane, then the Ca-Cur submicron modified material is dispersed in the dichloromethane, and a leaching solution is obtained; and the LPBF-NiTi alloy matrix on which the Ag-DCPD film layer is deposited is subjected to repeated dipping and pulling in the leaching solution, and the LPBF-NiTi alloy matrix coated with the Ag-DCPD / PLA / Ca-Cur composite film layer is obtained. According to the invention, the corrosion resistance, the biocompatibility and the antibacterial and anti-inflammatory performance of the Ag-DCPD film layer are successfully improved.

The invention relates to the technical field of pharmaceutical preparations, and discloses a high-drug-loading risperidone sustained release microsphere for subcutaneous injection and a preparation method thereof, and the preparation method comprises the following steps: mixing risperidone, polylactic acid and dichloromethane to obtain an oil phase; dissolving a pore-forming agent in water to obtain a pore-forming agent solution; mixing polyvinyl alcohol, sodium chloride and water to obtain a water phase; mixing the oil phase with the pore-forming agent solution to obtain primary emulsion; mixing and stirring the primary emulsion and a water phase until dichloromethane is completely volatilized to obtain microspheres loaded with speridone; mixing cellulose acetate, polyethylene glycol and an organic solvent to obtain a coating solution; and coating the risperidone-loaded microspheres with a coating solution to obtain the high-drug-loading risperidone sustained-release microspheres capable of being used for subcutaneous injection. According to the invention, the efficient drug loading is realized, the injection comfort is improved, the slow permeation and release of the drug are realized, and the onset speed and the long-acting treatment demand are balanced.

The application relates to the technical field of pharmaceutical chemistry, and particularly discloses a key impurity of netupitant and a preparation method thereof. The preparation method of the key impurity of netupitant is as follows: netupitant is placed in a dichloromethane medium, stirred, heated and refluxed, and the netupitant and the dichloromethane are reacted. The structure of the netupitant contains an N-methyl piperazine ring, and a chloromethyl group is connected to a tertiary amine nitrogen of the ring. The reaction generates a chloromethylated quaternary ammonium salt, which is the key impurity of the netupitant. The impurity belongs to an impurity possibly generated in a preparation route of the netupitant. The application discloses reaction conditions for generating the key impurity of the netupitant, and provides a reference for quality control of the netupitant.

The invention relates to the technical field of catalyst preparation, in particular to a supported TBD-IPTS / SBA-15 catalyst and a preparation method and application thereof.The preparation method comprises the following steps that an SBA-15 carrier is treated with acid liquor, washed to be neutral and then dried, and an activated carrier SBA-15-OH is obtained; the preparation method comprises the following steps: dispersing SBA-15-OH in anhydrous toluene under the protection of nitrogen, adding IPTS (isopropyl-beta-d-thiosulfate) for reflux reaction, and washing and drying after the reaction is finished to obtain IPTS / SBA-15; iPTS / SBA-15 is dispersed in anhydrous dichloromethane, a TBD solution is added for a reaction, washing and drying are performed after the reaction is finished, and a supported TBD-IPTS / SBA-15 catalyst is obtained; the problems that in existing captopril intermediate synthesis, a by-product L-MAT is difficult to utilize, a traditional homogeneous TBD catalyst is difficult to recycle and reuse, and in an existing loading technology, active components are poor in stability and low in catalytic efficiency are solved.

The application provides a method for synthesizing an eplerenone intermediate N-1 by one-pot method, and belongs to the technical field of organic synthesis. The method is characterized in that: the eplerenone intermediate N-4 is dissolved in dichloromethane, a potassium carbonate aqueous solution and dibromohydantoin are added to perform an opening ring reaction; after the reaction is completed, hydrochloric acid is directly added to perform a rearrangement reaction; then water is separated and methanol is added in the organic layer to perform an ozonation reaction; then sodium sulfite is added to perform a reduction reaction; then hydrochloric acid is added to perform a methyl esterification reaction, so as to obtain the eplerenone intermediate N-1 crude product, and finally the eplerenone intermediate N-1 fine product is obtained through refining. The method realizes the one-pot synthesis of the eplerenone intermediate N-1 from the eplerenone intermediate N-4 through the continuous reactions of opening ring, rearrangement, ozonation, reduction and methyl esterification, and can avoid column chromatography purification, so that the method becomes a green chemical process route with greatly reduced organic solvent consumption and wastewater.

The invention discloses a method for synthesizing a polysubstituted trifluoromethyl olefin compound from gem-difluoroallyl alcohol. The preparation method comprises the following steps: in a nitrogen (N2) atmosphere, sequentially adding a gem-difluoroallyl alcohol (R1R2OHCR3C = CF2) compound, acetic anhydride (Ac2O), a solvent dichloromethane (DCM) and a fluorine source pyridine hydrofluoride (Py.9HF) reagent into a 10mL Schlenk tube to obtain a mixture, stirring the mixture at room temperature (rt) until the reaction is finished, filtering, washing and drying to obtain the compound. A crude product obtained by the reaction is subjected to silica gel column chromatography separation to obtain the high-selectivity polysubstituted trifluoromethyl olefin compound. The preparation method disclosed by the invention can be carried out under mild conditions and is simple and convenient to operate, most of the adopted raw materials are simple and easily available or commercialized reagents, the reaction raw materials are easily available, the yield of the target product is high, the functional group compatibility of the product is good, and the application range of a substrate is relatively wide; the obtained polysubstituted trifluoromethyl olefin compound contains a plurality of functional groups such as trifluoromethyl, olefin and the like. The method provides a more efficient and safer new strategy for synthesizing the polysubstituted trifluoromethyl olefin under mild conditions, particularly, metal participation is avoided, a new opportunity is provided for green medicine synthesis, and the method is predicted to have wide application prospects in the fields of medicine research and development, natural product derivative synthesis, life science and the like.

The application discloses a synthesis method of afugan, which comprises the following steps: 1-[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroacetone and 4-acetylnaphthalene carboxylic acid are added into a solvent, a base is added, DMAP is added after complete reaction at 50-80 DEG C, acetic anhydride is added dropwise, tetrabutylammonium bromide is added after complete reaction, and an aqueous solution of sodium hydroxide and hydroxylamine hydrochloride is added, and reaction is carried out at 0-5 DEG C, so that an intermediate is obtained; the intermediate is reacted with acyl chloride under the action of DMF and dichloromethane, so that 4-(5-(3-chloro-5-(trifluoromethyl)phenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole-3-yl)-1-naphthalene carboxylic chloride is prepared; 2-amino-N-(2,2,2-trifluoroethyl)acetamide hydrochloride and a dichloromethane solution of a base are added dropwise, and reaction is carried out at 0-5 DEG C, so that afugan is obtained. The method has a short route, high yield and suitability for large-scale industrial production.

The invention belongs to the field of organic synthesis, and discloses tetrahydronaphthalene-1-ketone as well as a preparation method and application thereof.The tetrahydronaphthalene-1-ketone is obtained by mixing tetrahydronaphthalene, carbon nitride and persulfate in an organic solvent (acetonitrile or dichloromethane) and reacting under the illumination condition of 395-457 nm. The preparation method disclosed by the invention is relatively high in yield, conforms to a green production concept, is environment-friendly, low in cost, simple to operate and high in selectivity, and is expected to be used for industrial production.

This invention discloses a fluorine-free oil-resistant agent for internal sizing, its preparation method, and its application method, belonging to the field of papermaking additives technology. Using agricultural waste as raw material, silicon carbide and silicon dioxide are mixed and pyrolyzed with nitrogen and dichloromethane. The pyrolysis products are condensed and allowed to stand to obtain an aqueous phase, a hydrophobic and oleophobic phase, and a dichloromethane phase. The hydrophobic and oleophobic phase is treated to generate chain-like siloxane compounds. These are then added to the dichloromethane phase and subjected to a halogenation reaction to generate halosiloxane compounds. The dehydrated aqueous phase is then added to the halosiloxane compounds to undergo an oxidation reaction, generating siloxane oxide compounds, i.e., the fluorine-free oil-resistant agent for internal sizing. The fluorine-free oil-resistant agent for internal sizing prepared by this method is used in the wet-end chemical stage of papermaking. It can be dispersed in water and adsorbed onto fibers. During the papermaking drying stage, it cross-links with the fibers through esterification, giving the paper good ring crush strength and oil-resistant effect.

The invention relates to the technical field of heme purification, in particular to a heme extraction and purification method. Comprising the following steps: taking fresh animal blood, centrifugally collecting lower red blood cell precipitate, adding normal saline, uniformly mixing and washing; adding an ethanol solution with the concentration of 1-10%, uniformly mixing, and ultrasonically crushing for 15-60 seconds under the power of 300-800W to obtain erythrocyte crushing liquid; adding an acidic acetone solution into the erythrocyte crushing liquid, uniformly mixing, extracting at normal temperature, centrifuging, and collecting supernate to obtain an acidic acetone extracting solution; slowly adding a NaOH solution to adjust the pH value; adding sodium acetate, stirring, standing, taking precipitate, washing and drying to obtain a crude product; filling a silica gel column; loading the crude product, eluting with an eluent, and collecting an elution component containing a target product; the eluent comprises dichloromethane, methanol and formic acid; and removing the mobile phase in the elution component. The method has the advantages of simple process, low cost, environmental friendliness and capability of obtaining a high-purity product.

The invention discloses a hydrogenated lecithin synthesis method based on a nickel catalysis continuous flow strategy, relates to the technical field of preparation of hydrogenated lecithin, and aims to solve the problem that the cost of preparing the hydrogenated lecithin is greatly increased due to the fact that the hydrogen pressure is relatively high and recycling of a catalyst is not considered in an existing method. The preparation method is technically characterized by comprising the following steps: (1) performing heat treatment on moso bamboo powder in a protective gas atmosphere to obtain a carbon carrier; dipping the carbon carrier in an alkali solution, and then carrying out a high-temperature activation reaction in a protective gas atmosphere; an activated carbon carrier is obtained; the preparation method comprises the following steps: loading a nickel source, an auxiliary agent and a structure stabilizer into an activated carbon carrier by dipping to obtain a catalyst precursor, and pyrolyzing the catalyst precursor in a protective gas atmosphere to obtain a Ni / C catalyst, and (2) preparation of hydrogenated lecithin: dissolving lecithin in a mixed solution of dichloromethane and methanol, taking a Ni / C catalyst, filling a catalytic pipeline with the Ni / C catalyst, and carrying out a hydrogenation reaction under hydrogen flow to obtain the hydrogenated lecithin.

The application discloses a method for regionally selective C3-H alkyne of triazolopyridazine compounds, and belongs to the field of organic synthesis. The method uses triazolopyridazine and high-valence iodine (III) alkyne reagent as raw materials, and a double catalytic system composed of Ph3PAuNTf2 (5 mol%), AgOTf (5 mol%) and 1,10-phenanthroline (20 mol%) in dichloromethane, and after reaction at 50 DEG C, the C3 alkyne product is obtained through purification. The method solves the problems of catalyst deactivation and poor selectivity caused by nitrogen-rich heterocyclic rings through gold / silver synergistic catalysis, and realizes precise functionalization of the C3 position. The reaction condition is mild, the substrate is widely applicable (R¹ contains various aryl groups and heteroaryl groups, and R² is compatible with different substituted aryl groups), the yield is 60% to 95%, the step is economical, and the method is suitable for large-scale preparation.

The invention discloses an ultraviolet-controlled photo-reversible dynamic crosslinking high polymer material with reversible antibacterial, shape deformation and toughening functions, and a preparation method thereof, belonging to the technical field of high polymer materials. Comprising the following steps: step 1) dissolving coumarin-3-formic acid, three-arm PCL (polycaprolactone), dicyclohexylcarbodiimide and 4-dimethylaminopyridine in dry dichloromethane in an inert atmosphere to obtain a reaction mixture; the invention relates to a preparation method of a coumarin-terminated three-arm polycaprolactone cross-linked polymer material.The preparation method comprises the following steps of (1) preparing coumarin-terminated three-arm polycaprolactone, (2) heating a reaction mixture obtained in the step (1) for set time, and filtering and separating an obtained product to obtain coumarin-terminated three-arm polycaprolactone, and (3) cross-linking and curing for set time through 365 nm ultraviolet to obtain a target product cross-linked polymer material.The function is highly integrated and dynamically adjustable, and the limitation that a traditional material is single in function is broken through.

The invention belongs to the technical field of synthesis of extraction agents, and particularly relates to a preparation method and application of amido diphosphinic acid. The preparation method comprises the following steps: (1) mixing a solvent, primary amine, cyclohexylphosphinic acid and inorganic acid, and heating until the solution is clear and transparent; (2) adding a formaldehyde solution or paraformaldehyde into the clear and transparent solution for reaction; and (3) removing a water phase from the mixture obtained after the reaction in the step (2) is finished, dissolving jelly obtained after the water phase is removed by using dichloromethane, and carrying out washing, rotary evaporation and drying to obtain the amido diphosphinic acid.