17744results about "Organic compound preparation" patented technology

The invention relates to a preparation method of phenylmethylamine. The technical scheme adopted by the invention for mainly solving the problems of high catalyst loss, low production efficiency and high intermittent operation labor intensity is as follows: the preparation method of the phenylmethylamine comprises the following steps: mixing the raw material of cyanobenzene with a solvent material or at least one of one part of product materials in a mixing unit, introducing the mixture into a fixed bed hydrogenation reactor to be in contact with hydrogen and a catalyst and carry out multi-phase continuous hydrogenation reaction to obtain a product material containing phenylmethylamine, separating the product material to obtain a phenylmethylamine product, wherein the catalyst is a metal loaded catalyst; and the metal is selected from at least one of Pd, Pt, Cu, Ni, Mo and Fe. The preparation method can be used for preparing phenylmethylamine.

This invention discloses a fluorene-based organic small molecule hole transport material and its applications. The general structural formula of the fluorene-based organic small molecule hole transport material is as follows: where n = 1-4, and R represents the hole transport capacity. This fluorene-based organic small molecule hole transport material is used as an undoped hole transport material in perovskite solar cell devices. By introducing dicarboxylic acid groups onto the fluorene-based organic small molecule hole transport material, when used in an inverted perovskite solar cell device, it can form chemical bonds with the hydroxyl groups of the glass conductive substrate, forming a directionally aligned self-assembled layer on the surface of the glass conductive substrate. This effectively improves the charge transport capability at the interface and increases the photoelectric conversion efficiency of the perovskite solar cell device. Furthermore, since this perovskite solar cell device does not contain lithium salts, it exhibits high water and oxygen stability. In addition, the synthesis process of this fluorene-based organic small molecule hole transport material is simple, and the raw materials are inexpensive and readily available, making it highly valuable for practical applications.

The invention discloses a catalyst used for preparing acrylic acid and butyl ester by the dehydration of butyl lactate and a preparation method thereof. The catalyst is a composite catalyst, comprising a main catalyst A and auxiliary catalysts B, C, D and E, wherein, A is calcium sulphate, B is sulphuric acid, C is phosphate, D is alkaline matter and E is promoter. The preparation method comprises the steps as follows: five compositions A, B, C, D and E are sufficiently mixed, baked for 2-10 hours at the temperature of 200-800DEG C and formed for standby. The catalyst has high catalytic activation; under the catalysis of the catalyst, the molar yield reaches 75.1 percent and the molar selectivity of the acrylic acid and butyl ester reaches 71.5 percent. The preparation method has the advantages that the crystal structure of the main catalyst can be improved so as to be beneficial for carrying out the reaction; and the introduction of different auxiliary catalysts and quantities is helpful to improve the conversion ratio of the raw material and the product selectivity and is beneficial for improving the strength of the catalyst.

Compound (I), deuterated derivatives, and pharmaceutically acceptable salts of any of the foregoing are disclosed. Methods of treating cystic fibrosis using these compounds are also disclosed.

The invention relates to the technical field of scintillator materials and X-ray detection, in particular to a rare earth organic-inorganic hybrid complex scintillator and a preparation method and application thereof. The general formula of the rare earth organic-inorganic hybrid complex scintillator is [RE (L) 4] <->. [A] < + >, wherein RE is selected from Eu, Tb, Sm or Dy; l is a beta-diketone ligand; [A] < + > is selected from long-chain hydrophobic quaternary ammonium salt cations or heterocyclic quaternary ammonium cations which have the carbon atom number of C8-C20 and do not contain active functional groups. The rare earth organic-inorganic hybrid complex scintillator provided by the invention has good solubility and molecular-level dispersion capability. The scintillator film based on the rare earth organic-inorganic hybrid complex prepared by using the rare earth organic-inorganic hybrid complex has the characteristic of compatibility of high scintillator load and high light transmission, overcomes the problems of low scintillator load rate, poor transparency and limited imaging resolution of the traditional scintillator film, and has excellent practical value and popularization prospect.

The invention relates to the technical field of organic chemical synthesis, in particular to a preparation method of 3, 4 '-diaminodiphenyl ether.The preparation method comprises the steps that S1, under inert gas and in a first solvent, m-dinitrobenzene and p-acetamidophenol are subjected to a heating reaction under the condition of a weak base catalyst, and 3-nitro-4-acetamido diphenyl ether is prepared; s2, in a second solvent, the 3-nitro-4-acetamido diphenyl ether is subjected to a hydrogenation reduction reaction, and 3-amino-4-acetamido diphenyl ether is prepared; and S3, dissolving the 3-amino-4-acetaminodiphenyl ether in an alcohol solvent system, adding an aqueous solution of alkali, controlling the reaction temperature, carrying out a hydrolysis reaction, and after the reaction is finished, carrying out post-treatment to obtain the 3, 4 '-diaminodiphenyl ether. The preparation method provided by the invention has the advantages of easily available raw materials, low price, good selectivity and high product yield, and is more suitable for industrial production by comprehensively considering economical efficiency and safety.

The invention provides a method for recovering a BHET monomer from a waste polyester textile alcoholysis solution, and is characterized in that the recovery method comprises the following steps: (1) filtering: mixing the waste polyester textile alcoholysis solution with water under a stirring condition, and filtering at 55-70 DEG C; and (2) cooling crystallization: under a stirring condition, carrying out primary cooling on the filtrate obtained by filtering in the step (1) from 55-70 DEG C to 45-55 DEG C, then adding a BHET seed crystal, then carrying out secondary cooling to 5-15 DEG C, and maintaining the temperature for 20-60 min to obtain the BHET monomer. The mixed solution cooling crystallization method is developed on the basis of complexity of components of the waste polyester textile fabric, the problems that in the conventional production process, a BHET crystal product is low in quality, prone to scaling, difficult to filter and dry and the like are solved, and the obtained BHET product is large in particle size, narrow in particle size distribution, high in purity, good in fluidity and high in stability.

The invention relates to the technical field of methanol production, and discloses an efficient gas-liquid distribution device for a methanol synthesis reaction tower. The liquid distribution assembly is used for distributing a catalyst; the filler assembly is used for promoting gas-liquid contact; when the liquid distribution assembly runs, the liquid distribution assembly drives the atomization assembly to atomize the catalyst flowing on the inner wall of the tank body; the liquid distribution assembly comprises a rotating shaft, the rotating shaft is rotationally installed in the tank body, a wind wheel is fixedly connected to the rotating shaft, a liquid disc is fixedly connected to the top end of the rotating shaft, a plurality of first spray heads are hinged to the liquid disc, and hoses are arranged between the first spray heads and the liquid disc. Through the arrangement of the liquid distribution assembly, the multiple first spray heads can swing in a reciprocating mode in the rotating process, so that the spraying range of the first spray heads is expanded, the situation that spraying blind areas occur in the tank body is avoided, catalysts in the tank body are distributed more evenly, and the gas-liquid contact efficiency is improved.

The invention relates to a preparation method and application of a porous material for preparing methanol through carbon dioxide adsorption and conversion. When the material is prepared, firstly, 4, 4 '4' '-(1, 3, 5-triazine-2, 4, 6-trimethylene) triphenylamine and 1, 2-acenaphthequinone are treated in a mixed solvent containing dioxane / acetonitrile / 6M acetic acid, and AT-COF is obtained; further synthesizing by adopting an impregnation method to obtain IrRu-COF; and finally, uniformly mixing the active gamma-aluminum oxide and the IrRu-COF material to form a carrier dispersion liquid, and then carrying out PEI loading, vacuum impregnation, washing and drying to obtain the PEI functionalized gamma-Al2O3 / COF composite catalyst. The technical closed loop from low-concentration CO2 capture to solar driven conversion is realized, the process flow is simple, and the energy consumption is low.

The invention relates to the technical field of chemical engineering, in particular to a method and a device for removing heavy components from cyclohexanol. Comprising the following steps: a, rectifying a cyclohexanol-containing material from a cyclohexene hydration reaction to obtain a first solution containing cyclohexanol and heavy components in a tower kettle; b, carrying out heavy component removal operation on the first solution to obtain a third solution containing a catalyst and heavy components, a first gas phase and a second gas phase; and c, rectifying the first gas phase and the second gas phase to obtain a fourth solution subjected to heavy component removal, namely cyclohexanol subjected to heavy component removal. The entrained catalyst and heavy components are removed together, and the fluidity required by the catalyst waste liquid is maintained by using the heavy components, so that the loss of cyclohexanol is reduced.

The invention relates to the technical field of automatic control, in particular to a monitoring method and system for synthesizing ceramide based on alpha-hydroxy fatty acid, and the monitoring system for synthesizing ceramide based on alpha-hydroxy fatty acid comprises a raw material feeding module, a reaction control module, a quenching-crystallization joint control module and a data integration module; carrying out dynamic weighing monitoring on the raw materials based on the received synthesis instruction, and starting a reaction kettle according to weighing data; performing multi-dimensional data acquisition in real time according to the set reaction data, and performing dynamic feeding control according to the set reaction data; when the TLC detection substrate reaction is completed, the cooling process and the crystallization process are regulated and controlled in real time according to the reaction data until the end point judgment standard is met; according to a received synthesis completion instruction, product quality data is obtained, a monitoring data packet is generated, the synthesis instruction is marked and then stored, process control is accurately monitored and controlled, and the purity and crystal form of the product are ensured.

The invention discloses a supported nickel catalyst for preparing 1, 3-propylene glycol through hydrogenation of 3-hydroxypropionaldehyde as well as a preparation method and application of the supported nickel catalyst, and relates to the technical field of catalysts. The modified long-chain multi-carbon inducer is used, and a special long-chain molecular structure and a branched chain group of the inducer can effectively and selectively adsorb and occupy a micropore impregnation site; the preparation method has the beneficial effects that more active component nickel species are obviously promoted to be dispersed in main reaction confinement spaces such as mesopores and macropores and interact with the carrier to form effective active sites, and active component steeping liquor is inhibited from entering micropore channels due to capillary action; the active site failure caused by agglomeration of nickel species in micropores in the subsequent drying and roasting process of the catalyst precursor is avoided, the efficient and directional reaction is ensured, the generation of by-products is greatly reduced, the pressure is relieved for the subsequent product rectification separation, and the final product purity is improved. The catalyst provided by the invention can still keep an excellent catalytic effect when the air speed of a 3-hydroxypropionaldehyde solution is increased to 6.5 h <-1 >.

The invention relates to the technical field of guanidine nitrate preparation, in particular to a method for preparing guanidine nitrate by a continuous dynamic tubular reaction process, which comprises the following steps: uniformly mixing dicyandiamide, target ammonium nitrate and target ammonium carbonate according to a mass ratio of 1: (1-3): (1-0.5); conveying the uniformly mixed material to a feeding section in a dynamic tubular reactor through a first conveying screw rod for mixing treatment, wherein the dynamic tubular reactor further comprises a heating section, a reaction section and a cooling section; sequentially conveying the target mixed material to a heating section for heating melting treatment, a reaction section for synthesis reaction treatment and a cooling section for cooling forming treatment through a second conveying screw rod to obtain an initial product; conveying the initial product into a cooling and crushing device for cooling and slicing to obtain a target guanidine nitrate product. According to the method disclosed by the invention, the mass and heat transfer efficiency can be improved, the online quantity and liquid holdup of the material are reduced, meanwhile, the raw material ratio and the reaction path are optimized, and the safety and the product purity are improved.

A method of synthesizing the benzoate salt of 5-MeO-DMT comprising the step of treating the hydrochloride salt of 5-MeO-DMT with a base, prior to the addition of benzoic acid.

This invention discloses a method for preparing a CuZnAlGa-based layered double hydroxide (TLH)-derived catalyst for methanol production from carbon dioxide-rich syngas. Using Cu, Zn, Al, and Ga metal salts as precursors, Na₂CO₃ and NaOH as precipitants, and a mixed alcohol-water solution as an auxiliary solvent, co-precipitation is performed under controlled temperature and pH to obtain a LDH-like catalyst precursor. After high-temperature calcination and in-situ reduction in a hydrogen atmosphere, a layered framework structure of Cu nanoparticles immobilized by oxides is obtained. The LDH-like structure provides lattice confinement, preventing Cu particle aggregation, and the interaction between Cu and the oxides enhances the catalyst surface's adsorption capacity for CO and CO₂, thereby improving the activity and stability of methanol production from carbon dioxide-rich syngas.

The invention relates to a fly ash-based MOFs adsorption-catalysis material integrated preparation method, and belongs to the field of solid waste treatment and resource utilization. The material takes industrial solid waste fly ash as a matrix, and is prepared by the following steps: firstly, carrying out alkali modification and silane coupling agent surface activation treatment on fly ash to form a high-activity matrix; then loading a metal organic framework (MOFs) on the surface of the activated fly ash through an in-situ synthesis process to form a porous composite carrier; the integrated material with CO2 adsorption and catalytic conversion functions is further prepared through impregnation of a copper-based active component and a high-temperature calcination process. According to the invention, the problems of high energy consumption, high cost and low comprehensive utilization rate of fly ash of the traditional CO2 capture and utilization technology (ICCU) are solved, high-valued resource utilization of industrial solid waste and efficient capture and conversion of CO2 are synchronously realized, and the method has dual values of environmental protection and economy.

The present disclosure, among other things, provides technologies for synthesis, including reagents and methods for stereoselective synthesis. In some embodiments, the present disclosure provides compounds useful as chiral auxiliaries. In some embodiments, the present disclosure provides reagents and methods for oligonucleotide synthesis. In some embodiments, the present disclosure provides reagents and methods for chirally controlled preparation of oligonucleotides. In some embodiments, technologies of the present disclosure are particularly useful for constructing challenging internucleotidic linkages, providing high yields and stereoselectivity.

The invention provides tegorasan monoethyl fumarate as well as a preparation method, a pharmaceutical composition and an application of the tegorasan monoethyl fumarate. The tegorac monoethyl fumarate provided by the invention is relatively good in solubility and good in stability, the bioavailability of a medicine is increased by improving the solubility of the medicine, and the tegorac monoethyl fumarate is suitable for industrial production and has a good market prospect.

The invention discloses a method for synthesizing electronic-grade ethyl acetate through catalytic esterification of acidic ion exchange resin, and belongs to the technical field of ethyl acetate preparation. The method comprises the following steps: mixing crosslinked polystyrene white balls and a swelling agent, and dropwise adding concentrated sulfuric acid for reaction to obtain S-PS resin; mixing an EDTA disodium salt saturated solution and a polyacrylic acid solution, adding a cross-linking agent and an emulsifier, and carrying out a cross-linking curing reaction to obtain EDTA microcapsules; the preparation method comprises the following steps: dispersing S-PS resin in a solvent, adding EDTA microcapsules, a dehydration condensation agent and a catalyst, reacting under the protection of inert gas, and filtering and recovering after the reaction is finished to obtain S-PS-EDTA resin; mixing glacial acetic acid, absolute ethyl alcohol and S-PS (at) EDTA resin for reaction, and filtering and collecting liquid after the reaction is finished; and rectifying the collected liquid to obtain the product. According to the method provided by the invention, metal impurities can be chelated in the synthesis process, and the electronic-grade ethyl acetate with high purity and low impurity content is produced.

The invention discloses a preparation method for selectively oxidizing thioether into sulfoxide through photo-initiation, and belongs to the field of synthesis of medical compounds. The preparation method comprises the following steps that in the air atmosphere, a thioether compound is dissolved in an acetonitrile-water mixed solvent, inorganic metal salt catalysts such as ferric chloride and copper sulfate are added, the mixture reacts for 8-48 h at the temperature of 0-45 DEG C under illumination with the wavelength of 295-405 nm, selective oxidation is carried out, and the sulfoxide product is obtained, and the molar ratio of thioether to the catalysts is 5: 1. The method overcomes the problems of excessive oxidation risk, complicated operation, environmental pollution and the like caused by dependence of a noble metal catalyst and use of a strong oxidant in the existing thioether oxidation method, has the advantages of high catalytic efficiency, high yield and excellent selectivity, can greatly reduce the production cost, is suitable for later industrial synthesis and amplification, and has wide application prospects. The method has the advantages of no expensive metal catalyst or oxidant, simple preparation process, high efficiency, environmental protection, safety and cost saving.

The invention provides a catalyst, a preparation method and application thereof, and a method for preparing primary amine by catalyzing nitrile compound hydrogenation, and particularly relates to the technical field of catalyst synthesis. The catalyst comprises a nickel / cobalt-based catalyst and a metal salt; wherein the nickel / cobalt-based catalyst is selected from any one of a supported nickel / cobalt-based catalyst, a Raney nickel / cobalt catalyst or a nickel / cobalt nanocrystal; the metal salt comprises any one or a combination of at least two of tungsten salt, molybdenum salt, vanadium salt, aluminum salt and cerium salt. The metal salt and the nickel / cobalt main catalyst have a synergistic effect: the surface electron density is adjusted through electron transfer, the hydrogen dissociation and cyano adsorption activation capacities are enhanced, the hydrogenation activity is improved, and the mild condition reaction is assisted; the surface chemical environment is changed or steric hindrance is borrowed, the primary amine selectivity is improved, and byproducts are inhibited; aluminum salt, cerium salt and the like inhibit nickel / cobalt agglomeration, increase active sites, enhance stability, prolong the service life and reduce the dosage.

The invention discloses a copper-silicon catalyst as well as a preparation method and application thereof, and the copper-silicon catalyst comprises the following components in percentage by weight: 43-79wt% of silicon dioxide; the content of copper oxide is 15-35 wt%; the content of the auxiliary agent A is 3-10 wt%; the auxiliary agent B accounts for 3-12 wt%; the auxiliary agent A comprises one or more of alkali metal or alkaline earth metal oxides; and the auxiliary agent B comprises one or more of VB to VIIB group metal oxides. The raw materials of the catalyst are cheap and easy to obtain, the reaction condition is mild, the catalyst is environment-friendly, and the prepared catalyst is small in copper species particle size, high in dispersity, high in conversion rate and selectivity and good in stability.

The present invention provides a method for synthesizing alacastran, comprising reacting an amino compound of formula V with a chiral intermediate of formula VI, reducing the resulting product with a reducing agent capable of providing an ethyl group to produce a compound of formula VII, and then deprotecting the compound to obtain alacastran, as shown in the following reaction formula. The method for synthesizing alacastran of the present invention avoids the low yield caused by amide reduction and the risk of substrate racemization, has a high yield, low material cost, safe operation, and is suitable for industrial production.

The invention relates to the field of molecular targeted therapy, and discloses an application of an SLC16A5 (MCT6) small-molecule inhibitor MCT6-Ai7-2 in preparation of a medicine for treating acute myeloid leukemia (AML). The inhibitor takes an SLC16A5 protein structure predicted by Alphafold as a target spot, and is obtained through compound database screening, molecular docking and druggability optimization. An in-vitro experiment proves that MCT6-Ai7-2 can remarkably inhibit proliferation of AML cell lines such as U937 and MOLM-13, induce cell apoptosis and retard a cell cycle, has an inhibiting effect on a primary AML patient specimen and is relatively low in toxicity to normal cells; in-vivo experiments show that the compound is effective and has good safety in AML model mice. In addition, the MCT6-Ai7-2 and the vinca can be combined to synergistically enhance the inhibition effect on vinca drug-resistant cells, and by reducing the expression of anti-apoptotic protein MCL-1, the activation of pro-apoptotic factors BIM and tBID is promoted to play a role. The invention provides a novel targeting drug and strategy for treatment of AML (especially drug-resistant or recurrent patients).

The invention discloses a method for preparing high-purity nickel acetate from crude nickel carbonate in the technical field of nickel compound purification, which comprises the following steps: mixing the crude nickel carbonate with deionized water to obtain a suspension, and adding glacial acetic acid to react to obtain a nickel acetate solution; then a specially-made hierarchical-pore titanium silicalite molecular sieve loaded bimetallic nanocluster material is added for purification treatment, the material is obtained through precise preparation, the method comprises the steps of carrier modification, bimetallic loading, hydrophobic modification, activation balance and the like, and the material has excellent impurity adsorption capacity and chemical stability; carrying out concentration crystallization and solid-liquid separation on the purified solution to obtain wet nickel acetate crystals; the mother liquor is subjected to adsorption treatment again, crystals in the mother liquor are recycled, and finally all the crystals are combined and dried to obtain a high-purity nickel acetate product. The process is simple and efficient, the purity of the prepared nickel acetate exceeds 98.5%, the content of each impurity is superior to the industrial standard, and the mother liquor can be recycled, is environment-friendly and is suitable for industrial production.

The invention discloses a reaction device based on dichlorobenzonitrile synthesis and a use method thereof, and relates to the field of reaction devices.According to the technical scheme, the reaction device comprises a reaction tank and a cover located at the top end of the reaction tank, a heating interlayer is arranged on the reaction tank, and a spiral conveying pipe surrounding a reaction cavity in the middle of the reaction tank is arranged in the heating interlayer; the heating medium is conveyed through the spiral conveying pipe, and the gap between the heating interlayer and the spiral conveying pipe is filled with the heat preservation material, so that the heating medium is conveyed around the reaction cavity in the heating interlayer through the spiral conveying pipe, and the spirally distributed conveying pipe can enable the heating medium to uniformly act on the outer wall of the reaction cavity; heat loss is reduced through the heat preservation material between the heating interlayer and the spiral conveying pipe, accurate control and uniform distribution of the reaction temperature are achieved, side reactions caused by local overheating are avoided, and therefore generation of polychlorinated impurities is reduced, and the purity of the dichlorobenzonitrile product is improved.

The invention provides a novel chiral ferrocene bridged binaphthyl skeleton phosphine ligand and application thereof. The ligand has the advantages of low cost, simplicity in synthesis, air stability and the like. The ligands have good catalytic activity and enantioselectivity in the asymmetric hydrogenation reaction of ketone, and have certain industrial application prospects in the synthesis of pharmaceutical molecules.

The invention discloses a method for degrading polystyrene (PS) plastic and upgrading and recycling the PS plastic into benzoic acid based on nano MnO2 photocatalytic ozonation, and belongs to the technical field of solid waste recycling. The method comprises the following steps: firstly, mixing PS plastic fragments with nano MnO2 and an organic solvent, then simultaneously introducing ozone into a reaction system at normal temperature and normal pressure, and irradiating with light. Through synergistic catalysis of light and ozone, molecular chains of the PS plastic can be efficiently and selectively broken and oxidized, and finally the PS plastic is directionally converted into benzoic acid with high additional value. After the reaction is finished, a benzoic acid product can be obtained through simple separation, concentration and purification steps. The method provided by the invention realizes high-valued recycling of the waste PS plastic under mild conditions, solves the problems of high energy consumption, complex products, easy generation of secondary pollution and the like in a traditional treatment method, and has the outstanding advantages of green process, efficient reaction, high product value and the like.

The invention belongs to the technical field of biochemical engineering, and particularly relates to an amitriptyline hapten and a preparation method thereof, an amitriptyline antigen and a preparation method thereof, an antibody, a kit and application. The amitriptyline hapten has a structural formula shown as a formula (I) or a formula (II). Compared with an existing structure, the amitriptyline hapten prepared by the invention has a better immune effect. The obtained antibody is high in titer, strong in specificity and high in affinity, the LOD of amitriptyline by using an Elisa method established by the antibody is 0.013 ng / mL, the IC50 of amitriptyline is 0.865 ng / mL, the quantitative detection range is 0.07-470.3 ng / mL, the detection sensitivity is high, and the linear range is wide.

The invention discloses a method for preparing 12-mercaptan through solid organic acid catalysis, belongs to the technical field of 12-mercaptan preparation, and aims to solve the problems of low catalyst activity, harsh reaction conditions, serious pollution, high cost and dependence on import in the prior art. N-dodecanol and hydrogen sulfide are used as raw materials and are mixed according to the molar ratio of 1: 1.2-1: 1.3; the method comprises the following steps: gasifying n-dodecanol, mixing with purified hydrogen sulfide, preheating to 210-240 DEG C, introducing into a fixed bed reactor filled with a solid organic acid catalyst, and reacting at-0.08-3.0 MPa for 3.5-4 hours; and cooling and condensing the reaction product, carrying out gas-liquid separation, rectifying and purifying the liquid product to obtain 12-mercaptan with the purity of more than or equal to 99.5%, and recycling unreacted hydrogen sulfide. The solid organic acid can be a catalyst of p-toluenesulfonic acid and the like or mesoporous silica loaded nickel, cobalt and molybdenum metal oxides. The method has the advantages of high catalytic activity, mild reaction conditions, high product yield (the conversion rate of n-dodecanol is greater than or equal to 94.5%), environmental protection and low cost, can realize the domestic mass production of 12-mercaptan, and meets the market demand.