235 results about "Formylation reaction" patented technology

The invention belongs to the technical field of catalysts, and particularly relates to a supported Co-based catalyst with a nano molybdenum carbide auxiliary as well as a preparation method and application of the supported Co-based catalyst. The preparation method comprises the following steps: depositing molybdenum oxide on the surface of a carrier material by adopting an atomic layer deposition method, then carrying out carburizing treatment to obtain a molybdenum carbide catalyst, depositing cobalt oxide on the surface of the molybdenum carbide catalyst by adopting the atomic layer deposition method, and then carrying out reduction treatment to obtain the supported cobalt-based catalyst with the nano molybdenum carbide assistant. According to the preparation method provided by the invention, the size of molybdenum carbide and the dispersity and valence state of cobalt are controlled by regulating and controlling the deposition times of molybdenum oxide, and the prepared catalyst has excellent catalytic activity and stability in the hydroformylation reaction of long-chain olefin with the carbon atom number being greater than or equal to 5.

The invention relates to the technical field of liquid chromatography, and discloses a mixed product liquid chromatography comprehensive analysis method which comprises the following steps: S1, mixing products: respectively mixing aldehyde compounds and ketone compounds with different mobile phases, and then injecting into an injection chromatographic system; s2, liquid chromatographic analysis: separating and analyzing a mixed product by using a liquid chromatograph; s3, performing qualitative analysis; on the basis of liquid chromatographic analysis, each peak in a chromatogram is identified. The method aims at qualitative and quantitative analysis of main substances (groups) in an organic reaction mixed product system; the method is suitable for analyzing the relative percentage content of products related to organic chemical reactions such as raw materials (nonylphenol) related to a core production process, nonylphenol formylation reaction, nonylphenol esterification reaction, phenolic ester Fris rearrangement reaction and the like, and samples in a refining process; the influence of absorption peaks and chromatographic line oscillation of other non-target substances on the content analysis result can be effectively avoided.

The invention relates to the technical field of heterogeneous catalysis and fine chemical engineering, and discloses a rhodium-tungsten para-site MOF-based catalyst as well as preparation and application thereof. The invention relates to a rhodium-tungsten para-site MOF-based catalyst, which is composed of a catalytic active component, a metal additive and a carrier. The rhodium-tungsten para-site MOF-based catalyst provided by the invention takes a metal organic framework material as a carrier, an active component Rh and a metal additive W are stably anchored on the surface of the carrier, and an Rh-WOx para-site is successfully constructed; the rhodium-tungsten para-site MOF-based catalyst provided by the invention shows excellent catalytic activity and excellent cycle stability in olefin hydroformylation reaction, and overcomes the technical bottlenecks that noble metals in a homogeneous catalysis system are easy to lose and energy consumption is high in a product separation process; an efficient and stable catalyst design thought is provided for olefin hydroformylation reaction, and the catalyst has a good industrial application prospect.

The invention relates to an olefin hydroformylation homogeneous catalysis continuous reaction process and system. The process comprises the following steps: mixing raw materials olefin, synthesis gas and a metal catalyst, and then carrying out hydroformylation reaction; removing a light component containing the product aldehyde from the hydroformylation reaction liquid to obtain a heavy component containing the metal catalyst; uniformly mixing the heavy component with a first extraction agent, and performing phase splitting to obtain a first heavy component phase and a first extraction agent phase; a metal catalyst and a second extraction agent are separated from the first extraction agent phase, the metal catalyst is circularly used for the hydroformylation reaction, and the second extraction agent is used as the first extraction agent mixed with the heavy components. Based on the characteristics of solubility difference and specific gravity difference between the metal catalyst and other substances in the heavy components under specific conditions, the heavy components in a reaction system are reacted at a lower temperature on the premise of not additionally adding a reagent which can influence the activity of the catalyst, and the activity of the catalyst can be well maintained within a longer reaction time.

The invention discloses a system device and a method for producing aldehyde compounds through supergravity two-phase hydroformylation. The system device comprises a supergravity reactor, a buffer tank, a first circulating pump, a tower kettle heat exchanger, a circulating heat exchanger, a split-phase tank, a second circulating pump, a crude aldehyde transfer pump, a supergravity rectification unit, a tower kettle reboiler, a product extraction pump and a cold and hot all-in-one machine. According to the system device, under the condition that a polar solvent and a surfactant are not added, the two-phase hydroformylation reaction process can be greatly enhanced through the supergravity reactor, the technological process is shortened, and then a product is separated and purified through the supergravity rectification unit to obtain an aldehyde compound; the problems of low two-phase hydroformylation reaction efficiency, serious self-polymerization in a hydroformylation product purification process and the like in the prior art are solved; by utilizing the method, the olefin conversion rate is more than 90%, the aldehyde selectivity of the product is more than 99%, the purity of the purified product is more than 99%, and the loss amount of the catalyst is less than or equal to 0.5 mg / kg.

The invention relates to a preparation method and application of a PtNi modified ZnO catalyst. The preparation method comprises the following steps: stirring Zn (NO3) 2.6 H2O, Ni (NO3) 2.6 H2O and CO (NH2) 2 in deionized water to form a mixed solution, transferring the mixed solution into a high-pressure kettle, carrying out hydrothermal reaction, washing and drying to obtain a precursor; calcining the precursor in the air to obtain NiO-ZnO; a H2PtCl6 solution is dropwise added to the surface of NiO-ZnO, dipping is performed at the room temperature, a NaBH4 solution is added, stirring, washing and drying are performed at the room temperature, Pt / NiO-ZnO is obtained, the Pt / NiO-ZnO is placed in a reducing atmosphere to be calcined, and the PtNi modified ZnO catalyst PtNi / ZnOx is obtained. The catalyst is applied to a benzylamine N-formylation reaction in which carbon dioxide participates, the conversion rate of a benzylamine substrate can reach 85.0%, and the selectivity of amide products can reach 99.4%. The preparation process is simple to operate, and has better large-scale industrial production potential.

The invention provides a catalyst for adjusting the normal / isomeric ratio of a butyraldehyde product and an adjusting method of the catalyst. The catalyst comprises a ligand A, a ligand B and a rhodium substrate, wherein the ligand A is one or more of # imgabs 0 #, # imgabs 1 #, # imgabs 2 # or # imgabs 3 #; and the ligand B is # imgabs4 #. The invention provides a catalyst for adjusting the normal / isomer ratio of a formaldehyde product in the process of preparing butyraldehyde through a propylene hydroformylation reaction, and the catalyst has propylene hydroformylation catalytic activity after complexing a ligand A, a ligand B and a rhodium substrate based on an accurately designed ligand combination. A mixed ligand composed of a ligand A and a ligand B according to a certain proportion is added in a propylene hydroformylation reaction to be complexed with rhodium, so that the n-iso-ratio of butyraldehyde can be flexibly adjusted in a range of 1-17.3.

This invention belongs to the field of homogeneous catalysis technology, and particularly relates to a method for the hydroformylation of propylene to prepare isobutyraldehyde. The method includes: in the presence of a bidentate P-N ligand and a rhodium metal compound, introducing propylene and syngas to carry out a hydroformylation reaction to prepare isobutyraldehyde. The structural formula of the bidentate P-N ligand is as follows: [Insert structural formula here]. Wherein, R1 is selected from one of C2-C4 alkyl groups, substituted or unsubstituted phenyl groups; R2 is selected from one of hydrogen, C1-C4 alkyl groups, alkoxy groups, substituted or unsubstituted phenyl groups. This method provides a highly active P-N ligand, which, while reducing the amount of rhodium catalyst, maintains high activity and can significantly improve the conversion rate of propylene, as well as the selectivity and yield of isobutyraldehyde.

A process for producing an aldehyde is disclosed. The process comprises: hydroformylating an olefin to form the aldehyde using a hydroformylation catalyst; recovering an effluent stream comprising the aldehyde, hydrogen and the hydroformylation catalyst; passing the effluent stream to a stripper; contacting the effluent stream with a strip gas in the stripper to produce a stripped effluent stream having a lower hydrogen concentration than the effluent stream; and recovering the stripped effluent stream.

The invention relates to the technical field of hydroformylation reaction, and discloses a bimetallic center Cr-Co catalyst and a preparation method and application thereof.The bimetallic center Cr-Co catalyst has the structure shown in the formula (1), R1 and R2 are independently selected from C1-C10 alkyl, C6-C15 aryl and-O-R ', and R' is selected from C1-C10 alkyl, C6-C15 aryl and C7-C15 alkaryl. The catalyst has high conversion rate and high aldehyde selectivity when being used for hydroformylation reaction, and especially can improve the selectivity of straight-chain products in aldehyde. # imgabs0 #

The present application provides a catalyst for preparing oxygen-containing compounds by olefin hydroformylation reaction, and a preparation method and use thereof, the catalyst is Fe x Co y M, the catalyst contains 0.1-15wt% M, 85-99.9wt% Fe and Co, the atomic ratio of x to y is 0.1-10, and M is a metal element. When the catalyst is used for preparing oxygen-containing compounds by olefin hydroformylation reaction, the conversion rate of olefin can reach 93-99.9%, and the selectivity of oxygen-containing compounds can reach 89-98.8%; and the catalyst is in a solid state during the reaction, which is easy to realize solid-liquid separation with the product, and also avoids the loss of the catalyst during the separation process.

The utility model belongs to the field of chemical reaction, and particularly relates to an automatic reaction system which comprises a microfluidic device, the microfluidic device is provided with a gas supply module for supplying gas, and the interior of the microfluidic device is used for hydrogenation reaction and hydroformylation reaction; the first mechanical arm module is used for moving a reagent; the first mechanical arm module and the micro-fluidic module are in signal connection with the control module. The utility model provides an automatic reaction system and aims to solve the problem of safety risk of manual operation in the prior art.

This invention provides a method for determining the deactivation temperature and deactivation characteristics of a hydroformylation catalyst, comprising: S1. preparing a hydroformylation reaction solution; S2. measuring the reaction solution and placing it in an adiabatic testing instrument to simulate a hydroformylation reaction, stopping the heating when the temperature reaches T0 and incubating the reaction under adiabatic conditions; recording the temperature change and obtaining the highest temperature T. m S3. After cooling the test ball, remove half of the reactant material, add the hydroformylation reaction raw material, and heat up to simulate the hydroformylation reaction. When the temperature reaches T1, stop heating and perform an adiabatic reaction. Record the highest temperature T. mf S4. Compare T1 and T m and T mf If T mf =T1, catalyst deactivation temperature is T m Irreversible inactivation; if T mf =T m The catalyst deactivation temperature is T m Reversible inactivation; if T mf >T m Remove the material from the test sphere and repeat steps S2 to S4. The judgment method of this invention has a short testing cycle, high safety, and eliminates the need for sample separation and component analysis. It provides guidance for research on catalyst operating limits and the selection of homogeneous catalyst recovery temperatures.

The application provides a method and device for continuously preparing aldehyde compounds through a hydroformylation reaction. The method for continuously preparing aldehyde compounds through the hydroformylation reaction comprises the following steps: using a catalyst to catalyze an olefin raw material and synthetic gas to perform a hydroformylation reaction, so as to obtain a reaction product containing aldehyde compounds; and separating the reaction product, so as to obtain the aldehyde compounds and recover the catalyst. The hydroformylation reaction comprises a homogeneous reaction or a heterogeneous reaction. The method can solve the problem of a large amount of catalyst loss in the hydroformylation reaction in the prior art and is suitable for the field of Fischer-Tropsch synthesis.

The application provides a preparation method of N,N-dimethylformamide (DMF). The method uses carbon dioxide, hydrogen and dimethylamine as reaction raw materials, and N,N-dimethylformamide is prepared through N-formylation of carbon dioxide under the action of a catalyst. The method uses an oxide supported transition metal as the catalyst, the catalyst composition and the preparation method are simple and low in cost, the reaction is carried out in a fixed bed reactor, the reaction continuity is good, the catalyst and the reaction system are easy to separate, the catalyst is convenient to recycle, the reaction condition is relatively mild, the conversion rate of dimethylamine and the selectivity of DMF are high, and the method provides an economic, environment-friendly and effective way for the synthesis of DMF.

The invention belongs to the technical field of chemical synthesis, and relates to a synthesis method of 2, 3-dimethoxybenzaldehyde. According to the invention, o-dimethoxybenzene reacts with butyl lithium in an organic solvent system, and butyl lithium is used as a strong base to'remove 'hydrogen atoms at specific positions in o-dimethoxybenzene molecules, so that an active intermediate 2, 6-dimethoxyphenyl lithium is formed. The intermediate has electronegative phenyl carbon anions, has relatively strong nucleophilic ability, and provides good reaction sites for subsequent formylation reaction, so that the yield of the target product 2, 3-dimethoxybenzaldehyde can reach a relatively high level, the purity of the target product 2, 3-dimethoxybenzaldehyde also reaches an industrial application standard, and the utilization rate of raw materials and the market competitiveness of the product are greatly improved.

The invention belongs to the technical field of preparation methods of fine compounds, and particularly relates to a preparation method of 3-(3-isopropyl phenyl) butyraldehyde. The method comprises the following steps: by taking a mixed material of m-isopropenyl cumene and phenylcyclopentene as a raw material, carrying out carbonylation reaction under the action of a catalyst; the catalyst is a noble metal carbonyl catalyst; after the reaction is finished, a reaction product is rectified, and isopropenyl isopropyl benzene is obtained; and carrying out formylation reaction on the product, and separating to obtain the 3-(3-isopropyl phenyl) butyraldehyde. The method has the advantages that raw material sources are simplified, physical and chemical properties of products obtained after different components react are changed through different reaction conditions of the different components in the reaction process, the purposes of separation, removal and purification are easily achieved, then the target product is obtained through the hydroformylation reaction, high purity is kept, and the method is suitable for industrial production. And moreover, the conversion rate is more thorough, and the cost can be greatly reduced compared with the existing production technology economically.

The invention discloses a monatomic photocatalytic material as well as a preparation method and application thereof in N-formylation reaction, and aims at innovating a high-energy-consumption and high-risk process for synthesizing traditional N-formylmorpholine and efficiently converting greenhouse gas CO2 into high-added-value chemicals through photocatalytic reaction at normal temperature and normal pressure. According to the catalyst disclosed by the invention, the separation and transfer efficiency of photo-generated charges is remarkably improved by constructing double active sites in which Sb single atoms and MnOx nano-particles are synergistic, in practical application, the catalyst shows excellent performance, the production rate of N-formylmorpholine reaches up to 13.8 mmol g <-1 > h <-1 > under 12-hour illumination, the selectivity exceeds 90%, the activity retention rate exceeds 95% after the catalyst is recycled for 5 times, and the catalyst has a good application prospect. The stability is excellent.

The invention relates to an application of a stabilizer in cobalt-catalyzed hydroformylation reaction, which is characterized in that a compound containing an o-phenylenediamine structure is used as the stabilizer of a cobalt catalyst, and the stabilizer is matched with the cobalt catalyst for use to catalyze olefin and synthesis gas to generate hydroformylation reaction so as to realize recycling of the cobalt catalyst. The stability of a reaction system can be greatly improved, the cost of the catalyst can be reduced, meanwhile, the cobalt catalyst can be prevented from generating precipitates after the reaction, and the catalyst is always kept in a homogeneous phase in the reaction system, is convenient to directly distill and separate and can be directly recycled.

Specifically, a process for controlling heavies in a recycle catalyst stream for use in a continuous hydroformylation process in which olefins are converted with synthesis gas in the presence of a hydroformylation catalyst to form an aldehyde product stream, followed by separation of the catalyst for recycle to the hydroformylation step, comprises removing a crude product stream from a hydroformylation reaction zone, the crude product stream comprising one or more aldehyde products, one or more heavy by-products, a transition metal-organophosphorus ligand complex catalyst, one or more unconverted reactants, and one or more inert lights; providing a water stream; combining the water stream with the crude product stream into an azeotropic vaporizer; removing from the vaporizer an overhead gas stream comprising the one or more aldehyde products, the one or more unconverted reactants, the one or more inert lights, a portion of the water, and a portion of the heavy by-products; a liquid recycle catalyst stream to be sent to the reaction zone, the liquid recycle catalyst stream comprising the transition metal-organophosphorus ligand complex catalyst, a remainder of the aldehyde product, and a remainder of the heavy by-products, as a residue stream from the azeotropic vaporizer, wherein at least 25% of the aldehyde product recovered in the overhead gas stream from the condenser is removed as a water azeotrope.

The present invention addresses the problem of providing a method for producing TCD-DA having less impurities generated as by-products, by depositing materials in a reactor in a batch and performing a hydroformylation rection at a low pressure.　The method for producing tricyclodecane dialdehyde is characterized by depositing a catalyst, dicyclopentadiene, and a solvent in a reactor in a batch, increasing the pressure to 2.0-4.0 MPaG by means of a gas mixture of hydrogen and carbon monoxide, and performing a hydroformylation reaction in the gas mixture in which the molar ratio of hydrogen : carbon monoxide is 90:10 to 100:99.

The invention relates to a preparation method of a pharmaceutical active molecule Azurimoline. According to the present invention, the brand new synthesis method is adopted, and comprises the selective metal-catalyzed Suzuki coupling reaction, the formylation reaction and the condensation reaction, such that the synthesis of the Azaurein can be achieved, and the total yield can be increased to 32.3%. The method is simple in route, the yield is greatly improved compared with that of a traditional method, and efficient and high-selectivity synthesis of Azurimulin is achieved. The novel and efficient preparation method of the pharmaceutical active molecule skeletal muscle relaxant Azumolene and the key intermediate of the pharmaceutical active molecule skeletal muscle relaxant Azumolene is more suitable for industrial production.

The invention relates to the technical field of synthesis of organic compounds, and discloses a synthesis method of boclean flood aldehyde, which is characterized in that 4-tert-butylstyrene is used as a raw material, and the boclean flood aldehyde is prepared through one-step hydroformylation reaction. Rh (CO) 2C5H7O2 and bis (2, 4-dicumyl phenyl) pentaerythritol diphosphite form a composite catalyst, the composite catalyst is matched with triethylamine organic alkali to react under specific process conditions, and a pure product is obtained through vacuum distillation. The method has the advantages of simple process, mild reaction conditions, raw material conversion rate of more than 98%, product yield of more than 80%, purity of more than 98%, easy reagent recovery and small environmental harm, and is suitable for industrial large-scale production.

The present invention relates to a method for synthesizing indole-3-carbaldehyde compounds in a microchannel. Using indole compounds as substrate raw materials, phosphorus oxychloride as a catalyst, and DMF as an aldehyde group source and solvent, a formylation reaction is carried out through a microchannel reactor to obtain the target product indole-3-carbaldehyde compounds. Compared with the prior art, the process route of the present invention is simple, efficient, and low-cost. The reaction is carried out at room temperature, shortening the reaction time, increasing the reaction yield, greatly reducing the reaction energy consumption, and facilitating continuous production on a kilogram scale.

A polyether-functional organosilicon compound and method for its preparation are provided. The method produces a polyether-functional organosilicon compound having a polyether group bonded to a silicon atom via a silicon-carbon bond. The method includes alkoxylation of a carbinol-functional organosilicon compound. The carbinol-functional organosilicon compound may be prepared by hydroformylation of an alkenyl-functional organosilicon compound to produce an aldehyde-function organosilicon compound and subsequent hydrogenation of the aldehyde-functional organosilicon compound.

The utility model relates to the technical field of chemical production, in particular to a separation and recovery device for olefin hydroformylation reaction liquid, which comprises an evaporator and a cyclone separator, the evaporator is provided with an olefin hydroformylation reaction liquid inlet and a gas-liquid outlet, and the gas-liquid outlet of the evaporator is communicated with an input port of the cyclone separator. According to the separation and recovery device for the olefin hydroformylation reaction liquid, provided by the utility model, in the separation process of the reaction liquid, the structures of the synthesis gas input pipe and the cyclone separator are introduced, and the synthesis gas and a liquid-phase material flow which is output by the evaporator and contains a catalyst are simultaneously introduced into the cyclone separator; the internal structure of the cyclone separator is modified, so that the synthesis gas is in full contact with the rhodium catalyst, the rhodium catalyst is protected, the deactivation rate of the rhodium catalyst is reduced, most of the rhodium catalyst is recycled, and the loss of the rhodium catalyst is greatly reduced.

The invention discloses a novel ketorolac synthesis method, which takes 2-(1H-pyrrole-1-yl) propionitrile as a raw material, and ketorolac is obtained through the steps of cyclization reaction, benzoylation reaction, Vanderson reaction, hydrolysis reaction and the like.

The application belongs to the technical field of metal-based catalysts, and discloses a metal Rh-based catalyst, a supported catalyst thereof, a preparation method and application. The metal Rh-based catalyst is formed by coordination of a metal Rh central atom with a butanedione oxime ligand and a triphenylphosphine and substituted derivative ligand, and has a structure shown in formula (1). The supported metal Rh-based catalyst is formed by loading the metal Rh-based catalyst on a porous carrier. The metal Rh-based catalyst and the supported catalyst thereof prepared by the application can realize efficient hydroformylation of isooctene to form iso-nonyl aldehyde, and show high isooctene conversion rate and iso-nonyl aldehyde selectivity.

A hydroformylation process is provided comprising: forming a well-mixed multiphase reaction medium comprising a liquid phase and a gas phase in a hydroformylation reactor, wherein the multiphase reaction medium comprises one or more olefins, molecular hydrogen (H2), carbon monoxide (CO), and a catalyst; in which the agitation power required to provide for a well-mixed multiphase reaction medium is substantially provided for by the gas streams entering the reaction medium comprising both fresh feed and recycle gas.

The invention relates to the technical field of organic alcohol synthesis, and discloses a method for synthesizing isononyl alcohol. The method comprises the following steps: (1) mixing octylene, a rhodium catalyst and a phosphine ligand, then introducing synthesis gas into the obtained mixture, and carrying out hydroformylation reaction to obtain isononanal; (2) in the presence of a hydrogenation catalyst, mixing the isononanal with hydrogen for hydrogenation reaction; wherein the phosphine ligand is selected from two or more of triphenyl phosphite, tris (2, 4-di-tert-butylphenyl) phenyl phosphite, triphenylphosphine, 6, 6 '-{[5, 5'-dimethoxy-3, 3 '-bis (2-methyl-2-propyl)-2, 2'-biphenyl diyl] bis (oxy)} bis [dibenzo (d, f) (1, 3, 2) dioxaphosphoheptane] and 4, 5-bis (diphenylphosphine)-9, 9-dimethyl xanthene. According to the method, the conversion rate of mixed octylene in the hydroformylation process and the selectivity and yield of isononyl aldehyde can be remarkably improved, so that the yield of isononyl alcohol is improved, reaction conditions are mild, and the method has remarkable economic value and wide industrial application prospects.