304 results about "Carbonylation" patented technology

The invention discloses a non-noble metal catalyst, a preparation method thereof and application of the non-noble metal catalyst in preparation of acetic acid through methane oxidation, and belongs to the field of direct conversion and utilization of methane. The active metal of the catalyst is transition non-noble metal MnOx, and the carrier is an MFI type molecular sieve (ZSM-5). The catalyst can directly react methane and oxygen at low temperature to prepare acetic acid without adding a co-reducing agent and carbonylation raw materials (such as H2 and CO). The nanometer MnOx catalyst has the advantages of mild reaction conditions, high acetic acid selectivity and the like, the acetic acid selectivity can reach 81.8%, and the nanometer MnOx catalyst shows good recycling stability.

The invention provides an energy-saving method and device for producing feed-grade propionic acid by using methanol carbonylation acetic acid waste liquid. The methanol carbonylation acetic acid waste liquid comprises the following components in percentage by mass: 40-80% of acetic acid, 20-60% of propionic acid and the balance of high-boiling residues, the method comprises the following steps: (1) evaporating the waste liquid by adopting a film evaporator with a scraper conical structure at the bottom to obtain a first gas phase and first kettle residues, controlling the evaporation rate to be 50-85% in the evaporation process, and keeping the first kettle residues in a flowing state; 2) directly feeding the first gas phase obtained in the step 1) into a recovery rectifying tower to obtain a second gas phase and crude propionic acid, and condensing the second gas phase to obtain acetic acid; 3, the crude propionic acid obtained in the step 2 passes through a resin tower, trace impurity metal ions are removed, and then the feed-grade propionic acid product is obtained.The method is simple in technological process, low in energy consumption and capable of running continuously, the content of the recycled propionic acid is larger than or equal to 99.5%, and the concentration of the impurity metal ions reaches the feed-grade standard.

The present invention relates to the field of organic synthesis, and more particularly to a method for the oxidation of allylic alcohols to α,β-unsaturated carbonyl compounds in the presence of a zirconium catalyst and a hydrogen acceptor.

The invention belongs to the technical field of synthesis of 2, 3-dipicolinic acid, and relates to a catalyst for synthesizing 2, 3-dipicolinic acid as well as a preparation method and application thereof, the catalyst is prepared from a carrier, and active components and auxiliaries loaded on the carrier; the carrier is boron nitride modified aluminum oxide, the active component is palladium-cobalt bimetal, and the auxiliary agent is magnesium; the catalyst comprises the following components in percentage by mass: 0.2 wt%-3wt% of palladium, 0.5 wt%-4wt% of cobalt, 0.05 wt%-0.3 wt% of magnesium, 5wt%-15wt% of boron nitride and the balance of an aluminum oxide carrier. The catalyst is prepared by adopting an ultrasonic-assisted sol-gel method, so that high dispersion and strong interaction of active components are realized. The catalyst shows high catalytic activity, high selectivity and excellent stability in a dichloropyridine carbonylation reaction, carbon monoxide is used as a carbonyl source, the atom economy is high, and the green chemical requirement is met.

The invention discloses a method for preparing isobutyric acid through propylene carbonylation, and belongs to the field of catalytic chemistry. The method comprises the following steps: enabling raw materials containing propylene, carbon monoxide and water to pass through a reactor loaded with an acidic molecular sieve catalyst, and reacting to obtain a product containing isobutyric acid, the acidic molecular sieve catalyst is selected from at least one of a hydrogen type ZSM-35 molecular sieve, a hydrogen type ZSM-11 molecular sieve, a hydrogen type ZSM-5 molecular sieve, a hydrogen type ZSM-57 molecular sieve, a hydrogen type ZSM-23 molecular sieve, a hydrogen type ZSM-22 acidic molecular sieve and a hydrogen type MCM-22 molecular sieve. According to the isobutyric acid preparation method, raw materials are cheap and easy to obtain, system corrosivity is small, products are easy to separate, emission of three wastes is small, a fixed bed process is easy to engineer, and the method is suitable for single-set large-scale production.

The application provides a reverse Markovnikov hydroamination reaction of trifluoromethyl enone under catalyst-free and base-free conditions, uses a sulfonhydrazide compound with good functional group tolerance as a nitrogen source, realizes the introduction of a nitrogen-containing functional group in a green and environment-friendly manner, and synthesizes a series of alpha-sulfonhydrazine-alpha-hexafluoroisopropyl-substituted carbonyl compounds. The method has the characteristics of no transition metal participation, mild conditions, wide substrate universality and the like.

The method for non-targeted mass spectrometric identification of tobacco carbonyl components includes the steps of: (1) preparing a tobacco sample extract; (2) derivatizing the extract with 2,4-dinitrophenylhydrazine (DNPH) to obtain a first tobacco sample; (3) derivatizing the extract with DNPH-d3 instead of DNPH to obtain a second tobacco sample; (4) preparing a mixed tobacco sample; (5) preparing a blank sample; (6) performing UPLC-Orbitrap-HRMS analysis on each of the first tobacco sample, the second tobacco sample, the mixed tobacco sample, and the blank sample to obtain LC-MS raw data; (7) processing the LC-MS raw data to obtain raw mass spectrometry characteristic data; (8) performing multistage filtering on the raw mass spectrometry characteristic data; and (9) performing structural annotation or identification on the finally retained chromatographic peaks to obtain tobacco carbonyl components. By performing multi-stage filtering on the mass spectrometry profile data, the chromatographic-mass spectrometry information of noise or interference components in the raw data set can be rapidly removed to obtain compositional information of aldehyde and ketone chemical components in cigarettes.

An electrochemical cell includes: a cathode having a first catalyst that reduces carbon dioxide to carbon monoxide; an anode; an electrolyte solution containing a reactant and an electrolyte; and a second catalyst that synthesizes a carbonyl compound from the carbon monoxide and the reactant.

The invention relates to the technical field of biological medicine, in particular to a novel amino acid or polypeptide side chain carbonylation modification reagent which can be used as a novel carbonylation reagent in a method for synthesizing gamma-C (sp3)-H bond carbonylation amino acid or polypeptide through palladium catalysis. Substituting ethylene with a novel carbonylation reagent 1-iodine-2-bromine under the action of a palladium catalyst, an additive and a solvent to realize carbonylation and methylation of the amino acid gamma-C (sp3)-H bond. The method disclosed by the invention has the beneficial effects that a novel carbonylation reagent easy to prepare is developed, substrate raw materials are easy to obtain, the operation is simple and convenient, the condition is mild, the substrate application range is wide, and a plurality of carbonylated amino acids and polypeptide derivatives can be efficiently and accurately synthesized at low cost; and a novel method is provided for modification of unnatural amino acids and polypeptide side chains.

The invention belongs to the field of organic synthesis, and provides a synthesis method of a novel acrylate monomer with a bifunctional structure, which comprises the following steps: S1, reacting an ester group-containing alcohol compound with a carbonylation reagent to obtain an intermediate product A; s2, acidifying an alcohol amine compound, and reacting with an acryloyl reagent to obtain an intermediate product B; s3, reacting the intermediate product A with the intermediate product B to obtain a target product C, namely the novel acrylate monomer with the bifunctional structure; wherein R1 is hydrogen or alkyl, R2 is an organic group containing an ester group, m is an integer greater than or equal to 1, R3 and R4 are independently selected from at least one of arene oxyl, halogenated hydrocarbon oxyl or heterocyclic ring containing nitrogen atoms, R5 is alkylene, and L is selected from at least one of halogen atoms, hydroxyl or hydrocarbon oxyl. The method is simple to operate, the reaction process is easy to control and realize, and industrial production is easy.

The application provides a bidentate phosphite polymer, a preparation method and application thereof, and a method for olefin carbonyl synthesis reaction. The bidentate phosphite polymer provided by the application is shown in formula (I) and is copolymerized by a specific bidentate phosphite ligand and 2-vinyl naphthalene. The bidentate phosphite polymer can be used in catalyzing the olefin carbonyl synthesis reaction, can not only ensure the catalytic performance of the olefin carbonyl synthesis reaction, but also can improve the solvent swelling resistance of the polymer, thereby being beneficial to ensuring the catalyst form stability and being beneficial to the stable production of aldehydes synthesized by the olefin carbonyl synthesis.

This invention provides a method for preparing chiral epoxy compounds, chiral β-lactones, and polyhydroxyalkanoates. The method involves three steps: chiral resolution of the epoxy compound, carbonylation of the chiral epoxy compound to prepare a chiral β-lactone, and ring-opening polymerization of the β-lactone. Using this method, polyhydroxyalkanoates with good tensile strength and toughness, as well as a wide processing window, can be prepared. This invention has advantages such as simple steps, low raw material costs, and no need to introduce a second monomer, making it easy to scale up production.

The application discloses a method and device for improving detoxification replacement efficiency of materials containing carbonyl substances, and belongs to the technical field of carbonylation metallurgy safety production. The application adopts the mode of hot nitrogen gas and cold nitrogen gas alternately passivating replacement, replaces the traditional single cold nitrogen gas continuous purging process, and adopts multiple pressure increase-pressure release pulse type operation for each round of replacement; the supporting device is provided with a parallel hot nitrogen gas supply unit and a cold nitrogen gas supply unit, a DCS interlocking control system and an annular tangent air inlet pipeline at the bottom of a storage bin. The application greatly improves the replacement efficiency and completeness of the materials containing carbonyl substances, shortens the replacement time by more than 80%, avoids problems such as material hardening, channeling and burning of material bags caused by continuous high temperature, guarantees continuous, stable and safe operation of carbonylation metallurgy production, and reduces production cost.

The invention discloses a method for preparing high-purity nickel through carbonylation of nickel chloride, belongs to the technical field of carbonylation metallurgy, and solves the problem that a high-purity nickel product cannot be prepared due to the fact that nickel pellets and nickel powder produced through an existing carbonylation method contain many impurities. The construction method comprises the following steps: adding water to dissolve NiCl2, preparing a solution, heating, adding analytically pure AlCl3 with the concentration of 1%-3%, mixing with H2O2, adding ammonia water into the mixed solution to adjust the pH value, continuously reacting, carrying out solid-liquid separation in the solution, extracting the ammonia water mixed solution at the upper end, carrying out carbonylation reaction, converting nickel chloride into carbonyl nickel gas, then converting the carbonyl nickel gas into liquid carbonyl nickel, and carrying out solid-liquid separation in the liquid carbonyl nickel gas. Liquid nickel carbonyl is gasified in a volatilizer and mixed with inert gas Ar, and then the mixture is introduced into a decomposer of nickel shots or nickel powder to produce high-purity nickel. The method is stable, reliable and convenient, preparation of the high-purity nickel with 99.999% (5N) Ni is achieved by optimizing the carbonylation method, mass production of the multipurpose high-purity nickel provides a wide prospect for high-quality development of new materials, and the application prospect is wide.

The invention discloses a preparation method and application of 1, 4-bis (diphenylphosphine) butane platinum dichloride (II), and the preparation method comprises the following steps: (1) mixing absolute methanol and dichloromethane, carrying out deoxidation treatment, and adding 1, 4-bis (diphenylphosphine) butane into the mixture; (2) dissolving potassium chloroplatinite in distilled water, filtering insoluble impurities, dropwise adding the potassium chloroplatinite into the reaction system in the step (1) under the protection of inert gas while keeping a stirring state, and after dropwise adding, heating, refluxing and stirring for reaction; (3) carrying out filter pressing under the protection of inert gas, passing through a silica gel column, and collecting filtrate; (4) concentrating the filtrate, and then adding an organic solvent for pulping; and (5) carrying out filter pressing under the protection of inert gas, washing a filter cake, and carrying out vacuum drying. According to the preparation method, the product yield is high, the purity is high, and the obtained 1, 4-bis (diphenylphosphine) butane platinum dichloride (II) is used for hydrogenation reaction of carbonyl compounds and has good catalytic performance.

Provided is a one-pot process for preparing propionic acid, which comprises (i) treating ethylene with a C1-C6 alkanol, water, and carbon monoxide in the presence of a catalyst system comprising the reaction product of (a) a Group 8 to 10 transition metal compound such as a palladium or ruthenium compound; and (b) an activating anion, at elevated temperature and pressure. The process also provides a facile, continuous process for the preparation of propionic acid via the alkoxycarbonylation of ethylene at elevated temperature and pressure followed by hydrolysis, in one reaction vessel.

This invention relates to the field of methanol production technology. It discloses a methanol production method and system based on ethanol production off-gas, comprising: Step S1: Off-gas from the ethanol carbonylation process is fed to the methanol washing process to obtain CO supplementary washing gas; Step S2: Off-gas from the ethanol hydrogenation process is fed to the methanol washing process to obtain H2 supplementary washing gas; Step S3: CO supplementary washing gas and H2 supplementary washing gas are mixed and fed, and the hydrogen-to-carbon ratio in the mixed washing gas is controlled between 1.8 and 1.9 by gas collection and detection combined with diversion flow control. Ethanol off-gas is used as the main supplementary gas for methanol production feedstock. The combination of off-gas from the ethanol carbonylation process and off-gas from the ethanol hydrogenation process forms a hydrogen-to-carbon ratio closer to that of methanol feedstock gas. After methanol washing, a feedstock gas containing mainly CO and H2, with a small amount of CO2 as a secondary component, is formed, making the methanol system more stable.

The invention relates to phosphine ligands and their use in the carbonylation of acetylene / ethylene for the synthesis of acrylate / propionate. The phosphine ligands according to the invention are represented by formulas I to VIII. The invention describes the use of these phosphine ligands in combination with palladium catalysts for carbonylation reactions of acetylene or ethylene for the production of acrylate or propionate compounds. The processes are characterized by high catalytic efficiency, excellent product yields, outstanding selectivity, and ease of implementation. Particular advantages include improved reaction kinetics due to the optimized ligand structures, economical process control due to high catalyst productivity, and a broad range of applications for various acrylate and propionate derivatives. The invention is particularly suitable for industrial synthesis processes in fine chemical production.

A process comprising: contacting a cobalt salt comprising one or more cobalt halides or cobalt esters with a reducing metal and a coordination compound under conditions to produce a tetracarbonyl cobalt salt of the reducing metal, optionally in the presence of an inert solvent and carbon monoxide; b) contacting a cobalt tetracarbonyl salt of a reducing metal with a porphyrin metal halide in the presence of a coordination compound, optionally in the presence of an inert solvent, under conditions to produce a complex comprising a porphyrin metal cation wherein the coordination compound is coordinated to the metal and an anion containing cobalt tetracarbonyl.

A process for producing and recovering acetic acid in an acetic acid production system is disclosed, the process comprising contacting methanol, methyl acetate, or a mixture of both with carbon monoxide in the presence of a reaction mixture comprising iodide under carbonylation conditions sufficient to form acetic acid. The reaction mixture comprises a carbonylation catalyst, water, and one or more promoters selected from the group consisting of Group I polyphosphates and polyphosphonates and Group II polyphosphates and polyphosphonates, and mixtures thereof. One aspect of the process includes a method for reducing water in an acetic acid production process.

Disclosed in the present invention are a method and system for preparing an oxime via an ammoximation reaction. The method comprises: (1) mixing a carbonyl compound, ammonia, and a circulating catalyst slurry at a specific feed ratio of the carbonyl compound to the circulating catalyst slurry to obtain a mixed stream, and then bringing the mixed stream into contact with hydrogen peroxide for an ammoximation reaction to obtain a reaction slurry; (2) mixing the reaction slurry with an organic solvent and then performing two-phase separation to obtain an oxime-containing organic phase and a catalyst-containing aqueous phase; (3) optionally, washing the organic phase obtained in step (2) with optional water and then performing separation to obtain an organic solvent and an oxime product; and (4) filtering the aqueous phase obtained in step (2) and then returning same to step (1) to provide at least part of the circulating catalyst slurry. The method and system for preparing an oxime according to the present invention significantly prolong the service life of a catalyst, improve the operating stability of a system, reduce the consumption of catalyst, and improve the quality of the prepared oxime product.

The invention discloses a catalyst for preparing methyl acetate through carbonylation of dimethyl ether as well as a preparation method and application of the catalyst, and belongs to the technical field of industrial catalysis. A preparation method of a catalyst for preparation of methyl acetate through carbonylation of dimethyl ether comprises the following steps: placing a template agent-containing sodium mordenite molecular sieve in low-temperature plasma, and carrying out modification treatment under a first preset condition to obtain a modified sodium mordenite molecular sieve; performing ammonium ion exchange treatment on the modified sodium-type mordenite molecular sieve to obtain an ammonium-type mordenite molecular sieve; and placing the ammonium type mordenite molecular sieve in low-temperature plasma, and carrying out modification treatment under a second preset condition to obtain the catalyst, wherein the first preset condition comprises that modification treatment is carried out under gradient voltage; the second preset condition comprises modification treatment under a constant voltage. According to the preparation method disclosed by the invention, the acid density, the micropore specific surface area and the micropore volume of the mordenite can be improved, and the mordenite shows higher catalytic activity and stability in a reaction for preparing methyl acetate through dimethyl ether carbonylation.

The invention discloses a synthesis method of a polysubstituted cyclopropyl carbonyl derivative, and belongs to the technical field of organic synthesis and the technical field of medicine synthesis. The method comprises the following steps: (1) taking substituted olefin as a raw material, and obtaining alpha-chlorocyclobutanone through [2 + 2] cycloaddition and reduction reaction; and (2) carrying out rearrangement reaction on the alpha-chlorocyclobutanone and different types of Grignard reagents or organic lithium reagents to obtain the polysubstituted cyclopropyl carbonyl derivative. The synthesis method provided by the invention has the advantages of wide substrate range, good functional group compatibility, mild reaction conditions, no need of preparation of active intermediates or use of expensive transition metal catalysts, simple operation, capability of obtaining various types of cyclopropyl carbonyl compounds, and the like. The practicability of the method is further shown through later-stage functional group modification of complex bioactive molecules and abundant derivatization of polysubstituted cyclopropyl carbonyl products of the complex bioactive molecules.

The invention discloses a synthesis method of a high-abundance C-13 ethylene oxide compound, which comprises the following steps: (1) carrying out reaction on 13CH3I and diphenyl sulfide to obtain [13C] diphenylmethyl iodide; and (2) reacting the [13C] diphenylmethyl iodide with a carbonyl compound to obtain the high-abundance [13C] ethylene oxide compound. Diphenyl sulfide is adopted to replace dimethyl sulfide, the obtained [13C] methyl diphenyl sulfonium iodide avoids C-13 loss in the subsequent reaction process, and the abundance of C-13 is effectively improved.

The invention belongs to the field of chemical synthesis, and discloses a methanol carbonylation reaction assembly and application thereof in an acetic acid synthesis method and a production system. The methanol carbonylation reaction assembly comprises a shell, a gas feeding pipe, a gas-liquid mixed feeding pipe, a methanol liquid feeding pipe, a liquid injection pipe, a liquid distributor, a gas distributor and liquid outlets, the liquid outlets are distributed in the upper portion and the top of the shell, and the liquid outlet in the upper portion of the shell is connected with the gas-liquid mixed feeding pipe. And the gas-liquid mixed feeding pipe is also communicated with the other end of the gas feeding pipe. The production system provided by the invention comprises the methanol carbonylation reaction assembly provided by the invention. The methanol carbonylation reaction assembly and the production system can be used for acetic acid synthesis. The methanol carbonylation reaction assembly is good in gas-liquid mixing effect, a reaction liquid part recycling system is beneficial to improving the reaction efficiency and the conversion rate, energy consumption is remarkably reduced, and the methanol carbonylation reaction assembly is suitable for acetic acid synthesis.

The application discloses a bubble column reactor for preparing methyl propionate, a reaction system and a method. The reactor comprises a bubble column body, a gas distributor and a sieve plate. The application divides the inner cavity of the reactor into multiple spaces through multiple sieve plates, and performs CO segmented feeding on the reaction of synthesizing methyl propionate from a carbonyl group through multiple gas distributors, so that the partial pressure ratio of CO and ethylene in the reactor is reduced, the gas-liquid ratio is obviously reduced, and the reaction conversion rate is obviously improved.

The application discloses a catalyst for preparing beta-lactone by epoxide carbonylation and a preparation method and application thereof. The catalyst is composed of a homogeneous metal complex and a heterogeneous supported cobalt catalyst. The homogeneous metal complex is one of a porphyrin metal complex and a Schiff base metal complex. The heterogeneous supported cobalt catalyst is composed of a metal center and an organic phosphine ligand polymer connected with the metal center through a coordination bond. The metal center is cobalt, and the organic phosphine ligand polymer is a cross-linked polymer containing a repeating phosphine ligand unit. The metal center is connected with P atoms in the organic phosphine ligand polymer through a coordination bond. The cobalt center forms a stable coordination structure through a ligand, and the coordination layer of cobalt satisfies an electronic saturation state. The cobalt catalyst has high stability, is suitable for a fixed bed or a slurry bed reactor, is favorable for realizing continuous and stable operation of an epoxide carbonylation reaction, and has good industrial amplification potential.

The invention belongs to the technical field of organic synthesis, and discloses a method for synthesizing an alkyl halide from a carbonyl compound through a one-pot method, the carbonyl compound (aldehyde or ketone) is used as a raw material, hydrazinium is added, on one hand, the hydrazinium can be used as a reducing reagent for reducing carbonyl, and on the other hand, the hydrazinium can be used as a halogen donor for a halogen substitution reaction; an efficient conversion effect is achieved in the presence of an additive, and the synthesized alkyl halide derivative can be used as an important raw material and an intermediate for organic synthesis and drug synthesis. The method is simple and convenient to operate and good in functional group compatibility, and a new thought is provided for synthesizing polysubstituted alkyl halide derivatives.

This invention discloses a method for synthesizing a mordenite molecular sieve-encapsulated metal catalyst for the synthesis of ester compounds, comprising the following steps: 1) mixing a water-soluble metal salt sequentially with an amine ligand and an alkali metal hydroxide to obtain a preliminary mixture solution; 2) mixing the preliminary mixture solution sequentially with an aluminum source and a silicon source to obtain a gel; 3) crystallizing the gel at 160–180 °C, cooling after crystallization, and separating to obtain an initial solid; 4) drying and calcining the obtained initial solid to obtain a preliminary molecular sieve; 5) placing the preliminary molecular sieve in an inorganic ammonium salt solution for ion exchange, separating the reactants after ion exchange to obtain a solid, drying and calcining the solid to obtain a mordenite molecular sieve-encapsulated metal catalyst for the synthesis of ester compounds. The catalyst obtained by this synthesis method can be used for the carbonylation of dimethyl ether to produce methyl acetate, exhibiting a relatively fast reaction rate while maintaining a high conversion rate of dimethyl ether.