34 results about "Decarbonylation" patented technology

The invention belongs to the technical field of coal ethylene glycol, and particularly relates to a process and a device for finely removing impurities from carbon monoxide after cryogenic separation of synthesis gas, the device comprises an impurity removal device, the impurity removal device comprises a desulfurization tank, a dechlorination tank and a decarbonylation tank which are sequentially connected in series, or an adsorption tower which is sequentially filled with desulfurization, dechlorination and decarbonylation adsorbents; the impurity removal device is arranged to remove trace hydrogen sulfide, hydrogen chloride, carbonyl iron and carbonyl nickel in CO after cryogenic separation, so that ppb-level removal of impurities in CO is realized, poisoning of a downstream dimethyl oxalate (DMO) synthesis catalyst is avoided, the service life of the catalyst is prolonged, the production cost of an enterprise is reduced, and the operation stability of the device is improved.

The present application relates to furan preparation technical field, specifically to a kind of furfural decarbonylation catalyst, preparation method and utilize the catalyst preparation furan process.The catalyst includes carrier and active component supported on it, with the mass of the carrier, Pt 0.2%‑0.6%, Co 4%‑8%, Al2O3 74%‑85%, ZrO2 11%‑16%, CeO2 4%‑13%.The present application adopts structural aid ZrO2 and CeO2 to modify Al2O3 carrier, obtains acid moderate composite oxide carrier, can avoid the influence of furfural polymerization and the activity and stability of catalyst;Using Co as auxiliary active component, under the premise of reducing the dosage of main active component Pt, ensure catalytic effect, not only reduce the cost of catalyst, more importantly, it can improve the conversion rate of furfural and furan selectivity in furfural decarbonylation reaction, ensure high furan yield.

The invention belongs to the technical field of organic synthetic chemistry, and discloses a preparation method of an aromatic ketone compound, which comprises the following steps: by taking an unsaturated carbonyl compound obtained by condensing aryl acetaldehyde / acid and aldehyde / ketone molecules as a precursor, carrying out a reaction on the unsaturated carbonyl compound in the presence of a free radical precursor and molecular oxygen under the conditions of illumination and / or heating to obtain the aromatic ketone compound. And carrying out free radical mediated decarbonylation functionalization reaction in an organic solvent to obtain the aromatic ketone compound. The functional group contained in the free radical precursor is introduced to the alpha position of the ketone compound. By improving reaction participants and a reaction mechanism, the aromatic ketone compounds with various structures can be efficiently and highly selectively constructed in one step, the functionalization of the alpha position of the aromatic ketone compounds is synchronously realized, and the preparation method which is simple and convenient to operate, high in atom economy, green and environment-friendly is provided for the aromatic ketone compounds; the obtained compound is especially applicable to the fields of drug synthesis and synthesis of other materials.

The invention discloses a preparation method of a chiral intermediate (S)-3-methyl-1-tert-butoxycarbonyl-1,4-diazepane for treating ocular hypertension, relating to the technical field of pharmaceutical chemicals. The invention comprises the following steps: using 1-benzyl-3-methylpiperidin-4-one as a starting raw material, performing chiral resolution to obtain an intermediate 1, performing an addition-elimination reaction on the intermediate 1 and hydroxylamine hydrochloride to obtain an intermediate 2, performing a Beckmann rearrangement reaction on the intermediate 2 to obtain an intermediate 3, performing an amino deprotection reaction on the intermediate 3 to obtain an intermediate 4, performing an amino protection reaction on the intermediate 4 and di-tert-butyl dicarbonate to obtain an intermediate 5, and performing a decarbonylation reaction on the intermediate 5 to obtain the (S)-3-methyl-1-tert-butoxycarbonyl-1,4-diazepane. The preparation method has the characteristics of readily available raw materials, a simple process and a high product yield, and is suitable for the industrial production of the (S)-3-methyl-1-tert-butoxycarbonyl-1,4-diazepane.

This invention proposes a heterogeneous catalyst and its application in the decarbonylation of alkyl oxalate to alkyl carbonate. The heterogeneous catalyst is a transition metal-modified organic amine-grafted polystyrene resin obtained by grafting chloromethylated polystyrene resin with an organic tertiary amine, followed by modification with a transition metal anion complex. This invention utilizes the heterogeneous catalyst to fully utilize dimethyl oxalate, an important intermediate in the coal-to-ethylene glycol process. By decarbonylating dimethyl oxalate, it can be efficiently converted to dimethyl carbonate and its derived alkyl esters under mild conditions.

The invention relates to a method for decarbonylation alkynylation of ketone, which comprises the following step: in an inert solvent, under the action of a metal catalyst and a ligand, carrying out decarbonylation-reduction coupling reaction on a ketone compound and alkynyl chloride to obtain an alkyne compound. The alkyne is synthesized under the strategy of nickel catalysis, and the method has the advantages of easily available raw materials, simple operation and mild conditions, has very good theoretical guidance significance and practical application value, and conforms to the sustainable green chemistry concept.

This invention relates to the field of gaseous decarbonylation of iron and nickel, specifically to a gaseous decarbonylation protective agent, its preparation method, application, and a method for removing decarbonylation of iron and nickel from methanol synthesis gas. The protective agent comprises an active component, a support, and an auxiliary agent. The active component comprises elemental copper and elemental zinc, and the support comprises kaolin. In this system, the active component is distributed between the kaolin support and adheres to the support. The copper-zinc active system protective agent exhibits good activity and a higher decarbonylation capacity, better protecting the long-term operation of the methanol synthesis catalyst. Kaolin has a large specific surface area and numerous micropores, enabling it to fully physically adsorb carbonylation of iron and nickel, which then catalytically dissociates and deposits afterward at the copper-zinc active centers.

The invention discloses a kind of ethyl benzoate and its preparation method, belong to the field of fine chemical preparation. The preparation method of ethyl benzoate is, in the first step, acrolein and ethyl malonate are subjected to Kneuwengel condensation reaction to generate enester under triethylenediamine catalyst; In the second step, the diene ester and acrolein generated by the first step undergo Diels-Alder reaction to obtain cyclohexene carboxylate substituted with aldehyde group; In the third step, the cyclohexene carboxylate substituted with aldehyde group is subjected to decarbonylation and dehydrogenation reaction to generate ethyl benzoate under metal catalyst. The reaction conditions of the present invention are simple, the catalyst is simple and easy to obtain, and the cost is low. It is a method for synthesizing spices and flavors through a biomass route with great industrialization prospects.

The invention belongs to the technical field of 2-acetylfuran preparation, and discloses a continuous flow synthesis method of 2-acetylfuran, which comprises the following steps: continuously preparing furan by using a furfural decarbonylation method; continuously-flowing acetic anhydride is adopted to absorb continuously-prepared furan, and continuously-flowing raw material mixed liquid is obtained; an acetic anhydride solution of a catalyst is introduced into the continuously flowing raw material mixed solution, a continuously flowing reaction mixed solution is obtained, and the molar ratio of furan to acetic anhydride to the catalyst is 1: (1.05-1.3): (0.05-0.2); the reaction mixed solution is heated to 80-140 DEG C in a continuous flow reactor for a reaction, the reaction pressure is 0.2-0.8 MPa, and 2-acetylfuran is continuously synthesized. No solvent participates in the reaction, continuous post-treatment can be carried out, continuous automatic production is realized, the reaction is completed within a short reaction retention time, the generation of furan ring-opening impurities is greatly reduced, and the reaction selectivity and yield are effectively improved.

The invention relates to a method for synergistically catalyzing a decarbonylation alkylation reaction of alkyl aldehyde through nickel electrochemistry, which comprises the following steps: in an inert solvent, under the action of a metal catalyst, a ligand, an electrode and an electrolyte, carrying out catalytic reaction on an aldehyde compound containing unsaturated alkyl and alkyl bromide to obtain an alkane compound. According to the present invention, the non-activated alkyl aldehyde is adopted as the alkylation reagent, the raw materials are easily available, the operation is simple, the condition is mild, the expensive active metal catalyst or additive is not required to participate in the reaction, the good atom economy is provided, the high value-added alkane compound is obtained under the cheap and easily available current condition, and the synthesis process is environmentally friendly.

The invention provides a preparation method of a melamine grafted chloromethylated bead-based decarbonylation catalyst and alkyl carbonate, and the melamine grafted chloromethylated bead-based decarbonylation catalyst is obtained by carrying out nucleophilic substitution on chloromethylated beads and polyamine to obtain aminated chloromethylated beads, and then carrying out Schiff base condensation on the aminated chloromethylated beads and an aldehyde-terminated melamine-dialdehyde prepolymer to obtain the melamine grafted chloromethylated bead-based decarbonylation catalyst. According to the invention, the melamine with strong coordination ability and chemical stability is chemically grafted to the surface of the chloromethylated resin to construct the multiphase decarbonylation catalyst with stable structure and excellent performance, and the multiphase decarbonylation catalyst shows excellent catalytic activity, selectivity and stability in the decarbonylation reaction of alkyl oxalate; the alkyl oxalate can be efficiently converted into the alkyl carbonate under a mild condition, and a new technical scheme is provided for solving the problems of high-value utilization of the coal-to-ethylene glycol intermediate and green synthesis of the alkyl carbonate.

The application belongs to the field of chemical catalysis, and particularly relates to a catalyst for catalyzing continuous decarbonylation hydrogenation reaction and a preparation method and application thereof. The catalyst is Ni-M / SNTs@MgO, which comprises active metal Ni, auxiliary metal M, carrier SNTs and surface-coated MgO, the auxiliary metal M is one or more of Cu, Co, Zn, Zr and Mo, and the carrier SNTs is a silicon dioxide nanotube; and the preparation method comprises surface-coating MgO on Ni-M / SNTs by using an atomic layer deposition method. The catalyst has low cost, excellent catalytic performance when used for preparing tetrahydrofuran by continuous decarbonylation hydrogenation of furfural, furfural conversion rate is greater than 99%, and tetrahydrofuran selectivity is greater than 90%. The catalyst has no obvious deactivation sign when continuously operated for more than 3000 hours, and has a good industrial application prospect.

The invention relates to a method for producing carbon monoxide by decarbonylation of a compound A, B or C, wherein compound A has the structural formula: R5-C6(R1-4)-[N(CHO)-C6(R1-4')] n -R5', compound B has the structural formula: R5-[C6(R1-4)-N(CHO)-C6(R1-4')] n -R5', and compound C has the structural formula: R5-[C6(R1-4)-N(CHO)-C6(R1- 4')-X] n -R5', wherein R1, R2, R3, R4, R1', R2', R3' and R4' independently of one another are H, D, F, an alkyl group or an aryl group, wherein X is an aliphatic bridge, is an aromatic bridge, has an ether group, has an ester group, has an amide group or has a urethane group, and n is in a range from 1 to 100,000. The invention also relates to a method for producing a synthetic fuel, in which method the carbon monoxide is reduced using hydrogen.

A process for producing a renewable aviation fuel component is described, wherein the process comprises providing a renewable feedstock and subjecting the feedstock to a decarboxylation and / or decarbonylation (DCO) reaction (20) in a DCO zone, thereby obtaining a DCO effluent (21); subjecting at least a portion of the DCO effluent to a hydrotreatment (HT) reaction (30) in a HIT zone, to obtain a hydrotreated effluent (31); subjecting the hydrotreated effluent to a gas-liquid separation (40) to obtain a degassed hydrotreated effluent (41); subjecting at least a portion of the degassed hydrotreated effluent to hydroisomerisation (H-ISO) (50), thereby obtaining a hydroisomerised effluent (51); and subjecting at least a portion of the hydroisomerised effluent (51) to a fractionation (60), and recovering at least the renewable aviation fuel component

The invention relates to the technical field of chemical engineering, in particular to a dimethyl oxalate decarbonylation catalyst and a preparation method and application thereof. A catalyst comprising a carrier; the active component is loaded on the carrier; the active component is one or more of Co, Ni and Pd; the loading capacity of the active component is 0.1%-5%. The preparation method of the catalyst comprises the following steps: S1, pretreating the carrier; s2, dipping the pretreated carrier in a transition metal salt solution, and after dipping, obtaining a first precursor loading body; s3, slowly drying the first precursor loading body, heating and continuously drying to obtain a second precursor loading body; the transition metal salt is one or more of nickel nitrate, palladium chloride and cobalt nitrate; and S4, under the protection of nitrogen, carrying out high-temperature roasting on the second precursor carrier to obtain the catalyst. The catalyst can be used for catalyzing decarbonylation reaction of dimethyl oxalate to prepare dimethyl carbonate, the conversion rate of dimethyl oxalate can reach 95% or above, the highest conversion rate can reach 100%, and the yield of dimethyl carbonate exceeds 90%.

The application discloses a catalyst for co-production of dimethyl carbonate and monomethyl malonate, and a preparation method and application thereof. The catalyst comprises rhodium nanoparticles and grafted ionic liquid coupling agents. When the catalyst is used in a coupling reaction of dimethyl oxalate decarbonylation for preparing dimethyl carbonate and methyl glycolate carbonylation for preparing monomethyl malonate, the modified rhodium nanoparticles can be uniformly dispersed in liquid-phase reaction raw materials, quasi-homogeneous catalysis is realized, CO generated by decarbonylation can be supplied to the carbonylation reaction, atomic utilization is improved, in-situ generated CO can reduce the activation energy required by the carbonylation reaction, the reaction temperature is lower, the selectivity is higher, and the catalytic life of the decarbonylation reaction is prolonged.

The invention relates to a method for preparing an isoquinolinone compound through decarbonylation of imide and intramolecular addition reaction of alkyne under catalysis of cobalt. The key of success of the reaction is to design a new substrate, develop a new catalytic system and realize decarbonylation and intramolecular cyclization addition of the imide. By investigating different catalysts, oxidants, ligands and solvents, the simple and easily available imide compounds are efficiently converted into the polynary ring-fused isoquinolinone compounds with high added value under mild conditions.

The invention provides a method for synthesizing delta-lactam containing a quaternary carbon center through nickel catalysis three-level C (sp3)-H activation. The invention relates to a method for constructing a quaternary carbon center-containing delta-lactam compound by activating and inserting alkyne into a three-level C-H bond of a formamide compound by connecting a phosphorus-oxygen ligand with a nickel-aluminum bimetallic catalyst, and belongs to the technical field of methodology development. The key points of the invention to solve the problem are as follows: (1) the coordination of Al to the substrate activates the substrate; (2) the bridging effect of the ligand guides the metal Ni to generate three-stage C-H bond fracture; (3) the catalyst and a substrate form a stable acyl Ni intermediate with a cyclic structure, and decarbonylation decomposition of the intermediate is inhibited; and (4) a protecting group with proper steric hindrance can repel a three-level C-H bond, so that the protecting group is close to the metal Ni center to be activated.

The invention discloses a metal salt-loaded molecular sieve catalyst as well as a preparation method and application thereof. The catalyst comprises a molecular sieve and nitrogen heterocyclic crown ether alkali metal carbonate grafted on the surface of the molecular sieve. When the catalyst is used for catalyzing decarbonylation of dimethyl oxalate to prepare dimethyl carbonate, the activity is high, the service life of the catalyst is long, and side reactions can be effectively reduced.

This invention discloses a method for preparing aviation fuel components from glycerol and cyclopentadiene, belonging to the field of biomass liquid fuel technology. The method includes: placing glycerol in a reaction vessel and performing a liquid-phase dehydration reaction under HPW catalysis to obtain acrolein; using acrolein as a raw material and methanol, ethanol, or diethyl ether as a solvent, performing a Diels-Alder reaction with cyclopentadiene in a reaction tube without catalysis to obtain 5-norbornene-2-carboxaldehyde; placing 5-norbornene-2-carboxaldehyde in a reaction vessel, adding benzonitrile and RhCl(PPh3)3 for a deoxygenation and decarbonylation reaction to obtain norbornene; placing norbornene in a reaction vessel, adding a molecular sieve catalyst and dichloromethane for a self-polymerization reaction to obtain a mixture composed of nortricycloane, norbornene dimers and trimers; placing the mixture composed of nortricycloane, norbornene dimers and trimers in a reaction vessel, adding a catalyst for a hydrogenation reaction to obtain fuel.

The invention relates to an acid-alkali synergistic molecular sieve carrier for a dimethyl oxalate decarbonylation reaction as well as a preparation method and application of the acid-alkali synergistic molecular sieve carrier. A preparation method of an acid-alkali synergistic molecular sieve carrier for dimethyl oxalate decarbonylation reaction comprises the following steps: (1) mixing a silicon source, an aluminum source, a trivalent metal M source, a template agent, an alkali source and water, and preparing gel; carrying out hydrothermal crystallization, filtering, washing and drying on the gel to obtain a molecular sieve of which the skeleton contains heteroatoms M; (2) roasting the molecular sieve in an oxygen-containing or inert atmosphere to remove the organic template agent to obtain a roasted molecular sieve; and (3) placing the roasted molecular sieve in an inert atmosphere containing water vapor, and carrying out heat treatment to obtain the acid-alkali synergistic molecular sieve carrier. According to the preparation method of the acid-alkali synergetic molecular sieve carrier for the dimethyl oxalate decarbonylation reaction, the defects that in an existing DMO decarbonylation catalyst carrier, acid and alkali active sites are spatially separated, functions are not synergetic, and stability is insufficient are overcome.

This invention provides a palladium-catalyzed method for the decarbonylation and cyclization of o-halobenzoic esters to synthesize 1-substituted phenanthrene compounds. The method involves the decarbonylation and cyclization of o-substituted iodobenzene, norbornadiene, and o-halobenzoic esters in an aprotic solvent under palladium catalysis to yield 1-substituted phenanthrene compounds. This method uses o-halobenzoic esters as cyclizing agents, which not only expands the applicability of cyclizing agents but also offers advantages such as milder reaction conditions, no need for inert gas protection (e.g., nitrogen), and no use of organophosphorus ligands. It is an economical and convenient method for preparing 1-substituted phenanthrene compounds.

The present invention relates to the technical field of organic compound preparation, and more specifically to a method for preparing gramine derivatives in one step by reacting indole-3-acetic acid derivatives with N,N-dimethylformamide under electrochemical conditions. Compared with the prior art, the present invention is the first to achieve a free radical-radical coupling reaction based on the decarboxylation of indole-3-acetic acid derivatives and the decarbonylation of N,N-dimethylformamide under mild electrochemical reaction conditions without transition metals or oxidants. The reaction raw materials are inexpensive and readily available, stable, and safe. The reaction does not require the consumption of organometallic reagents or the use of transition metals. KI is used as an additive, eliminating the need for the use of dangerous peroxides. The method is air-compatible and has the advantages of a one-step reaction, low cost, and simple operation. The method has good application prospects in the field of synthesizing gramine derivatives.

The application provides a melamine-grafted chloromacrolite-based decarbonylation catalyst and a preparation method of alkyl carbonate, wherein the melamine-grafted chloromacrolite-based decarbonylation catalyst is obtained by subjecting chloromacrolite to nucleophilic substitution to obtain amine group chloromacrolite, and then subjecting the amine group chloromacrolite to Schiff base condensation with aldehyde group-terminated melamine-dialdehyde prepolymers. The melamine with strong coordination ability and chemical stability is chemically grafted to the surface of chloromacrolite resin, and a multiphase decarbonylation catalyst with stable structure and excellent performance is constructed. The catalyst exhibits excellent catalytic activity, selectivity and stability in the decarbonylation reaction of alkyl oxalate, and can realize efficient conversion of alkyl oxalate into alkyl carbonate under mild conditions, thereby providing a new technical scheme for solving the high-value utilization of coal-to-ethylene glycol intermediates and the green synthesis of alkyl carbonate.

The invention discloses a method for synthesizing acetate by taking acetic anhydride, olefin and hydrogen as raw materials. The synthesis method of the acetate comprises the following step: in the presence of a palladium catalyst, an organic phosphine ligand and an iodide additive, acetic anhydride, olefin and hydrogen react in a solvent to obtain the acetate. According to the method disclosed by the invention, acetic anhydride, olefin and hydrogen react to synthesize acetic esters with different structures by utilizing a catalytic system consisting of a palladium catalyst, a phosphorus-containing ligand and an iodide additive. According to the method disclosed by the invention, efficient series connection of acetic anhydride decarbonylation, hydroformylation reaction, hydrogenation reaction and esterification reaction is realized, the acetic anhydride is simultaneously used as a carbonyl source and an esterifying agent in the method, a necessary acid environment is provided for the reaction, and atom economical utilization of the acetic anhydride is realized. The method provided by the invention is suitable for various aliphatic terminal alkenes and internal alkenes, and can be used for high-selectivity synthesis of straight-chain acetate products. The invention provides a new way for the utilization of acetic anhydride.

The invention relates to a process for producing carbon monoxide by decarbonylation of a compound A, B or C, wherein the compound A has the structural formula: R5-C6 (R 1-4 ) - [N (CHO) - C6 (R 1-4 ')] n - R5', compound B has the structural formula: R5 - [C6 (R 1-4 ) - N (CHO) - C6 (R 1-4 ')] n - R5', and compound C has the structural formula: R5 - [C6(R 1-4 ) - N(CHO) - C6 (R1-4') - X] n - R5', where R1, R2, R3, R4, R1', R2', R3', and R4' are independently H, D, F, an alkyl radical, or an aryl radical, where X is an aliphatic bridge, an aromatic bridge, an ether group, an ester group, an amide group, or a urethane group, where n is in a range from 1 to 100,000. Furthermore, the invention relates to a process for producing a synthetic fuel in which the carbon monoxide is reduced using hydrogen.

This application belongs to the field of chemical technology, specifically disclosing a catalyst and its preparation method for the gas-phase decarbonylation of dimethyl oxalate to dimethyl carbonate. The catalyst for dimethyl oxalate decarbonylation is a supported solid base catalyst, comprising a support and an active component and / or active agent supported on the support. The active component is an alkali metal carbonate, and the active agent is a transition metal carbonate. The catalyst disclosed in this application has a simple preparation method and is easy to use. It exhibits excellent reactivity in the decarbonylation reaction of dimethyl oxalate. When used in a gas-phase system to achieve the decarbonylation reaction of dimethyl oxalate, it demonstrates excellent conversion and selectivity, achieving a DMO conversion rate close to 100% and a DMC selectivity higher than 95%. Furthermore, it can be recycled multiple times and is suitable for various industrial reaction facilities such as fixed-bed reactors and batch reactors.

The invention provides a heterogeneous catalyst and application of the heterogeneous catalyst in preparation of alkyl carbonate by decarbonylation of alkyl oxalate. The heterogeneous catalyst is transition metal modified organic amine grafted polystyrene resin obtained by grafting chloromethylated polystyrene resin with organic tertiary amine and then modifying the chloromethylated polystyrene resin with a transition metal anion complex. According to the present invention, with the heterogeneous catalyst, the important intermediate dimethyl oxalate in the coal-to-ethylene glycol process can be completely utilized, and the dimethyl oxalate is subjected to decarbonylation so as to efficiently convert the dimethyl oxalate into the dimethyl carbonate and the derived alkyl ester thereof under the mild condition.

The invention discloses a molecular sieve supported ionic liquid catalyst as well as a preparation method and application thereof. The catalyst comprises a molecular sieve and quaternary ammonium methoxyl salt ionic liquid grafted on the surface of the molecular sieve, and by taking the weight of the catalyst as a reference, the content of the molecular sieve is 78%-90%, and the content of the quaternary ammonium methoxyl salt ionic liquid is 10%-22%. The catalyst is used for catalyzing decarbonylation of dimethyl oxalate to prepare dimethyl carbonate, high activity and high selectivity are maintained, and the service life of the catalyst is obviously prolonged.