403 results about "Formylation" patented technology

The invention relates to a crude oil demulsifier, and discloses a natural polysaccharide macromolecule-modified crude oil demulsifier. The demulsifier is prepared by adopting the following operation steps: (1) conducting halogenation modification, carboxylation modification, amination modification, formylation modification, or isocyanic acid esterification modification on polyethylene glycol monomethyl ether; (2) preparing glycidyl dimethyl alkyl ammonium chloride; (3) preparing quaternized polysaccharide; and (4) reacting the modified polyethylene glycol monomethyl ether with quaternized polysaccharide to obtain a product, namely the natural polysaccharide macromolecule-modified crude oil demulsifier. According to the crude oil demulsifier, as the raw material, the natural polysaccharide macromolecule compound has multiple advantages of being wide in source, natural, non-toxic, sustainable, good in usage safety and the like; and the prepared demulsifier has good demulsifying and dewatering effects; in addition, the molecules of the demulsifier contain a great deal of groups of hydroxyl and the like, which have certain chelating capability to metal ions, thus being capable of removing a certain amount of metal ions while demulsifying.

The invention relates to an olefin two-phase hydroformylation method, which consists of three parts: polyether guanidine mesylate ionic liquid (PGMILs) with room temperature solidifiable characteristics, complex catalysts (Rh-TPPTS) formed by RhCl3.3H2O or dicarbonylacetylacetonato rhodium and triphenylphosphine sodium trithionate (TPPTS), and reactants of C6-C14 straight chain 1-olefin, wherein the Rh-TPPTS is dissolved in the PGMILs to form a lower layer catalyst phase, the C6-C14 straight chain 1-olefin or product aldehyde forms an upper layer organic phase, the selectivity of high-carbon aldehyde is 85 to 99 percent, the mol ratio of normal aldehyde to isomerism aldehyde is 2.0 to 2.4, the PGMILs phase containing Rh-TPPTS can be cyclically used for 35 times, the activity and the selectivity are unchanged, the accumulated conversion number (TON) reaches higher than 30000, rhodium flowing to the product phase is 0.04 percent to 0.07 percent, and ultra-long-period catalysis activity and selectivity can be realized.

The invention relates to a preparation method of a polyether-grafted chitosan derivative crude oil desalting demulsifier. The preparation method comprises the following specific steps: firstly, performing formylation modification on polyethylene glycol monoethylether; secondly, preparing glycidyl dimethyl alkyl ammonium chloride; thirdly, preparing quaternarization carboxyalkyl chitosan; fourthly, enabling formylation modified polyethylene glycol monoethylether to react with carboxy alkyl chitosan to obtain the polyether-grafted chitosan derivative crude oil desalting demulsifier. The polyether-grafted chitosan derivative crude oil desalting demulsifier disclosed by the invention is prepared by taking chitosannatural polymeric compounds as raw materials, and has the advantages of wide sources, naturalness, no toxicity, sustainability, good biocompatibility of a product, degradability and the like. The prepared demulsifier is good in demulsifying and dehydrating effect; meanwhile, a demulsifying molecule contains a large amount of carboxyalkyl groups and quaternary ammonium salt groups which have strong combining capacity to metal cation, ions with negative electricity such as naphthenic acid radicals as well as particles of which the surfaces are electronegative, so the polyether-grafted chitosan derivative crude oil desalting demulsifier has capacity of removing oil-soluble salts while demulsifying.

A process for preparing aliphatic alcohols that includes cobalt-catalyzed hydroformylation of olefins, treatment of a hydroformylation mixture with oxygen-containing gases in the presence of acidic, aqueous cobalt(II) salt solutions, separation of a mixture into an aqueous phase comprising cobalt salts and an organic phase comprising the aliphatic aldehydes, and hydrogenation of an aldehyde-containing organic phase wherein the organic phase and treatment with an adsorbent to separate off cobalt compounds prior to hydrogenation.

A process for the catalytic hydroformylation of olefins having from 6 to 24 carbon atoms, in which the hydroformylation is carried out in one or more stage(s) and a mixture comprising at least one olefin and an aldehyde in a molar ratio of aldehyde to olefin of from 0.005:1 to 0.2:1 is used as feed in at least one of these stages which is carried out in the presence of an unmodified cobalt complex as catalyst.

The invention discloses a method for preparing hemostatic cotton through hyaluronic acid crosslinked gelatin and belongs to the field of biomedical materials. The method includes the steps that firstly, a novel hydroformylation hyaluronic acid crosslinking agent is prepared; then, the hydroformylation hyaluronic acid crosslinking agent is mixed with gelatin for foaming, refrigerating and drying are conducted, and the gelatin hemostatic cotton can be obtained after sterilization. According to the method, strong oxidant sodium periodate is utilized to oxidize a carbon-carbon bond of cis diol in the hyaluronic acid so that the hyaluronic acid can react with amidogen for formylation; the hyaluronic acid obtained after formylation serves as a macromolecular crosslinking agent and reacts with the gelatin containing an amino functional group, and the gelatin is made to form a cross-linked structure, so that mechanical performance is enhanced, and the sponge function is given to the gelatin. The gelatin is good in biocompatibility, has the hemostatic and anti-microbial functions and serves as a sponge base material, the hydroformylation hyaluronic acid serves as the crosslinking agent, the prepared hemostatic cotton is good in mechanical performance, safe and non-toxic, the hemostatic property is remarkably improved, a good pain relieving function is achieved, and the effect of promoting healing of injured tissues is achieved.

Prepn. of 1-valeric aldehyde by hydro-formylation of 1-butylene, carbon monoxid and hydrogen, catalyzed by rhodium trichloride and sodium m-triphenylphosphine trisulfonate, in mixed water solution of [Bmin] BF4. Then, the product is obtd. by gravitational settling and liquid separation. This method has advantages of: high yield, high selectivity, good prodn. environment and simple producing process. The product can be used as intermediate of perfumery, 1-pentoric acid and other fine chemicals.

The present invention relates to a continuous hydroformylation process for the production of an aldehyde by hydroformylation of an olefin which comprises: providing a hydroformylation zone containing a charge of a liquid reaction medium having dissolved therein a rhodium hydroformylation catalyst comprising rhodium in combination with carbon monoxide and a ligand; supplying the olefin to the hydroformylation zone; maintaining temperature and pressure conditions in the hydroformylation zone conducive to hydroformylation of the olefin; recovering from the liquid hydroformylation medium a hydroformylation product comprising aldehyde; recovering from the hydroformylation zone a stream comprising the rhodium catalyst; contacting at least a portion of the stream with a solid acidic absorbent under process conditions which allow at least some of the rhodium to become bound to the absorbent; subjecting the rhodium bound to the absorbent, under process conditions which allow desorption of the metal, to a fluid stripping medium comprising hydrogen and solvent; recovering the rhodium hydride catalyst; and recycling the rhodium hydride catalyst to the hydroformylation zone.

The present invention relates to a catalyst composition for hydroformylation and a method for preparing aldehydes using the same, wherein the catalyst composition for hydroformylation comprises: a triaryl phosphine ligand; a phosphine oxide or phosphine sulfide ligand having a specific chemical formula; and a transition metal catalyst. The catalyst composition provides high catalyst activity and stability and selectivity to normal aldehydes when used in the hydroformylation for preparing aldehydes from olefins.

The invention discloses a catalyst for producing aldehyde through hydroformylation of alkene, wherein, the catalyst comprises ionic organic phosphorus ligands and rhodium compounds; the molar ratio of the ionic organic phosphorus ligands and the rhodium compounds is 1 to 20:1; the ionic organic phosphorus ligands are ionic compounds and comprise positive ions and negative ions; the rhodium compounds are neutral rhodium complexes or ionic rhodium compounds; the catalyst is used for catalyzing the reaction of aldehyde preparation through hydroformylation of alkene, wherein, the related alkene is Alpha-alkene that is a straight chain of C3 to C12; and an adopted solvent is room-temperature imidazolyl or pyridyl ionic liquid. The catalyst is characterized by favorable catalytic performance, prolonged service life and circulating application in the liquid phase reaction of aldehyde production through hydroformylation of alkene.

The invention discloses a synthetic process of berberine. The synthetic process comprises the following synthetic route: pyrocatechol and dichloromethane are taken as raw materials and dimethyl sulphoxide is taken as a solvent to synthesize 1,3-benzodioxole; 1,3-benzodioxole is subjected to ViLsmeiar formylation to synthesize heliotropin; heliotropin undergoes nitration through a Henry reaction to generate beta-nitro-3,4-dioxomethenyl styrene; beta-nitro-3,4-dioxomethenyl styrene is subjected to Clemmensen reduction to generate 3,4-(methylenedioxyphenyl)ethylamine; and 3,4-(methylenedioxyphenyl)ethylamine and 2,3-dimethoxy benzaldehyde condense, and the obtained product is reduced to generate N-2,3-dimethoxybenzyl [3,4-(methylenedioxy)phenyl]ethylamine hydrochloride. N-2,3-dimethoxybenzyl [3,4-(methylenedioxy)phenyl]ethylamine hydrochloride is cyclized in a condition of glyoxal, formic acid and copper sulphate to generate berberine hydrochloride. According to the synthetic route, cyanation is avoided and toxicity is reduced. Zinc amalgam is adopted to replace H2Ni and LiAlH4, so that the cost is greatly reduced, the process difficulty is reduced, and the product yield is increased.

This invention is directed to a class of compounds that can be both monodentate and bidentate in their association with a transition metal to form a catalyst for reactions such as the hydroformylation of olefins to produce aldehydes. The compounds contain two phosphorus atoms having different steric and / or electronic nature. In hydroformylation catalysts, the compounds advantageously can produce a variable n / iso product mixture of aldehyde products that can be varied by simply changing process variables such as [H2] / [CO] partial pressure gas ratio or temperature / inert gas partial pressure.

The invention discloses a method for preparing a load-type noble metal nanometer catalyst by a solvent-free microwave-assisted pyrolysis method and application thereof, belonging to the technical field of catalysis. The method comprises the following steps of: fully grinding and mixing a noble metal coordination compound and a vector, and forming the stable load-type noble metal catalyst by the microwave-assisted pyrolysis in an inert atmosphere. The invention has the advantages of simple process, no solvent, low energy consumption in the process, and the like. In the prepared catalyst, Ru, Rh, Re, Pd, Pt, and other particles are evenly distributed on the outer surface of the vector, therefore, the utilization ratio of noble metal particles is improved, the cost of the catalyst is effectively reduced, and the method has potential industrial application value. The load-type noble metal catalyst has favorable catalysis performance in a plurality field of hydrogenation, hydrogenolysis, ammonia synthesis, ammonia decomposition, hydrocarbon synthesis, hydrogenation formylation, and the like, shows the characteristics of high activity, good stability, reduced reaction energy consumption, and the like and has wide application prospect.

A method for preparing aldehyde through olefin hydroformylation is characterized in that compositions in portion by weight of 1 to 10 portions of rhodium complex, 10 to 1,000 portions of phosphine ligand, 0.01 to 1 portion of double long chain surface-active agent and 500 to 5,000 portions of deionized water are added in a reaction kettle with an agitator and a thermocouple, and are completely dissolved; synthetic gas in which the volume ratio of hydrogen to carbon monoxide is equal to 1to 1 is used to carry out substitution 3 to 5 times inside the reaction kettle; 100 to 2,000 portions of olefin is added through pressurization and then the pressure of the synthetic gas is increased to 1 to 6MPa so as to carry out reaction at a temperature of between 50 and 150 DEG C for 2 to 8 hours; and finally, reactants are taken out after cooling, and are separated to obtain the product aldehyde.

Disclosed are novel catalyst systems comprising (1) a diorgano fluorophosphite ligand; (2) rhodium, wherein the ratio of gram moles fluorophosphite ligand (1) to gram atoms of rhodium is at least 1:1; and (3) a Group VIII metal, other than rhodium, or Group VIII metal-containing compound, in an amount effective to reduce the formation of HF during the use of the catalyst system. The presence of the other Group VIII metal decreases the amount of hydrogen fluoride produced during the use of the catalyst system. The hydrogen fluoride originates from very low level degradation of the ligand. Also disclosed are novel catalyst solutions of the aforesaid catalyst system and the use of the catalyst system in the hydroformylation of olefins to produce aldehydes.

The invention discloses a phosphine-containing organic mixed polymer-metal heterogeneous catalyst and its use in butyraldehyde production. The heterogeneous catalyst comprises one, two or three of Rh, Co and Ir as active ingredients and utilizes a multistage pore-structure phosphine-containing organic mixed polymer as a carrier. The phosphine-containing organic mixed polymer is prepared from an alkylene-containing polydentate organic phosphine ligand and a single dentate organic phosphine ligand through copolymerization. The coordination bond-type heterogeneous catalyst is suitable for a fixed bed reactor, a slurry bed reactor, a bubbling bed reactor and a trickle-bed reactor. The heterogeneous catalyst has good effects in hydrogen-propene formylation preparation of butyraldehyde, can produce high-normal / isomeric ratio butyraldehyde with a normal / isomeric ratio of 25 or more and realizes product propane content less than 0.1%. The heterogeneous catalyst has good stability and can be simply and efficiently separated from reactants and products.

The present invention concerns a process for preparing 3,5bis(trifluoromethyl)benzylalcohol by formylation in a solvent of an appropriate organo-magnesium derivative with solid paraformaldehyde and optionally its conversion into a 3,5-bis(trifluoromethyl)benzyl halide.

A multi-phase chiral metal catalyst used for preparing chiral aldehyde product by catalytic asymmetric hydroformylation of olefin is composed of the homogenous chiral ligand chosen from C-2 symmetric chiral biphosphine ligand, N-contained phosphinate type chiral ligand, biphosphinte-type ligand, etc, the active component chosen from Rh, Pt, Ru and Ir, and carrier. Its preparing process is also disclosed.

The invention relates to a preparation method of palbociclib. The method comprises the following steps: carrying out N-acetoacetylation reaction by using cyclopentylamine and an acetoacetylation agent to obtain N,N-di(acetoacetyl) cyclopentylamine (II), carrying out intramolecular condensation on N,N-di(acetoacetyl) cyclopentylamine (II) in the presence of an alkaline reagent to obtain N-cyclopentyl-3-acetyl-4-methyl-6-hydroxy-2-pyridone (III), enabling N-cyclopentyl-3-acetyl-4-methyl-6-hydroxy-2-pyridone (III) to react with a formylation reagent to prepare N-cyclopentyl-3-acetyl-4-methyl-5-formyl-6-chlorine-2-pyridone (IV), carrying out pyrimidine ring reaction by using N-cyclopentyl-3-acetyl-4-methyl-5-formyl-6-chlorine-2-pyridone (IV) and N-(5-(4-tert-butoxy carbonyl-1-hexahydropyrazinyl)-2-pyridyl) guanidine sulfate (V), and then hydrolyzing under the alkaline condition to prepare palbociclib. The preparation method of palbociclib is easily available in raw materials, short in process, simple and convenient to operate and safe and environmentally friendly in process.

The invention discloses a preparation method of 4-chloro-3-(4-ethoxybenzyl)benzaldehyde. The preparation method comprises the following steps that 2-chloro-5-bromobenzoic acid is dissolved in an organic solvent, an acylating chlorination reagent is added into the solution, the mixed solution undergoes a reaction to produce 5-bromo-2-chlorobenzoyl chloride, 5-bromo-2-chlorobenzoyl chloride is dissolved in an organic solvent, the solution is cooled, the cooled solution is added with phenetole and acid catalysts, the mixed solution undergoes a reaction to produce (5-bromo-2-chlorphenyl)(4-ethoxyphenyl)ketone, (5-bromo-2-chlorphenyl)(4-ethoxyphenyl)ketone is dissolved in an organic solvent, the solution is added with a reduction reagent system, the solution undergoes a reaction to produce 4-bromo-1-chloro-2-(4-ethoxybenzyl)benzene, 4-bromo-1-chloro-2-(4-ethoxybenzyl)benzene is dissolved in an organic solvent, a formylation reagent is added into the solution and the mixed solution undergoes a reaction to produce 4-chloro-3-(4-ethoxybenzyl)benzaldehyde. The preparation method utilizes cheap and easily available raw materials and reagents and has a simple synthesis route, simple processes and a high yield.

The invention relates to a preparation method of olefin hydrogen formylated homogeneous phase complex catalyst, in particular to the method of using rhodium chloride hydrate as raw material for preparing tri-(triphenyl phosphine) carbonyl hydrogenation rhodium. In the hydrogen atmosphere, alcohol-water component solvent is adopted, and rhodium chloride hydrate is adopted as raw material, and alkali metal hydrated oxide and borohydride mixture are adopted as deoxidizer to directly compose the objective product. Compared with the traditional method, the invention solves the problems of having low obtaining rate and big rhodium loss. The synthesis obtaining rate of tri-(triphenyl phosphine) carbonyl hydrogenation rhodium reaches more than 99 percent measured by rhodium content, and the toxical impurity content of element Cl is less than 0.02 percent. The homogeneous phase catalyst used for propylene hydrogen formylation aldehyde making reaction has good catalytic activity. The invention is applied to the organic chemical industry field.

A gas phase catalytic hydroformylation process for producing at least one aldehyde product in the presence of a transition metal-ligand complex hydroformylation catalyst and water vapor. Surprisingly, catalyst activity can be sustained by having traces of water vapor in the feed stream. Additionally, additional ligand can be added to replace lost ligand to maintain activity. In addition, it has been found that treatment of the catalyst with a buffer can rejuvenate catalyst activity.

The invention discloses a method for artificially synthesizing galanthamine, which uses isovanillin and bromine as the raw materials. After the raw materials are subjected to substitution reaction, the reaction and industrial chemicla tyramine are subjected to amination and formylation to obtain formamide, the formamide is subjected to reaction to obtain a derivative of racemic narwedine, the derivative of racemic narwedine is reduced into racemic narwedine, N-methylephedrine is used to reduce unsaturated ketone and tartaric acid is used to carry out resolution to obtain levogyrate galanthamine. The method not only can conveniently and rapidly prepare the galanthamine, but also adopts artificial preparation so as to have little limination in the preparation process.

The invention discloses pyrazole amide and pyrazole imine derivatives containing substituted 1, 3, 4-thiadiazole thioether as well as a preparation method and an application of the derivatives. The compounds have the structures as shown in formulae (I) and (II). The preparation method comprises the following steps: by taking substituted hydrazine as an initial raw material, carrying out closed loop, chlorine formylation, oxidation and chloro reaction to obtain pyrazole acyl chloride; carrying out a reaction on 2-amino-5-mercapto-1, 3, 4-thiadiazole and substituted benzyl chloride to obtain 2-amino-5-substituted 1, 3, 4-thiadiazole thioether; and then, carrying out a substitution reaction on 2-amino-5-substituted 1, 3, 4-thiadiazole thioether and substituted pyrazole acyl chloride to obtain the pyrazole amide compound (I) containing substituted 1, 3, 4-thiadiazole thioether; by taking substituted hydrazine as an initial raw material, carrying out closed loop and chlorine formylation to obtain pyrazole aldehyde; carrying out an additive elimination reaction on pyrazole aldehyde and 2-amino-5-mercapto-1, 3, 4-thiadiazole under a backflow condition of anhydrous ethanol to obtain 2-substituted pyrazole imidogen-5-mercapto-1, 3, 4-thiadiazole; and then carrying out a reaction on 2-substituted pyrazole imidogen-5-mercapto-1, 3, 4-thiadiazole and substituted benzyl chloride to generate the pyrazole imine compound (II) containing substituted 1, 3, 4-thiadiazole thioether. The compounds disclosed by the invention have a good inhibiting effect on tobacco mosaic virus and can be used for preparing anti-plant virus drugs.

A process for removing degradation acids from a catalyst solution comprising a phosphorus-containing hydroformylation ligand used in a hydroformylation reaction is described. The process involves using a supported epoxy compound. Also described is a hydroformylation process that includes the degradation acids removal process.

The invention is a production course of making al kinds of organic aldehyde by alkene-hydrogen formylation, which adopts the developed catalyzer, the paste-state bed reaction techinque, the separation of gas and liquid product and paste-state liquid with the catalyzer, the separation of gas and liquid product with paste-state liquid and the catalyzer circulation. The produced lkiquid product in the catalyzing course is separated with the catalyzer, after simply filtered, and the paste-state liquid and the product can directly be the organic aldehyde be flash-evaporation separation or rectification. The organic aldehyde can produce corresponding alcohol by adding hydrogen.

The process of preparing 3-hydroxy propionic aldehyde and 1, 3-propyelene glycol includes: the hydrogenation and formylation of ethylene oxide and synthetic gas inside the organic solvent with the shown expression and in the presence of carbonyl cobalt catalyst; introducing air or oxygen to oxidize the carbonyl cobalt catalyst into cobalt precipitate; centrifugally separating the cobalt precipitate from the solution, filtering and returning the cobalt precipitate to reactor for next reaction; adding deionized water into the filtrate and vacuum distilling the filtrate to obtain water solution containing 3-hydroxy propionic aldehyde; and final hydrogenating to produce 1, 3-propyelene glycol. The said process has high efficiency and low cost.

The invention discloses a synthetic method of pyrroloquinoline quinone. The synthetic method comprises the following steps: carrying out alkali treatment on 2-methoxy-5-nitroaniline hydrochloride as a raw material, so as to obtain a compound 1; carrying out formylation on the compound 1 under a catalysis condition of an ionic liquid, so as to obtain a compound 2; adopting sodium borohydride to reduce the compound 2 to obtain a compound 3; carrying out diazotization on the compound 3, and then enabling action between the diazotized compound 3 and HBF4 to obtain a compound 4; enabling reaction of the compound 4 and 2-methylethyl acetoacetate to obtain a compound 5; treating the compound 5 with formic acid to obtain a compound 6; carrying out amid catalysis and exchange with the ionic liquid on the compound 6 to obtain a compound 7; enabling reaction of the compound 7 and 2-oxodimethyl glutaconate to obtain a compound 8; feeding hydrogen chloride to the compound 8 under the action of Cu(OAc)2*2H2O to obtain a compound 9; carrying out basic hydrolysis on the compound 9 to obtain a compound 10. The synthetic method disclosed by the invention is cheap and accessible in raw materials, stable, high in reaction yield, quick in reaction, and easy for product separation, and is environment-friendly as the catalyst can be recycled.