27 results about "Palladium compound" patented technology

The invention provides a synthesis method of a thioether ligand and a palladium-catalyzed 2-aryl indole compound, and designs an application of the biphenyl thioether ligand and a palladium catalyst in preparation of the 2-aryl indole compound. Indole and arylboronic acid are subjected to a reaction under the action of a palladium catalyst and a biphenyl sulfide ligand, and the structural formula of the biphenyl sulfide ligand is shown in the specification. Ar is phenyl, furyl, thienyl, naphthyl or phenyl substituted by one or more substituent groups; r1 is methyl, methoxyl, fluorine atom, chlorine atom, bromine atom or methyl ester group; r2 is the same or different and is methyl, ethyl, isopropyl, isobutyl, cyclohexyl, benzyl, n-butyl or n-hexyl; r3 is alkoxy, alkylthio, substituted amino or halogen; the palladium catalyst is a divalent palladium compound.

The invention relates to a synthesis method of a 3-olefine acid ester compound. The method comprises the following steps: carrying out contact reaction on an organic phosphine ligand, a palladium compound, conjugated olefin, an alcohol compound and carbon monoxide; wherein the structural formula of the organic phosphine ligand is shown in the specification, and in the structural formula, R0 and R1 are respectively selected from hydrogen, alkyl, alkoxy, halogen or halogenated alkyl; and R2 and R3 are respectively selected from hydrogen or alkyl. The method provided by the invention has the advantages of mild conditions, no need of an acid auxiliary agent, high yield and selectivity of the generated 3-olefine acid ester compound, reduction of corrosion to a reactor, and good application prospect, and the speculation is that the electrical property of phosphorus atoms can be regulated and controlled by using the organic phosphine ligand provided by the invention, so that the reaction activity of the palladium-organic phosphine ligand catalyst is regulated and controlled, and the yield and selectivity of the 3-olefine acid ester compound are improved. Therefore, the palladium-organic phosphine ligand catalyst generated by the ligand and a palladium compound in situ can efficiently catalyze the reaction of conjugated olefin, carbon monoxide and alcohol compounds.

The invention discloses a preparation method of a magnetic metal composite nanomaterial. The invention relates to a preparation method of a metal palladium-iron nano material. The preparation method comprises the following steps: adding spherical nano ferroferric oxide powder into a solvent (water, ethanol, acetonitrile, methylbenzene and the like), carrying out ultrasonic reaction for half an hour, adding pentacarbonyl iron (1-10mmol / L) and palladium compounds (0.1-1mmol / L, palladium chloride, palladium nitrate, palladium sulfate, palladium acetate, bis (dibenzylideneacetone) palladium, bis (acetonitrile) palladium dichloride and the like, and the ratio of the amount of substance of the palladium element to the amount of substance of all iron elements is 0.01-0.1), sealing a reaction container, carrying out ultrasonic reaction for half an hour, and cooling to room temperature to obtain the spherical nano ferroferric oxide. Reacting at 80 DEG C for 2 hours, opening the reaction container, cooling to room temperature, and continuously reacting for 2 hours; and centrifuging the obtained reaction liquid to obtain brown solids, washing the brown solids, and carrying out vacuum drying on the obtained black solids to obtain black powder, namely the palladium-iron composite nanomaterial loaded on the spherical ferroferric oxide. The composite material obtained according to the method is good in dispersity and uniform in particle size, and the size is intensively distributed between 2 nm and 3 nm.

The invention provides a preparation method of octadiene monomethyl ether and a used catalyst, the catalyst comprises a palladium-containing compound and a ligand, the ligand has a structure as shown in a formula I, substituent groups R1, R2, R3, R4, R5, R6, R7, R8, R9, R10, R11, R12, R13, R14 and R15 are independently selected from fluorine, methyl and hydrogen, and at least one substituent group is fluorine. According to the invention, the F atom is introduced to the substituent outside the ring of the ligand, so that the electron withdrawing capability of the ligand is enhanced, the catalytic activity of the catalyst is improved, and the requirements on reaction conditions are reduced. In addition, by introducing F atoms, the steric hindrance effect of the ligand is enhanced, and the selectivity of the catalyst can be improved.

The invention discloses a method for preparing polyadipate from butadiene, and belongs to the field of polymer synthesis. According to the method, 1, 3-butadiene, carbon monoxide and polyol are taken as polymeric monomers, a palladium compound and a phosphine ligand are taken as catalysts, acid is taken as an additive, a hydrocarbonylation esterification polymerization reaction is performed in an organic solvent such as toluene, and a polyadipate product is obtained with high selectivity. And when the ratio of the polyol to butadiene is increased, the polyadipate polyol with hydroxyl at the chain end is controllably obtained, and the obtained product polyadipate can be applied to the field of high polymer materials such as plastics or textiles.

The invention provides a method for preparing carboxylic ester through high-carbon olefin hydrogen ester carbonylation reaction, and relates to the technical field of carboxylic ester preparation. The method comprises the following steps: reacting olefin, alcohol and carbon monoxide in the presence of a homogeneous catalyst to obtain a carboxylic ester-containing reaction solution; the homogeneous catalyst comprises a palladium-containing compound, an organic phosphine ligand and an acidic additive. According to the invention, efficient conversion is realized under mild conditions, and the catalyst has good activity especially for high-carbon olefin with large steric hindrance and built-in double bonds. In addition, high-efficiency hydrogen esterification reaction of high-carbon olefins and separation and reuse of a homogeneous catalyst are realized, and the catalyst still has relatively high catalytic activity after multiple cycles and has a wide industrial application prospect.

The invention belongs to the technical field of organic synthesis, and particularly relates to a method for catalytically synthesizing a dibenzo [b, d] azepine compound by using an N-heterocyclic carbene oxazoline cyclic palladium compound. The invention aims to provide a novel synthesis method of a dibenzo [b, d] azepine compound, and particularly relates to a method for synthesizing the dibenzo [b, d] azepine compound by using a high-catalytic-activity N-heterocyclic carbene oxazoline cyclic palladium compound as a catalyst through a carbon-nitrogen / carbon-carbon bond cascade reaction. The 2, 2 '-dihalogenated biphenyl compound and an N-alkyl substituted allylamine compound are directly synthesized into the dibenzo [b, d] azepine compound in one step. The catalyst used in the invention has high catalytic activity, and the reaction has good compatibility of products and functional groups; the catalyst is easy to synthesize, and the raw materials of the 2, 2 '-dihalogenated biphenyl compound used in the synthesis route are cheap and easy to obtain.

The invention discloses a method for preparing propionate through ethylene hydrogen esterification reaction, which is characterized in that raw materials ethylene, carbon monoxide and low-carbon alcohol are subjected to hydrogen esterification reaction in the presence of a catalyst by taking propionate as a solvent to synthesize propionate, the catalyst is composed of a palladium compound, a naphthyl bidentate phosphine ligand and an acidic auxiliary agent, and the structure of the naphthyl bidentate phosphine ligand is shown in the following formula. Wherein m is 0 or 1, and n is 1 or 2; r1 is selected from phenyl, tertiary butyl, cyclohexyl, 2-pyridyl, 2-thienyl or 2-furyl, and R2 is selected from tertiary butyl, cyclohexyl, 2-pyridyl, 2-thienyl or 2-furyl. According to the method, the naphthyl bidentate phosphine is used as the ligand, the product propionate is used as the reaction solvent, the catalyst activity is high, the yield of the target product propionate is high, and byproducts are few.

The application belongs to the technical field of organic synthesis, and particularly relates to a method for catalytically synthesizing N-substituted-3-methyl indole compounds by using aza carbene oxazoline ring palladium compound. The application aims to provide a new synthesis method for N-substituted-3-methyl indole compounds, specifically, a high-catalytic-activity aza carbene oxazoline ring palladium compound is used as a catalyst to catalyze a direct coupling cyclization reaction of o-dichlorobenzene or o-bromochlorobenzene compounds and allyl arylamine, so as to obtain N-substituted-3-methyl indole compounds. The catalyst used in the application has high catalytic activity, the reaction has good product and functional group compatibility, in addition, the catalyst itself is easy to synthesize, and aryl chlorides used in the synthesis route are cheap and easy to obtain. Therefore, the synthesis route provided in the application has great competitive advantages and industrial production utilization value.

The invention provides a palladium-based catalyst and a preparation method and application thereof, and belongs to the technical field of catalyst preparation.The preparation method of the palladium-based catalyst comprises the following steps that S1, an organic amine dispersing agent is added into a mixed aqueous solution of soluble aluminum salt and soluble cerium salt, the pH is adjusted to be 8-12, and turbid liquid is obtained; s2, heating and stirring the turbid liquid, filtering, washing, drying and roasting to obtain a carrier Al2O3-CeO2; and S3, dropwise adding an aqueous solution of a palladium compound to the carrier Al2O3-CeO2, standing for aging, drying, roasting and reducing to obtain the palladium-based catalyst. The organic amine dispersing agent is added in the preparation process of the catalyst, in the roasting process, the dispersing agent decomposes residual carbon compounds, the specific surface area and dispersity of Al2O3 and CeO2 are improved, and the hydrogenation activity of Pd to acetone is improved.

This invention provides a method for isomerizing 3-butenol compounds in a hydrogen-medium environment to prepare 2-butenol compounds, comprising the following steps: In a hydrogen atmosphere, a mixture of an inorganic base and a 3-butenol compound is passed through a catalyst bed to undergo an isomerization reaction, yielding the 2-butenol compound; the amount of inorganic base added is 0.01–1.5% of the mass of the 3-butenol compound; the catalyst is porous silica supported on palladium, cerium, and selenium. This invention, by adding an additional base to the 3-butenol feedstock, effectively prevents the unsaturated alcohol from converting to a saturated alcohol during the hydrogen-containing isomerization process. Simultaneously, the addition of the electron promoter selenium to the catalyst in this application inhibits the adsorption capacity of the palladium catalyst for hydrogen, thereby reducing the hydrogenation activity of the palladium catalyst while maintaining the stability of the palladium compound cation. Furthermore, the structure promoter cerium improves the diffusivity of palladium, increases the active centers and coordination of palladium, and structurally improves the performance of the palladium catalyst.

The application discloses a kind of mechanical activation method for quickly preparing palladium sulfate and palladium nitrate, belongs to the field of palladium compound product preparation, comprising the following steps: (1) pretreatment: ceramic jar and ceramic ball are used as ball milling container and medium, ceramic ball diameter includes two specifications of 5mm and 10mm, and is mixed according to the mass ratio of 3:1;(2) raw material mixing: palladium powder with purity ≥99.95% and ammonium persulfate are mixed according to the mass ratio of 1: (2.36~2.57);(3) slurry preparation;(4) mechanical activation;(5) post-treatment: after filtering, washing treatment of ball milling product, according to the purification path of target product, palladium sulfate or palladium nitrate is selected.The application replaces heat energy with mechanical energy as reaction driving force by mechanical activation method, and stable and consistent products can be prepared in a short time at room temperature, and nitrogen oxide toxic gas generation is also eliminated.

This invention provides a method for the oxidation reaction of Freon with oxygen in the air. The method includes: co-supporting palladium and cerium compounds on an Al₂O₃ or TiO₂ support, followed by calcination and hydrogen reduction to obtain a palladium-cerium bicomponent catalyst; loading the catalyst into a fixed-bed reactor, introducing a mixture of Freon and air, and carrying out a catalytic oxidation reaction at 300-400°C and atmospheric pressure to convert Freon into CO₂, HF, HCl, and H₂O; the reaction products are then condensed, absorbed by alkaline solution, and adsorbed by activated carbon before being discharged in compliance with standards. This invention addresses the problems of easy agglomeration, poisoning, and short lifespan of single-component palladium catalysts by introducing a cerium component to construct a Pd-Ce synergistic system, effectively inhibiting palladium particle migration and agglomeration, and enhancing the catalyst's resistance to carbon deposition and halogen poisoning. This invention has advantages such as high degradation efficiency, long catalyst lifespan, mild process conditions, and no secondary pollution, and is suitable for the harmless treatment of waste refrigerants and industrial waste gas containing Freon.

The invention provides a bidentate organic phosphine ligand and a preparation method thereof, a novel polyketone catalyst and a use method and application thereof, and belongs to the technical field of catalysts. The structure of the bidentate organic phosphine ligand is as shown in a formula I. The ligand has a rigid annular bridging group, is higher in symmetry and moderate in steric hindrance, and can enhance the coordination stability of a subsequent ligand and palladium, so that the catalytic efficiency and the thermal stability are improved. In the invention, the polyketone polymerization catalyst obtained by the coordination reaction of the ligand and the palladium compound has a novel structure, and tests show that the catalyst has high catalytic efficiency (up to 37.2 kg / (gPd.h)), can tolerate repeated heating and can be repeatedly used for at least four times without obvious activity reduction, thereby solving the problems that the existing polyketone catalyst has low efficiency, poor stability and poor catalytic activity. And repeated utilization is difficult.

Disclosed are a thienopyrimidine derivative and a preparation method therefor. Provided is a method for preparing a compound as shown in formula B, which method is characterized by comprising the following steps: subjecting a compound as shown in formula C with a compound as shown in formula K to a coupling reaction as shown below under a protective gas atmosphere, in a solvent and in the presence of a catalyst and a base, wherein the catalyst comprises a palladium compound and a phosphine ligand. The preparation method of the present invention can improve the yield of products, and reduce the production cost; in addition, the preparation method has simple reaction conditions and a strong process operability, which is beneficial to industrial production and the reduction of the generation of three wastes.

The application provides a sulfide ligand and a synthesis method of a 2-arylindole compound catalyzed by palladium, designs the application of a biphenyl sulfide ligand and a palladium catalyst in the preparation of the 2-arylindole compound. The biphenyl sulfide ligand is used in the reaction of indole and aryl boronic acid under the action of a palladium catalyst and the biphenyl sulfide ligand, wherein the structural formula of the biphenyl sulfide ligand is as follows: Ar is a phenyl, furanyl, thienyl, naphthyl or phenyl substituted by one or more substituents; R 1 is a methyl, methoxy, fluorine atom, chlorine atom, or bromine atom or methyl ester group; R 2 is a methyl, methoxy, fluorine atom, chlorine atom, or bromine atom or methyl ester group; R 3 is an alkoxy, alkylthio, substituted amino or halogen; and the palladium catalyst is a divalent palladium compound.

The invention belongs to the technical field of precious metal palladium catalyst preparation, and discloses a preparation method of a novel N-heterocyclic carbene palladium compound. Specific bivalent palladium is selected as a palladium precursor and directly reacts with ligand N-heterocyclic carbene hydrochloride and 3-chloropyridine under the action of proper reaction conditions and the organic alkali reagent to synthesize the target product novel N-heterocyclic carbene palladium compound, so that the reaction time is shortened, the environmental pollution is reduced, the required energy consumption is low, and the method is suitable for industrial production. The yield and purity of the target product are further improved, the yield is greater than 87.8%, and the purity is greater than 98.5%. The whole reaction process does not involve dangerous chemicals, the operation environment is better and safer, the product quality is reliable, and the method has important economic and social values.

The application discloses a kind of palladium complex excitation agent, by palladium compound and containing double amine group or hydroxyl compound in nonpolar solvent Complexation reaction is made.Therein, the palladium compound is soluble palladium salt, preferably palladium chloride, palladium nitrate or palladium sulfate;The compound containing double amine group or hydroxyl group includes at least one of catechol or o-phenylenediamine;The nonpolar solvent includes at least one of pyridine or n-hexane;The mass ratio of palladium element in the palladium compound and the compound containing double amine group or hydroxyl group is 1:5-5:1;The reaction temperature of the complexation reaction is 50~110 DEG C, pressure is 0.1~0.3MPa, reaction time is 2~5h.The palladium complex excitation agent prepared by the method of the application can be compounded with negative ion emission functional powder, significantly improve the excitation efficiency of composite material, and can reduce harmful radiation.

Presented is a method for making a catalyst that can produce vinyl acetate with very high selectivity while ensuring high catalyst activity. A method for preparing a catalyst for the production of vinyl acetate comprising a carrier, copper, palladium, gold and acetate, the method comprising the following steps: Step 1) a step for impregnating the carrier with an alkaline solution; Step 2) a step for impregnating the carrier with a solution containing a copper-containing compound, a palladium-containing compound and a gold-containing compound; Step 3) a step for carrying out a reduction operation; and Step 4) a step for causing the carrier to carry acetate.

The present application relates to the technical field of metal ion chemistry, and provides a method for reducing an azidomethoxy group, a sequencing method, and a kit. The method for reducing the azidomethoxy group provided in the present application comprises: mixing a compound I comprising the azidomethoxy group, a palladium compound, and an organic phosphine to give a mixed system, and placing the mixed system under a condition suitable for a chemical reaction to reduce the azidomethoxy group of the compound I into hydroxy, wherein the azidomethoxy group has a chemical formula of —O—CA1(N3)-A2, and A1 is selected from one of hydrogen, substituted or unsubstituted hydrocarbyl, substituted or unsubstituted cyclic hydrocarbyl, substituted or unsubstituted heteroatom-containing hydrocarbyl, substituted or unsubstituted heteroatom-containing cyclic hydrocarbyl, substituted or unsubstituted aryl, and substituted or unsubstituted heteroaryl. According to the method provided in the present application, the palladium compound is introduced into the reaction system, so that an oxidation-reduction reaction between the azidomethoxy group and the organic phosphine is accelerated.

The invention provides a preparation method of a Pd-based small-pore molecular sieve catalyst, which comprises the following steps: dispersing a carrier in deionized water to form uniform slurry; dropwise adding a solution of a palladium-containing compound into the slurry, supplementing deionized water to adjust the solid-to-liquid ratio after dropwise adding is completed, stirring, dipping and drying to obtain solid powder; the solid powder is sequentially subjected to first roasting and second roasting, the temperature of the first roasting is 400-550 DEG C, the temperature of the second roasting is 700-800 DEG C, and the Pd-based small-hole molecular sieve catalyst is obtained. The catalyst prepared by the invention not only can strongly adsorb short-chain olefins such as ethylene, but also can be used as an active site to catalytically convert the olefins into harmless substances (such as CO2 and H2O) in the subsequent desorption or reaction process, so that purification of low-concentration olefin pollutants is realized; the problems that a traditional adsorbent only enriches pollutants and cannot eradicate the pollutants, frequent regeneration is needed, and secondary pollution is easily formed are solved.

The invention discloses a large-steric-hindrance triazole carbene monodentate palladium compound containing surplus N and N chelating ligands as well as a preparation method and application of the large-steric-hindrance triazole carbene monodentate palladium compound, and the structural formula of the large-steric-hindrance triazole carbene monodentate palladium compound is shown as a formula I. The preparation method comprises the following steps: (1) adding a compound S and a compound Ar into an organic solvent, reacting at 80-120 DEG C for 12-24 hours, and purifying to obtain large-steric-hindrance triazole salt L containing the surplus N and N chelating ligands; and (2) adding L, palladium salt and alkali into an organic solvent, stirring for 6-12 hours at 50-90 DEG C, and purifying and drying to obtain a target product. Compared with a traditional carbene palladium compound, the large-steric-hindrance triazole carbene monodentate palladium compound containing the surplus N and N chelating ligands has the high electron donating capacity, an N-heterocyclic carbene framework contains a pair of surplus coordination sites, the N-heterocyclic carbene monodentate palladium compound can be stably combined with a palladium center, meanwhile, coordination with metal copper can still be achieved through the surplus coordination sites, and therefore the large-steric-hindrance triazole carbene monodentate palladium compound containing the surplus N and N chelating ligands is obtained. Therefore, the C-H bond arylation reaction of the oxazole derivative is efficiently and synergistically catalyzed by the bimetal.

This invention discloses a method for preparing succinate. The method includes the steps of reacting methyl acrylate with a lower alcohol in a catalytic system to obtain succinate; wherein the catalytic system includes a palladium compound, a quinoline derivative, and a phosphine ligand.

The invention belongs to the field of catalyst preparation, and provides a catalyst for preparing methyl isobutyl ketone (MIBK) and diisobutyl ketone (DIBK) through acetone condensation-hydrogenation and a preparation method of the catalyst. Mixing the prepared aluminum-containing compound aqueous solution and the lanthanide-containing compound aqueous solution, and stirring for a period of time at a certain temperature to obtain a solution A; adding a surfactant in proportion, and stirring for a period of time at a certain temperature to obtain a solution B; adjusting the pH value of the solution B by using an alkaline solution with a certain concentration to obtain a turbid liquid C; stirring the turbid liquid C for a period of time at a certain temperature, filtering, washing, drying and roasting to obtain a solid D; preparing an aqueous solution of a palladium-containing compound with a certain concentration, slowly dropwise adding the aqueous solution into the solid D, standing for a period of time at room temperature, drying and roasting to obtain an oxidation-state catalyst E; and reducing the oxidation-state catalyst E to obtain the catalyst for preparing MIBK and DIBK through acetone condensation-hydrogenation. The catalyst prepared by the invention is suitable for the reaction for preparing MIBK and DIBK through acetone condensation-hydrogenation, and has good acetone conversion rate and MIBK and DIBK selectivity.

Provided is a calcined body that generates photons. The calcined body of the present invention is a calcined body of a composition comprising: (i) alumina; (ii) at least one selected from the group consisting of silica and titanium oxide; (iii) at least one selected from the group consisting of platinum, platinum compounds, palladium, palladium compounds, iridium, iridium compounds, rhodium, and rhodium compounds; and (iv) silicon nitride, in 100 parts by mass of the composition, 5-10 parts by mass of the (iv) silicon nitride is contained.

Disclosed are a catalyst composition, and a use thereof in the preparation of an isomeric carboxylate ester by means of hydroesterification of a highly branched olefin. The catalyst composition comprises a palladium compound, a phosphorus-containing ligand, and an acid promoter. The catalyst composition exhibits excellent activity, selectivity, and stability for a reaction converting highly branched olefins to isomeric carboxylate esters. The method for preparing an isomeric carboxylate ester by means of a hydroesterification reaction using a highly branched olefin as a starting material has a simple synthesis route, mild reaction conditions, and a high target product yield, and is suitable for industrial production.

A semiconductor composite is provided comprising an organic semiconductor and an organo-palladium compound, which can be solution processed into semiconductor thin films for use in organic thin film transistors for carbon monoxide sensing. The semiconductor composite comprises a p-type organic semiconductor having a HOMO energy level ≥ −5.7 eV and an organo-palladium compound of formula PdLaXb, where L is an organophosphine ligand and X is an anion. Also provided are thin films made using the composite films, organic thin-film transistors (OTFTs) incorporating such films, and methods of making same.