48 results about "Palladium compound" patented technology

The invention provides a polyurethane epoxy polymer network as well as a preparation method and application thereof, and belongs to the technical field of woven polymer networks, the preparation method comprises the following steps: (1) carrying out reaction on polyalcohol, a small molecule chain extender, diisocyanate and a tridentate ligand to obtain polyurethane; (2) dissolving the obtained polyurethane in an organic solvent, and adding a bivalent palladium compound and a monodentate ligand to carry out a coordination reaction; and (3) adding epoxy resin and a curing agent into the reaction liquid obtained in the step (2), mixing, removing the solvent, and curing to obtain the polyurethane epoxy polymer network. Linear polyurethane and epoxy resin penetrate through each other through palladium coordinated weaving nodes, the mechanical performance and energy absorption capacity of polyurethane and epoxy resin are enhanced through a weaving network, the phase separation trend between two polymers is weakened, the material can bear a higher stress level, the toughness of the material is improved, and the service life of the material is prolonged. And the original strength of the polymer is maintained, and meanwhile, the maximum extensibility and the plastic deformation capacity of the polymer are improved.

The present invention provides a polyurethane epoxy polymer network and its preparation method and application. The present invention belongs to the technical field of braided polymer networks. The preparation method comprises: (1) reacting a polyol, a small molecule chain extender, a diisocyanate and a tridentate ligand to obtain a polyurethane; (2) dissolving the obtained polyurethane in an organic solvent, adding a divalent palladium compound and a monodentate ligand to carry out a coordination reaction; (3) adding an epoxy resin and a curing agent to the reaction solution obtained in step (2), removing the solvent after mixing, and curing to obtain a polyurethane epoxy polymer network. In the present invention, linear polyurethane and epoxy resin are interpenetrated through palladium-coordinated braided nodes, and the braided network is used to enhance the mechanical properties and energy absorption capacity of the polyurethane and epoxy resin, reduce the phase separation tendency between the two polymers, enable the material to withstand higher stress levels, improve its toughness, and improve its maximum elongation and plastic deformation capacity while maintaining the original strength of the polymer.

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 present application discloses a method for preparing an organic carboxylic acid ester by alkoxycarbonylation of an olefinic unsaturated compound, and relates to the technical field of chemical intermediate preparation. The method includes: under the action of a combined catalyst including a palladium compound, a phosphine-containing ligand and an acidic additive, an olefinic unsaturated compound, CO and an alcohol are subjected to an alkoxycarbonylation reaction to generate an organic carboxylic acid ester in the presence of an inhibitor; the olefinic unsaturated compound has a structural formula wherein R is an alkyl group, a carboxyalkyl group or an ester alkyl group having a total carbon atom count of 1 7; the inhibitor is selected from one or more of a phenolic inhibitor, a quinone inhibitor, an aromatic amine inhibitor and a metal salt inhibitor. The present application solves the problem that the conversion rate and yield of the existing olefinic unsaturated compound alkoxycarbonylation reaction are low and the Pd-based catalyst is difficult to recycle, and improves the recovery rate of metal Pd while improving the catalytic activity of the Pd-based catalyst.

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 present invention provides a degradable polyurethane material, a preparation method thereof, and an application thereof. The present invention belongs to the field of polymer chemistry. The preparation method comprises the following steps: (1) reacting a polyol, a small molecule chain extender, a diisocyanate, and a tridentate ligand to obtain a linear polyurethane; 2) performing a coordination reaction between the linear polyurethane obtained in step (1) and a divalent palladium compound and a monodentate ligand; (3) performing a coordination reaction between an o-phenanthroline ligand and a monovalent copper compound; and (4) mixing the solution obtained in step (3) with a diprimary amine compound and the solution obtained in step (2), removing the solvent, and hot pressing to obtain the degradable polyurethane material. The polyurethane material of the present invention has good tensile strength and toughness and has degradability.

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.

Provided is a method for producing a compound having a dicarboxylic acid derivative structure, the method comprising a reaction step in which an olefin, an alcohol, carbon monoxide, and oxygen are reacted in the presence of an ammonium salt and a heterogeneous catalyst formed by supporting a palladium-containing compound on a carrier. Preferably, the ammonium salt is ammonium chloride. Preferably, the olefin is an alicyclic olefin.

The invention provides an intrinsically safe method for preparing a succinate compound through olefin oxidation double carbonylation, which comprises the following steps: taking olefin and alcohol as reactants, taking a palladium compound and a copper compound as bimetallic catalysts, filling a mixed gas of CO, O2 and inert gas, and reacting for 24-72 hours under the conditions that the temperature is 25-120 DEG C and the pressure is 0.1-5 MPa to generate the succinate compound. According to the technical scheme provided by the invention, the potential explosion risk of olefin oxidation double carbonylation can be remarkably reduced, and a safe and feasible technical scheme is provided for high-value utilization of olefin and synthesis gas. The reaction conditions provided by the invention have the advantages of mild reaction conditions, high product yield and the like, and are suitable for industrial production and wide in 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.

Disclosed is a method for preparing an organic carboxylic ester by using a combined catalyst of an aryl bidentate phosphine ligand. The method includes subjecting a terminal olefin, carbon monoxide, and an alcohol to a hydroesterification reaction in the presence of a combined catalyst of a palladium compound, an aryl bidentate phosphine ligand, and an acidic additive, to generate an organic carboxylic ester having one more carbon atom than the terminal olefin.

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.

The invention discloses a process for extracting sponge palladium from palladium-containing wastewater, which comprises the following steps of: filtering the palladium-containing wastewater by filter cloth to remove impurities, and adding a mixed palladium precipitation agent of a complexing agent A and a trapping agent B which are excessive by 50 percent into filtrate; the molar ratio of the complexing agent A to the palladium compound is determined according to the type of the palladium compound, the theoretical reaction ratio of single components and a complex mixture through small tests. Carrying out solid-liquid separation to obtain palladium-containing precipitate, dissolving the precipitate with nitric acid, precipitating palladium with ammonium chloride, dissolving with ammonia water, and repeating the steps for three times; and finally, after the ammonium chloride palladium precipitation slag is pulpified, hydrazine hydrate is used for reduction, the sponge palladium with the purity being at least 99.95% is prepared, and the concentration of tail water palladium is smaller than or equal to 0.5 ppm. The process is high in compatibility and suitable for various kinds of palladium-containing wastewater and various palladium compounds. Compared with a traditional resin and activated carbon adsorption method, the method is low in tail water concentration, high in recovery rate and simple in post-treatment, can also be used for comprehensive recovery and separation of precious metals such as gold, silver, platinum and rhodium, and has remarkable advantages in the aspects of environmental protection and resource utilization.

The present invention provides a method for producing a catalyst that makes it possible to produce vinyl acetate with improved selectivity while ensuring high catalytic activity. Provided is a method for producing a catalyst that is for vinyl acetate production and that contains a carrier, palladium, gold, copper, and an acetate, said method comprising: step 1, which is for impregnating an alkaline solution into the carrier; step 2, which is for causing a solution containing a compound that includes palladium, a compound that includes gold, and a compound that includes copper to come into contact with and impregnate the carrier; step 5, which is for performing a liquid phase reduction treatment in the range of 0-15°C; and step 6, which is for causing the carrier to support the acetate.

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 present invention discloses an electroless palladium plating bath comprising at least a palladium compound, a reducing agent, a complex, and a stabilizer. The stabilizer is an organic compound formed by bonding a divalent sulfur compound to a compound having a heterocyclic structure, and the organic compound lacks thiol groups and disulfide bonds. Therefore, the stabilizer can suppress the reduction in palladium precipitation on nickel-plated films while improving the stability of the plating bath.

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.

One embodiment of the present invention provides an organic compound, a light-emitting element, and a method for synthesizing the organic compound. The method for synthesizing the organic compound includes reacting an organic material with an amine compound and purifying the organic compound by sublimation. The reaction is performed using a palladium compound.

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 discloses a method for rapidly preparing palladium sulfate and palladium nitrate through a mechanical activation method, and belongs to the field of palladium compound product preparation, and the method comprises the following steps: (1) pretreatment: adopting a ceramic tank and ceramic balls as a ball milling container and a medium, the diameters of the ceramic balls comprise two specifications of 5mm and 10mm, and mixing the ceramic balls according to a mass ratio of 3: 1; (2) raw material mixing: mixing palladium powder with the purity of more than or equal to 99.95% and ammonium persulfate according to the mass ratio of 1: (2.36-2.57); (3) preparing slurry; (4) mechanical activation; and (5) post-treatment: filtering and washing a ball-milled product, and selecting a purification path of palladium sulfate or palladium nitrate according to a target product. According to a mechanical activation method, mechanical energy is used for replacing heat energy to serve as reaction driving force, a product with high stability and high consistency can be prepared at normal temperature within a short time, and meanwhile toxic gas of nitric oxide is completely eradicated.

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.