30 results about "Palladium(II) acetate" patented technology

The invention discloses an activated carbon-supported nitrile group ionic liquid-palladium (Pd) catalyst for synthesizing polyketone and a preparation method thereof, wherein the homogeneous membrane of palladium acetate and N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid are supported on pretreated activated carbon. The preparation method comprises the following steps: dissolving palladium acetate and N-valeronitrile-N'-methylimidazolium hexafluorophosphate ionic liquid in solvent acetone to stir, then adding pretreated activated carbon in the solution, continuously stirring, distilling, and drying to obtain the activated carbon-supported nitrile group ionic liquid-Pd catalyst. The invention has the advantages that polar group nitrile groups can increase the binding force between ionic liquid and activated carbon, the nitrile group ionic liquid membrane coating activated carbon can increase the dispersivity of Pd<2+>, reduce the loss of Pd<2+>, prevent the product polyketone from blocking the pores of activated carbon, prevent Pd<2+> from being embedded and increase the reactivity of the copolymerization of carbon monoxide and styrene for preparing polyketone.

A continuous process is provided for selective formation of a vinyl ester by reactive distillation from a corresponding carboxylic acid. Carboxylic acid, vinyl acetate, and a palladium acetate—bidentate ligand catalyst complex are provided and reacted in a typical embodiment. Acetic acid and vinyl acetate are continuously removed from the reaction mixture and vinyl acetate is recycled to the reaction mixture. The vinyl ester product is separated from the vinyl acetate, residual carboxylic acid, residual acetic acid, and catalyst.

The invention relates to a cross coupling reaction of an arenesulphonate substrate and organic titanium. The cross coupling reaction comprises steps as follows: A), after palladium acetate and indole phosphine ligands are utilized to generate a catalyst, the arenesulphonate substrate, aryl titanium, potassium phosphate and an organic solvent are added; B), the components react for 12-24 h at the temperature of 110-130 DEG C, and a biaryl compound is obtained. Compared with the Suzuki coupling reaction, the cross coupling reaction of the arenesulphonate substrate and organic titanium has the advantages that with addition of a small amount of alkali, organic titanium can be catalyzed to have the cross coupling reaction, and the reaction cost can be reduced. Besides, organic titanium is adopted as nucleophile for reaction, and compared with a Grignard reagent required to be stored in an organic solvent in the Kumada coupling reaction, solid organic titanium is easier to apply, has high stability, can be massively synthesized and is easy to store. Compared with organic tin in the Stille cross coupling reaction, organic titanium has lower toxicity and assists in improvement of applicability of the reaction.

The invention discloses a catalyst for preparing polyketone via copolymerization of carbon monoxide and styrene, belonging to the preparation technique of polyketone; wherein, the catalyst comprises palladium acetate, benzoquinone and p-toluene sulfonic acid, sulfamic acid, fluoboric acid or the mixture with Pka less than three; and 4, 4'-dimethyl-2, 2'-bipyridine and rare earth salt of praseodymium phosphate, neodymium phosphate, europium phosphate, dysprosium phosphate, holmium phosphate or the mixture with different proportions are adopted as the ligand of the catalyst. The catalyst for preparing polyketone via copolymerization of carbon monoxide and styrene has the advantages that catalytic activity of the catalyst is improved by one to three times when the 4, 4'-dimethyl-2, 2'-bipyridine and a certain amount of rare earth phosphate salts are added under the condition of the same amount of palladium acetate as the main catalyst; and catalyst cost is effectively reduced.

The present invention relates to bidentate ligand 4,4'-dihydroxy methyl-2,2-dipyridine and an application for preparing and synthesizing silicone. The catalyzer for synthesizing the silicone comprises: acetic acid palladium, para-benzoquinone, paratoluenesulfonic acid, sulfamic acid, fluoboric acid or a mixture thereof, and the bidentate ligand 4,4'-dihydroxy methyl-2,2-dipyridine. Carbon monoxide and styrene which are raw materials is polymerized with absolute methanol which is a solvent, for 1 to 3 hours and at a condition that the catalyzer is existed, the temperature is 20 to 80 DEG C and the pressure is 1 to 10 MPa. The catalyzer is good in catalytic activity, the yield of the silicone is high, and the synthesized silicone is high in relative molecular weight. At a condition that the dosage of main catalyzer acetic acid palladium is the same, the addition of the 4,4'-dihydroxy methyl-2,2-dipyridine causes that not only the catalytic activity of the catalyzer is improved by 1 to 3 times, but also the relative molecular weight of the produced silicone is improved by 2 times.

The invention relates to a catalyst used for synthesizing polyketone by copolymerization of carbon monoxide and cinnamene and a method for synthesizing the same. The catalyst comprises palladium acetate, para-benzoquinone, paratoluenesulfonic acid, fluoboric acid or a mixture of the palladium acetate, the para-benzoquinone, the paratoluenesulfonic acid and the fluoboric acid and 4, 4'-dicarboxylic acid carbethoxyl group-2,2'- dipyridyl. In the invention, carbon monoxide and cinnamene are taken as materials, and absolute methanol is taken as a solvent, and under the conditions of a temperature of between 20 and 80 DEG C and a pressure of between 0.1 and 10Mpa and in the presence of the catalyst, the materials undergo the polymerization reaction for 1 to 3 hours. The catalyst provided by the invention has the advantages of good activity, high yield of the polyketone and high relative molecular mass of the synthesized polyketone; under the condition of the same use level of the main catalyst palladium acetate, the addition of the 4, 4'-dicarboxylic acid carbethoxyl group-2, 2'- dipyridyl can not only improve the activity of the catalyst by 1 to 3 times, but also improve the relative molecular mass of the polyketone by 1 to 2 times.

The present invention relates to a process for preparing polyketone with improved catalytic activity and intrinsic viscosity, and specifically a process for preparing polyketone wherein an organometallic complex comprising acetate-palladium and 1,3-bis[bis(2-methoxy-5-methylphenyl)phosphino]propane is used as a catalyst component, and a mixed solvent of 70 to 90 vol% of acetic acid and 10 to 30 vol% of water is used as a liquid medium.

The invention belongs to the technical field of catalysts and discloses application of a Pd-C nano-composite material to oxidative catalysis of an organic matter. The application of the Pd-C nano-composite material to the oxidative catalysis of the organic matter is characterized in that the organic matter is methanol or formic acid; the Pd-C nano-composite material is obtained by the following processes: (1) uniformly mixing a carbon source material, a stabilizing agent and water, putting in a high-pressure reaction kettle for hydrothermal reaction, filtering and drying to obtain a hydrothermal reaction product; (2) performing heating treatment on the hydrothermal reaction product under H2 / N2 to obtain a spherical carbon material; (3) dispersing the spherical carbon material in the waterto obtain a suspension; dropping the suspension in a palladium acetate solution, performing heating treatment, adding a reducing agent solution, centrifuging, washing and drying to obtain the Pd-C nano-composite material. The Pd-C nano-composite material disclosed by the invention not only is high in catalytic efficiency, good in catalytic performance and low in cost, but also is high in active ingredient loading rate and uniform in dispersion.

A method for preparing a sensitizing material and an organic light emitting diode are provided, the method including: adding C24H16Br2P2 and dichloromethane to a hydrogen peroxide solution to react therewith, dissolving a reactant in a dichloromethane solution and subjecting the solution to a purification with a first silica gel column; adding a purified product, a predetermined electron donor material, palladium acetate, and tri-tert-butylphosphine tetrafluoroborate in sodium tert-butoxide and toluene to react; extracting with dichloromethane and purified by a second silica gel column.

The invention belongs to the technical field of fine chemical industry. A heterogeneous catalyst technology is adopted, a complex catalyst is of a chelate structure and is formed by diphosphine ligandand transition metal compounds, the complex catalyst is used for catalyzing heterogeneous rearrangement of 3-methyl-3-butene-1-alcohol, production of by-products such as isoamyl alcohol and isopreneare inhibited at the same time, the conversion rate of raw materials is increased, and the product selectivity is improved. The invention provides a preparation method of the catalyst. The invention relates to a preparation method of allylic alcohol. Preparation is carried out by adopting a 3-methyl-3-butene-1-alcohol heterogeneous rearrangement technology. The preparation method is characterizedin that heterogeneous rearrangement is completed with the 1,3-bi(diphenylphosphine)propane-palladium-acetate chelate complex as the catalyst and on the conditions that hydrogen exists, the temperatureranges from 50 DEG C to 80 DEG C, and the time ranges from 20 minutes to 2 hours. According to the preparation method, the raw materials are easy to get, the cost is low, the repeated usage time number of catalysts is large, no three wastes are produced, and the energy consumption is low; and because of energy saving, consumption reduction and environmental protection, and the high conversion rate of the raw materials and the high product selectivity, the preparation method is suitable for preparing allylic alcohol and is especially suitable for preparing high-quality allylic alcohol.

The invention provides synthesis of a pH-responding palladium N-heterocyclic carbene chelate and catalytic application thereof. The synthesis process consists of: taking dimethyl sulfoxide as a solvent, adding palladium acetate and a benzoate-containing dibromodiimidazole ionic salt, leaving them to react for 12h at 60DEG C, then raising the temperature to 130DEG C to make them further react for 2h, conducting concentration, carrying out washing with tetrahydrofuran, and performing vacuum drying to obtain a water insoluble N-heterocyclic carbene chelate of palladium; and hydrolyzing the ester group in the chelate by lithium hydroxide, then conducting acidification with hydrochloric acid or hydrobromic acid, thus obtaining the pH-responding palladium N-heterocyclic carbene chelate. The palladium N-heterocyclic carbene chelate synthesized in the invention contains a carboxyl group and has a pH-responding function. The palladium N-heterocyclic carbene chelate has high catalytic activity to the coupling reaction of aryl halides in water, and a catalyst can be separated by adjusting the pH of the reaction system and can be recycled repeatedly. The catalytic system is environment-friendly, thus providing a new path for development of organometallic chemistry and application of N-heterocyclic carbine compounds.

The invention relates to the technical field of catalysts, in particular to a palladium-copper catalyst and a preparation method and application thereof. The preparation method of the palladium-copper catalyst comprises the following steps: preparing palladium nanoparticles: dissolving palladium acetate in absolute ethyl alcohol, and performing treating at the constant temperature of 0-20 DEG C for 24-48 hours to obtain an absolute ethyl alcohol solution containing the palladium nanoparticles; preparing a palladium-modified copper-based metal organic framework: dissolving trimesic acid in the absolute ethyl alcohol solution containing the palladium nanoparticles, adding a copper nitrate aqueous solution, performing uniform mixing, and performing solvothermal reaction to obtain the palladium-modified copper-based metal organic framework; and performing roasting: roasting the palladium-modified copper-based metal organic framework in an inert gas atmosphere to obtain the palladium-copper catalyst taking the porous carbon as the carrier. According to the preparation method, the palladium-copper catalyst with good catalytic activity on furfural can be obtained, and the preparation method is simple in step, does not need to additionally use a reducing agent, and has a better industrial application prospect.

The invention belongs to the field of electrochromic materials, and discloses an EDOT unit-containing polymer, a preparation method thereof, and an application of the polymer as an electrochromic material. The EDOT unit-containing polymer has a structure represented by formula (I) shown in the description. The preparation method comprises the following steps: dissolving EDOT, tetrabutylammonium bromide and an alkali in an organic solvent, uniformly stirring and mixing at room temperature, then adding 2,6-dibromo-9,10-biphenyl anthracene and palladium acetate, carrying out a stirring reaction for 22-24 h at 130-140 DEG C under the protection of nitrogen, and separating and purifying the obtained reaction product to obtain the EDOT unit-containing polymer. The EDOT and a large conjugated aromatic compound are introduced into a polymer structure together, so that the electrochromic property of the polymer is improved.

The invention relates to a catalyst for synthesizing dimethyl oxalate through CO gas phase coupling and a preparation method thereof. Alumina is first modified with additives to prepare modified α-Al2O3, and then impregnated with palladium acetate / acetone solution that has been treated with ultrasonic waves and light irradiation to prepare a catalyst with modified α-Al2O3 as the carrier and noble metal Pd as the active component. The Pd / α-Al2O3 catalyst prepared by modifying the α-Al2O3 carrier in the present invention not only has a low palladium load, but also can improve the utilization rate of methyl nitrite, efficiently synthesize dimethyl oxalate and the like.

The present invention relates to a process for the preparation of a compound of formula (I) said process comprising the steps of: a) reacting a compound of formula (II), with an acylating or a silylating agent to produce a compound of formula (III), wherein P1 and P2 are each independently a protecting group selected from R2—Si—R3R4, or R1CO—, wherein R1 is a group selected from C1-6alkyl or C3-6cycloalkyl, each group being optionally substituted by one or more substituents independently selected from fluoro or C1-4alkyl; R2, R3 and R4 are each independently a group selected from C1-6alkyl or phenyl, each group being optionally substituted by one or more substituents independently selected from fluoro or C1-4alkyl; b) reacting the compound of formula (III) in the presence of palladium acetate or a derivative thereof to produce compound of formula (IV); and c) reacting the compound of formula (IV) with a reducing agent to produce compound of formula (I).

The invention relates to a high-boiling-point all-organic cooling liquid and a preparation method thereof, wherein a molar ratio of a 2-alkoxy imidazoline compound to diol monoether to diol to diol diether is (0.5-2):(1-3):(1-3):(1-3). The preparation method comprises the following steps: adding palladium acetate into excessive micromolecular organic acid solution to prepare micromolecular organicacid palladium-micromolecular organic acid homogeneous catalyst solution; mixing ethylenediamine and diol monoether, adding the micromolecular organic acid palladium-micromolecular organic acid homogeneous catalyst solution, and preparing a 2-alkoxy imidazoline compound under the condition of introducing air; mixing the 2-alkoxy imidazoline compound, diol monoether, diol and diol diether to prepare the high-boiling-point all-organic cooling liquid. According to the high-boiling-point all-organic cooling liquid, a pH regulator, a bactericide, an enzyme inhibitor and an anticorrosive agent do not need to be added additionally, and all indexes meet the GB29743-2013 motor vehicle engine cooling liquid standard.

The invention discloses a compound containing a nitrate functional group and a synthesis method of the compound. According to the compound containing the nitrate functional group, an alcohol substrate of an oxime quinoline guiding group is subjected to a one-pot heating reaction to prepare a beta-position nitric acid esterification product under the catalytic action of palladium acetate and under the conditions that silver nitrite serves as a nitrate source, a selective fluorine reagent serves as an oxidizing agent, tetrabutylammonium hydrogen sulfate serves as a phase transfer catalyst, 1,2-dichloroethane serves as a solvent. The method is mild in condition, carbon-oxygen atom chemical bonds of specific reaction sites can be effectively constructed in one step, the pre-functionalization process is omitted, reaction steps are reduced, and high atom economy is achieved. Meanwhile, the substrate is wide in application range, the alcohol molecular structure is modified, and the generated nitrate functional group-containing compound has a wide application prospect in the fields of medicines and energetic materials.

The invention relates to the field of herbicides, and discloses a preparation method of 2-nitro-4-methylsulfonylbenzoic acid. The preparation method of 2-nitro-4-methylsulfonylbenzoic acid comprises the following steps of: (1) in the presence of alkali and in the presence of a catalyst and a catalyst ligand, carrying out coupling reaction on 2-nitro-4-methylsulfonylchlorobenzene, carbon monoxide and alcohol with the carbon atom number of 1-3 to obtain 2-nitro-4-methylsulfonylbenzoic acid alkyl ester; and (2) carrying out a hydrolysis reaction on the 2-nitro-4-methylsulfonylbenzoic acid alkyl ester obtained in the step (1), the catalyst being one or more of palladium acetate, palladium chloride, palladium nitrate and cupric acetate, and the catalyst ligand being one or more of triphenylphosphine, bis (diphenylphosphino) ethane, bis (diphenylphosphino) propane, bis (diphenylphosphino) benzene and bis (diphenylphosphino) dimethyl xanthene. The preparation method is simple and convenient to operate, and is safe and environment-friendly because nitric acid and sulfuric acid mixed acid is not used as an oxidizing agent, a heavy metal oxidizing agent, toxic raw materials and the like.

The invention discloses a preparation method of a palladium hydroxide carbon carrier catalyst. The method specifically comprises the following steps: firstly, adding palladium acetate into acetone to form a palladium solution, soaking activated carbon with the palladium solution, and carrying out ultrasonic treatment, filtration and drying; adding high-substituted hydroxy propyl cellulose into a methanol solution, injecting the methanol solution into pores of the coated activated carbon by adopting a soaking and filling method, drying, repeatedly filling to obtain activated carbon with blocked pores, soaking in a sodium hydroxide solution, continuously stirring, drying, soaking the above in methanol, drying, repeatedly soaking with sodium hydroxide and methanol for 3-5 times, cleaning and drying to obtain the palladium hydroxide carbon carrier catalyst. According to the method disclosed by the invention, through multiple reactions from outside to inside, high-substituted hydroxy propyl cellulose filled in the pores of the activated carbon can be fully dissolved out, and the exposed palladium is converted into palladium hydroxide step by step, so that the palladium can be uniformly distributed on the inner and outer surfaces of the carbon carrier, and uniform active metal component distribution is formed.

The invention provides a nano core-shell combustion catalyst and a preparation method thereof. The preparation method comprises the following steps: taking cis-5-norbornene-exo-2, 3-dicarboxylic anhydride, hexanediol, p-toluenesulfonic acid and dichloromethane to prepare a dibromide monomer sample; taking pure triamine, cis-5-norbornene-exo-2, 3-dicarboxylic anhydride and a toluene solvent to prepare a cross-linking agent; and taking a dibromide monomer, a catalyst, copper sulfate or palladium acetate to prepare a nano core-shell combustion catalyst. The method has the advantages and positive effects that: the two problems of agglomeration of metal active molecules and incapability of accurately controlling the shell thickness are solved. A dibromide monomer with an active center at the tail end is synthesized through a ring-opening metathesis polymerization reaction, then a cross-linking agent is added for further cross-linking so as to form a combustion catalyst with a compact shell structure composed of linear macromolecular arms and a core containing a ligand structure, the particle size of the combustion catalyst is in the nanometer size, the activity is high, the catalytic combustion efficiency is high, and the preparation method is beneficial to large-scale production.

The invention provides a cesium neopentanoate co-catalyzed aryl borate preparation method, which comprises: dissolving a compound represented by a formula (I) and a diboron compound in an organic solvent, adding an organic solvent in which cesium neopentanoate, palladium acetate and triphenylphosphine are dissolved, and carrying out a reaction to obtain aryl borate, in the formula (I), R1, R2, R3, R4 and R5 being independently selected from H, C1-C10 alkyl, C2-C10 alkenyl, C2-C10 alkynyl, C1-C10 alkoxy, hydroxyl, hydroxyl-substituted C1-C10 alkyl, phenyl and C1-C10 alkylamino respectively; x being selected from F, Cl, Br and I. The preparation method is low in production cost, high in product yield and purity, easy to operate and suitable for industrial mass production.