19 results about "Palladium nitrate" patented technology

This invention belongs to the field of hydrogenation catalyst technology, specifically relating to a Pd-Cu bimetallic catalyst, its preparation method, and its application. Using palladium nitrate and copper nitrate as metal sources, 2-methylimidazole as an organic ligand, and SiO2 as a support, a metal-organic framework precursor is constructed via a solvothermal method. This precursor is then subjected to a two-step heat treatment process: N2 atmosphere pyrolysis and air atmosphere calcination, yielding a PdxCu@SiO2 catalyst with an adjustable Pd / Cu molar ratio. The Cu loading is 4.0 wt.%, and the Pd loading is 0.5~5.5 wt.%. This invention features a mild and easily controllable process, allowing for precise optimization of the catalyst's active site structure. The SiO2 support effectively improves the catalyst's dispersibility and stability. The resulting catalyst exhibits excellent performance in CO2 hydrogenation to methanol, with a maximum CO2 conversion rate of 16.3%, a methanol selectivity of 64.5%, and a space-time yield approximately 18.5 times higher than that of the traditional impregnation method, while also demonstrating excellent long-term operational stability.

The application belongs to the technical field of palladium powder material, and particularly relates to a chemical synthesis method of high-dispersion spherical palladium powder, which comprises the following steps: preparing a palladium-containing solution: adding water and a palladium nitrate solution into a container in sequence, adding ammonia water after stirring uniformly, adjusting the pH to 9-10, and preparing the palladium-containing solution A after sufficient stirring; in volume units, water:ammonia water=100:50-100; preparing a reducing agent solution: adding water, a dispersing agent and hydrazine hydrate into the container in sequence, and preparing the solution B after sufficient stirring; in mass-volume units, water:dispersing agent:hydrazine hydrate=100-300:0.1-0.5:20-40; pouring the solution A into the solution B, slowly stirring, cleaning with water and alcohol in sequence after precipitation, drying in an oven, and screening to obtain the palladium powder. The prepared palladium powder is spherical and has good dispersity, and the specific surface area is 1.5-2.5 m 2 / g.

The invention discloses a nano spherical SnPd oxide, which is prepared by the following steps: firstly, cross-linking tannic acid and formaldehyde at room temperature by taking F127 as a surfactant, then adding stannous sulfate and palladium nitrate dihydrate for chelation, carrying out hydrothermal reaction to obtain a SnPd phenolic hybrid, and finally, calcining to obtain the nano spherical SnPd oxide, namely SP for short. SP is an n-type semiconductor, and the chemical composition of SP is SnO2 and Pd; the diameter of the mesoporous nanosphere is 100-150nm, and the average pore size of the mesoporous nanosphere is 5-7nm. The preparation method comprises the following steps: 1, preparing the SnPd phenolic hybrid SPZ; 2, preparation of an SnPd oxide SP; according to the SP-based hydrogen sensor and the preparation method thereof, the response value is 14.6, the response time is 1.5-2 seconds, the recovery time is 7-10 seconds, and the minimum hydrogen concentration detection is 0.2 ppm; the cycling stability reaches 30 days; the catalyst has selectivity on ammonia gas, methane, carbon dioxide, carbon monoxide and nitrogen dioxide.

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 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.

The invention relates to the technical field of precious metal electroplating, in particular to a preparation method of palladium tetraammine sulfate, which comprises the following steps: palladium powder dissolution: adding palladium powder into concentrated nitric acid, heating to 60-70 DEG C, stirring and dissolving, and filtering to remove insoluble substances to obtain a palladium nitrate solution; preparing a palladium nitrate solid: heating the palladium nitrate solution to 70 DEG C, and concentrating into the palladium nitrate solid under a vacuum condition; preparing tetraamminepalladium nitrate: adding ammonia water into the palladium nitrate solid at normal temperature to react to generate a large amount of white precipitate, and filtering to obtain tetraamminepalladium nitrate; the method comprises the following steps: preparing tetraammine palladium sulfate: adding tetraammine palladium nitrate into a 6-8 mol / L sulfuric acid solution for dissolving, dropwise adding methanol at 90-100 DEG C, decomposing tetraammine palladium nitrate along with nitric acid to gradually generate tetraammine palladium sulfate, and concentrating the system to a solid state to obtain a tetraammine palladium sulfate crude product; purification of palladium tetramine sulfate: adding the palladium tetramine sulfate crude product into deionized water according to the mass ratio of 1: (8-10), stirring and dissolving at normal temperature, adding ammonium sulfate at one time to separate out white precipitate, filtering, transferring to a vacuum oven, and drying to obtain a palladium tetramine sulfate target product.

The invention discloses a preparation method and application of a noble metal-modified nickel-magnesium bifunctional material, and the modification method comprises the following steps: adding a noble metal precursor, namely ruthenium nitrosyl nitrate or palladium nitrate dihydrate, into deionized water, stirring until the mixture is completely dissolved to obtain a noble metal solution, adding a charcoal-based nickel-magnesium bifunctional material into the noble metal solution, stirring, filtering, washing, and drying to obtain the noble metal-modified nickel-magnesium bifunctional material. Transferring the mixed solution into an oil bath pan, and drying while stirring until the moisture is completely evaporated; and transferring the solid substance into a crucible, and roasting under the protection of nitrogen atmosphere to obtain the modified nickel-magnesium bifunctional material. On the basis of the biochar-based nickel-magnesium bifunctional material, precious metal is further introduced for modification to form Ru-Ni-MgO (at) NC with a special structure, so that the anti-poisoning ability of the biochar-based nickel-magnesium bifunctional material in a real smoke environment is greatly enhanced, and the biochar-based nickel-magnesium bifunctional material not only has excellent ICCM performance under an ideal condition, but also has excellent anti-poisoning ability in a real smoke environment. And excellent ICCM performance and long-term stability can be still maintained under the condition of water-containing and oxygen-containing simulated flue gas.

The invention relates to the technical field of gas sensors, and particularly discloses an assembly-pairing-free catalytic combustion sensor and a preparation method thereof. Comprising a detection element, a compensation element and a supporting bracket, wherein the detection element and the compensation element are welded on the same bracket side by side; the detection element is composed of a gamma-Al2O3 carrier loaded with palladium nitrate and a platinum nitrate catalyst (the mass ratio of palladium to platinum is 2: 1-4: 1), and the compensation element is a composite ceramic body without a catalyst and is prepared by mixing seven oxides such as aluminum oxide (65-80%) and silicon dioxide (8-11%) according to a specific proportion. During preparation, the detection element is prepared into slurry through catalyst powder and an ethylene glycol solution, and the slurry is impregnated by a platinum wire coil and electrified to sinter and form; the compensation element is formed by blending slurry with composite oxide powder and an aluminum nitrate solution and adopting the same coil and sintering process. By innovating a compensation element material system and a preparation process, natural matching of initial resistance of the detection element and the compensation element is realized, and a traditional pairing process is thoroughly omitted.

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 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.

This invention belongs to the field of chemical synthesis technology and discloses a lactamide- 13 The preparation method of C includes the following steps: under nitrogen protection, acetaldehyde is added, and K is added. 13 CN, add 1 ml H2O, purge with nitrogen, add 30% sulfuric acid aqueous solution, react to complete, add sodium chloride solid until supersaturated, extract, and evaporate to dryness to obtain a yellow oily liquid; add 2-hydroxypropionitrile-1- 13 C. Add acetic acid, add hexamethylenetetramine, purge with nitrogen, allow the reaction to complete, add palladium nitrate, react for 30 minutes, concentrate, and column chromatography to obtain 2-hydroxypropionamide-1- 13 C. This invention avoids the use of reaction equipment with high airtightness requirements and low-temperature reaction conditions down to -78°C. It directly uses commercially available labeled potassium cyanide as the starting material, and the reaction conditions are mild and easy to implement. Moreover, the two-step reaction yield of this invention is higher than that of the prior art.

The application relates to the field of biological monitoring and particularly belongs to a detection method of chlorogenic acid and application thereof. The method comprises the following steps: taking palladium nitrate, iron nitrate nonahydrate and glutathione as raw materials to prepare FePd2S4 nano-enzyme particles; mixing different concentrations of chlorogenic acid standard solution with acetic acid-sodium acetate buffer solution, H2O2, 3,3',5,5'-tetramethylbenzidine and FePd2S4 nano-enzyme suspension, incubating, measuring the absorbance value at 652 nm, taking the concentration of chlorogenic acid as the abscissa and the absorbance difference as the ordinate, drawing a standard curve and obtaining a linear equation; processing a sample to be measured, extracting chlorogenic acid in the sample to be measured, and preparing a sample solution; taking the sample solution to replace the chlorogenic acid standard solution to repeat the above steps and measure the absorbance value; and calculating the content of chlorogenic acid in the sample to be measured according to the linear equation of S.2. The method has the advantages of simplicity, low cost, high stability, environmental friendliness and the like and is suitable for large-scale preparation.

The invention relates to a method for detecting aflatoxin B1 in edible oil. The method comprises the following steps: 1) preparing PdO nano-enzyme particles by taking palladium nitrate as a raw material; 2) drawing an aflatoxin B1 standard curve and obtaining a linear equation; (3) extracting aflatoxin B1 in to-be-detected edible oil, and preparing to-be-detected liquid; 4) replacing the aflatoxin B1 standard solution with the to-be-measured solution, and measuring the absorbance value of the to-be-measured solution at 652 nm; and 5) substituting the absorbance value into a linear equation, and calculating the concentration of aflatoxin B1 brought into the edible oil to be detected. According to the detection method, the aflatoxin B1 in the edible oil can be rapidly and efficiently detected, and meanwhile, the preparation method of the palladium oxide nano-enzyme particles is simple, low in cost, high in stability, environmentally friendly and suitable for large-scale preparation. In the detection process, the dosage of the required nano enzyme is small, the detection sensitivity is high, the response time is short, and the detection time is greatly shortened.

The invention relates to a potassium tetracyanopalladate synthesis method, which comprises: S1, acid dissolution oxidation: carrying out a dissolution reaction on a metal palladium powder raw material to generate a palladium nitrate-containing aqueous phase solution; s2, precipitation: carrying out precipitation reaction on the aqueous phase solution containing palladium nitrate prepared in the step S1 to generate a palladium cyanide solid intermediate; s3, washing: washing the palladium cyanide solid intermediate generated in the step S2 to remove impurity ions; and S4, reactive crystallization: reacting the palladium cyanide intermediate purified in the step S3 with potassium cyanide, and crystallizing to obtain a potassium tetracyanopalladate product. According to the method, synthesis of potassium tetracyanopalladate can be achieved through a simple and rapid method, and the obtained product is high in purity, uniform in crystal form, good in solubility and suitable for application scenes with high requirements for plating quality in the industries of semiconductors, PCBs, aerospace and the like; the potassium tetracyanopalladate is used as a key raw material of a palladium plating process and is used in the field with high requirements on material performance and appearance.

The invention discloses a PdGa / alpha-MoC bimetallic catalyst as well as a preparation method and application thereof. Respectively dissolving ammonium molybdate, gallium nitrate and palladium nitrate in water, mixing, drying and calcining to obtain a PdGa / MoO3 precursor, and further carbonizing and passivating to obtain the PdGa / alpha-MoC bimetallic catalyst. The prepared PdGa / alpha-MoC catalyst takes noble metal and transition metal as active components, and high dispersion of metal species is realized through high migration ability of molybdenum atoms on a carbide carrier. Wherein the doping of Ga enables the catalyst to have richer oxygen vacancies and acid sites, and the active sites significantly enhance the adsorption and conversion of reactants on the surface of the catalyst. The synergistic combination of bimetallic loading and oxygen vacancy regulation realizes efficient and selective hydrodeoxygenation of vanillin, keeps stable hydrodeoxygenation activity in the whole cycle test, and has good application prospects.

This invention relates to a method for preparing a carbon-supported core-shell platinum-nickel catalyst for proton exchange membrane fuel cells. The method involves thoroughly impregnating a carbon support with nickel salt and palladium nitrate, adjusting the pH of the impregnation solution with sodium hydroxide to obtain a precursor solution for preparing the nickel core, transferring it to a reactor, heating it to 120-180°C, and introducing hydrogen gas for a first pressurized hydrogen reduction to obtain carbon-supported nickel nanoparticles. Subsequently, the carbon-supported nickel nanoparticles are mixed with a platinum nitrate solution, and the solution pH is adjusted with ammonia water for a second impregnation and ultrasonic stirring. The mixture is then transferred to a reactor, heated to 40-90°C, and introduced hydrogen gas for a second pressurized hydrogen reduction to obtain the carbon-supported core-shell platinum-nickel catalyst product. The mass activity of the core-shell platinum-nickel catalyst prepared by this invention exceeds 0.70 A·mg. Pt ‑1 It is superior to the 0.25 A·mg of mainstream platinum-carbon catalysts currently on the market. Pt ‑1 .

The application relates to the technical field of gas sensors, and particularly discloses a catalytic combustion sensor free of assembly pairing and a preparation method thereof; the catalytic combustion sensor comprises a detection element, a compensation element and a supporting bracket, the detection element and the compensation element are welded side by side on the same bracket; the detection element is composed of a gamma-Al2O3 carrier loaded with a palladium nitrate and platinum nitrate catalyst (the mass ratio of palladium to platinum is 2:1-4:1), and the compensation element is a composite ceramic body without catalyst, which is made of seven oxides such as alumina (65-80%) and silicon dioxide (8-11%) mixed in a specific ratio. During preparation, the detection element is formed by slurry prepared by mixing catalyst powder and ethylene glycol solution, platinum gold wire coil immersion and electric sintering; the compensation element is formed by slurry prepared by mixing composite oxide powder and aluminum nitrate solution, and the same coil and sintering process are adopted. The application realizes the natural matching of the initial resistances of the detection element and the compensation element by innovating the material system and the preparation process of the compensation element, and the traditional pairing process is completely saved.

The invention discloses a method for converting sugar into 2, 5-hexanedione by monatomic catalysis, which comprises the following steps: taking glucose as a raw material, and reacting under the synergistic catalysis of a monatomic catalyst Pd-N-C and an auxiliary agent to prepare 2, 5-hexanedione; during the reaction, the hydrogen pressure is 1-2MPa, the reaction temperature is 120-160 DEG C, and the reaction time is 15-60 minutes; the preparation method of the monatomic catalyst Pd-N-C comprises the following steps: mixing palladium nitrate, phenanthroline and absolute ethyl alcohol to react; and heating to 300-700 DEG C at a heating rate of 2 DEG C / min in an N2 atmosphere, calcining for 1-2 hours, naturally cooling, carrying out acid etching for 6-8 hours in a water bath of 60-80 DEG C by using a 0.5 M H2SO4 solution, and carrying out suction filtration, washing and drying to obtain the monatomic catalyst Pd-N-C, and the auxiliary agent is AlCl3 and / or SnCl4. According to the method, the reaction conditions are effectively reduced, and the selectivity of the 2, 5-hexanedione is improved.

The present invention addresses the problem of providing a method for efficiently recovering palladium from a palladium-containing material. [Solution] A method for recovering palladium from a palladium-containing material, comprising: a step of dissolving the palladium-containing material in a nitric acid-containing solution to obtain a palladium nitrate solution; a step of passing the palladium nitrate solution through a resin to adsorb palladium onto the resin; and a step of calcining the resin with the adsorbed palladium to recover palladium, wherein acidic gases remaining in the resin layer during the step of passing the solution are vented.