202 results about "Palladium chloride" patented technology

The invention discloses a catalyst and method for preparing 3-methyl-2-aminobenzoic acid through continuous catalytic hydrogenation, and the method comprises the following steps: pretreating an activated carbon carrier by using pretreatment reagents such as nitric acid and hydrogen peroxide to remove impurities in the carrier; modifying the carrier by using an auxiliary component 1 such as sodium carbonate, stannic chloride, potassium carbonate and lanthanum nitrate, and then roasting and reaming; and finally, active components such as platinum chloride and palladium chloride are mixed and impregnated with an auxiliary component 2 such as oxalic acid, polyethylene glycol-400, sodium metavanadate and polyvinylpyrrolidone, the auxiliary component 2 promotes dispersion of the active metal, and the auxiliary component 2 and the auxiliary component 1 have a synergistic effect, so that the active metal is loaded more uniformly and firmly, and the obtained catalyst has higher activity and selectivity and longer service life. The catalyst is applied to preparation of 3-methyl-2-aminobenzoic acid through catalytic hydrogenation in a fixed bed reactor, the reaction can be continuously and automatically controlled, the three wastes in the reaction process are few, the yield of a target product is high, the service life of the catalyst is long, and the catalyst is suitable for industrial production.

The invention discloses a GO-TAPP microporous composite material as well as a preparation method and application thereof, and belongs to the technical field of biological medicines. The preparation method comprises the following steps: adding 5, 10, 15, 20-tetra (4-ethynylphenyl)-porphyrin, bis (triphenylphosphine) palladium chloride and cuprous iodide into tetrahydrofuran, uniformly mixing in a dark place, adding graphene oxide and triethylamine, mixing in a dark place, carrying out a reaction to obtain a black solid after the reaction is finished, and washing and drying the black solid to obtain the GO-TAPP microporous composite material. The GO-TAPP microporous composite material taking the graphene oxide and the porphyrin as structural units can resist bacteria synergistically through PTT and PDT, and is good in biocompatibility and free of toxic and side effects, and the hemolysis rate on cells is lower than 2%. The GO-TAPP is in a sheet shape and can be directly cut, pasted and directly used, post-processing is not needed, and the application prospect of the GO-TAPP is improved.

The invention belongs to the technical field of conductive microsphere preparation, and particularly relates to a preparation method and application of conductive microspheres with convex particles on the surfaces. The preparation method comprises the following steps: acidizing resin microspheres by using imidazole disulfate ionic liquid, and combining the acidized resin microspheres with aminated activated carbon through chemical bonds to obtain microspheres with convex particles on the surfaces; and sequentially carrying out stannous chloride sensitization, palladium chloride activation and chemical nickel plating on the microspheres with the convex particles on the surfaces to obtain the conductive microspheres with the convex particles on the surfaces. The conductive microspheres with the raised particles on the surfaces can generate more and more effective local contact points in the crimping process, so that the connection resistance is obviously reduced, and the excellent conductive performance is realized.

The invention provides a method for preparing a colloidal palladium activating solution by using a microfluidic method and the colloidal palladium activating solution, the method comprises the following steps: S1, preparing a palladium salt solution, a first tin salt solution and a second tin salt solution, the palladium salt solution is a solution containing palladium chloride and concentrated hydrochloric acid, and the first tin salt solution is a solution containing palladium chloride and concentrated hydrochloric acid; the first tin salt solution is an aqueous solution containing stannous chloride and concentrated hydrochloric acid, and the second tin salt solution is an aqueous solution containing stannous chloride, sodium chloride, ascorbic acid and concentrated hydrochloric acid; s2, mixing and reacting the palladium salt solution and 1 / 3-1 / 2 of the first tin salt solution by adopting a microfluidic method, and dispersing the reaction solution into a second tin salt solution to obtain a mixed solution; and S3, mixing the residual first tin salt solution with the mixed solution by adopting a micro-fluidic method to obtain the colloidal palladium activation solution. By introducing the microfluidic technology, the mixing reaction is more accurately controlled, and the catalytic activity of the colloidal palladium activation solution is improved. By supplementing the tin salt solution, the insufficient stability caused by low tin salt content in the synthesis process is made up.

The invention belongs to the technical field of organic synthesis catalysts, and particularly relates to a preparation method and application of a composite catalyst for synthesizing 1, 2-pentanediol through furfuryl alcohol hydrogenation. The preparation method comprises the following steps: preparing cerium nitrate, lanthanum nitrate, urea, a surfactant and water into an aqueous solution, dipping spherical gamma-Al2O3, and then sequentially carrying out hydrothermal reaction, drying and roasting to obtain CeO2-La2O3 / Al2O3; the preparation method comprises the following steps: preparing palladium chloride, ruthenium chloride, hydrochloric acid and water into an acidic solution, dipping CeO2-La2O3 / Al2O3, drying, roasting and performing hydrogen reduction in sequence, thereby obtaining the composite catalyst Pd-Ru-CeO2-La2O3 / Al2O3. The composite catalyst can be applied to preparation of 1, 2-pentanediol through furfuryl alcohol hydrogenation. By preparing the composite catalyst, the defects of the existing catalyst in the aspects of selectivity, stability and cost are overcome.

The invention discloses a surface nickel plating process for quartz glass, and aims to improve the adhesive force, uniformity and functional performance of a nickel plating layer, simplify the process flow and meet the environmental protection requirement. The process comprises the following steps: firstly, cleaning and roughening the surface of quartz glass, removing surface impurities through a 2% sodium hydroxide solution and a 10% hydrofluoric acid solution, and forming a microscopic rough structure; then treating in a sensitizing solution composed of stannous chloride and hydrochloric acid to enable the surface to adsorb stannous ions; then treating in an activating solution composed of palladium chloride and hydrochloric acid to form a catalytic active layer; then carrying out nickel plating reaction in a chemical nickel plating solution with the temperature of 85 DEG C and the pH value of 4.5, wherein the thickness of a plating layer is 5-10 microns; and finally, the waste liquid is neutralized and flocculated to realize environment-friendly discharge. The process is simple and convenient to operate, and the generated nickel coating is uniform and compact, has excellent conductivity and corrosion resistance, and can be widely applied to the fields of electronics, optics and chemistry.

The invention discloses a silver-coated copper powder preparation method based on nickel layer enhanced palladium catalysis and active hydrogen synergistic deposition, and relates to the technical field of powder surface treatment. The method specifically comprises the following steps that copper powder is soaked in acid liquor, then filtering, washing and drying are conducted, and pretreated copper powder is obtained; immersing the pretreated copper powder into a hydrochloric acid solution of nickel chloride hexahydrate, and then filtering, washing and drying to obtain sensitized copper powder; immersing the sensitized copper powder into a hydrochloric acid solution of palladium chloride, and then filtering, washing and drying to obtain activated copper powder; mixing the activated copper powder with the reduction solution to obtain a solid-liquid mixture, adding a silver-ammonia solution into the solid-liquid mixture, heating for reaction, and filtering after the reaction is finished to obtain a solid product; and washing and drying the solid product to obtain the silver-coated copper powder based on nickel layer enhanced palladium catalysis and active hydrogen synergistic deposition. The silver-coated copper powder with a compact silver layer and high binding force is prepared through the ternary synergistic effect of nickel layer sensitization, palladium nanometer activation and formaldehyde reduction.

The invention relates to the technical field of organic synthesis, in particular to 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine as well as a synthesis method and application of the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine. The synthesis method comprises the following steps: (1) synthesizing 2-chloro-3-fluoro-4-iodine-5-methylpyridine from 2-chloro-3-fluoro-5-methylpyridine and an iodine elementary substance to obtain 2-chloro-3-fluoro-4-iodine-5-methylpyridine; (2) synthesizing 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine, the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride, the tripotassium phosphate and the (2-formyl phenyl) boric acid, and further synthesizing the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde from the 2-chloro-3-fluoro-4-iodo-5-methylpyridine and the 1, 1-bis (diphenylphosphine) ferrocene palladium dichloride. And (3) synthesizing the 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine by using the 2-(2-chloro-3-fluoro-5-methylpyridine-4-yl) benzaldehyde and sodium tert-butoxide. The 4-chloro-1-methyl-6H-heterochromene [3, 4-c] pyridine compound constructed by the invention can be used for detecting the content of pesticide residue glyphosate.

The invention belongs to the technical field of amber core synthesis, and particularly discloses an amber core synthesis catalyst, a preparation method thereof and a synthesis method of an amber core. Palladium chloride, zinc chloride and nickel chloride are prepared into a mixed solution according to the mass ratio of (15-20): (5-10): 1; glucose is added into the mixed solution, heating reaction is performed, the reaction temperature is 50-78 DEG C, and the reaction time is 10-48 h; and carbonizing the solid obtained by the reaction in an inert atmosphere to obtain the catalyst. The preparation method comprises the following steps: mixing 1-(2-tert-butylphenyl oxy)-2-butanol and the catalyst according to a mass ratio of (15-25): 1, introducing hydrogen into a reaction system, controlling the pressure of the hydrogen to be 1.5-2.5 MPa, and carrying out a heating reaction at the reaction temperature of 140-160 DEG C for 3-15 hours, thereby obtaining the 1-(2-tert-butylphenyl oxy)-2-butanol. When the catalyst is used for preparing the amber core, the yield is increased to 90% or above, the ratio of cis-products to trans-products reaches 75: 25, the reaction temperature is reduced to 150 DEG C, and the reaction is milder and safer.

The invention relates to the technical field of new energy chemical catalysis, in particular to a catalyst for preparing formaldehyde through photo-thermal catalysis of methane under gas-solid continuous flow as well as a preparation method and application of the catalyst. The preparation method comprises the following steps: S1, preparing a pretreatment carrier; s2, preparing a precursor solution: S201, adding a palladium chloride solution into the zinc oxide suspension, stirring at room temperature, carrying out vacuum suction filtration, washing and drying to obtain a Pd / ZnO precursor; s202, dispersing the Pd / ZnO precursor in deionized water, adding rare earth metal salt, dropwise adding triethylene tetramine, stirring, and adding sodium hypophosphite to obtain a precursor solution; s3, preparing a composite precursor; and S4, carrying out post-treatment. The invention provides a catalyst for preparing formaldehyde through photo-thermal catalysis of methane under gas-solid continuous flow as well as a preparation method and application of the catalyst, and aims at solving the problems that in related technologies, the activation difficulty of methane C-H bonds is high, formaldehyde is prone to deep oxidation, and the operation efficiency of the catalyst in a gas-solid continuous flow system is low.

A method for recovering platinum group precious metal in a silicon carbide DPF catalyst comprises the steps that S1, smelting treatment is conducted, specifically, the silicon carbide DPF catalyst is crushed and then mixed with a smelting agent in a layered mode, a smelting reaction is conducted at the high temperature, and the smelting agent is composed of sodium carbonate and sodium peroxide; s2, leaching and separation are conducted, specifically, after the smelting product obtained in the step S1 is cooled, acid leaching treatment is conducted through hydrochloric acid, leaching liquid containing platinum group precious metal and residues are obtained through filtering separation, the residues are washed, and washing liquid is added into main leaching liquid; and S3, precious metal enrichment is conducted, specifically, the leachate obtained in the step S2 is enriched through a chemical precipitation method, the obtained precipitate is dissolved with aqua regia, and a platinum-palladium chloride mixed solution is obtained. The method is high in recovery rate, and under the optimal condition, the recovery rate of platinum can reach 91% or above, and the recovery rate of palladium can reach 96% or above; the process is simple, the cost is controllable, the used smelting agent is a common chemical raw material, and the cost is low.

The invention relates to the technical field of preparation of noble metal catalysts, and discloses a preparation method of a palladium-carbon catalyst for dehalogenation coupling reaction, which specifically comprises the following steps: 1, preparing nitric acid modified activated carbon: heating and refluxing activated carbon with nitric acid at 80 DEG C for 1 hour, and washing the activated carbon to be neutral to obtain the nitric acid modified activated carbon; 2, slurry preparation: adding nitric acid modified activated carbon into a sodium carbonate solution, mixing to prepare slurry, and stirring at room temperature for 0.5 h; 3, stirring and mixing treatment: adding a chloropalladic acid solution into the slurry while stirring, and continuously stirring for 0.5 h after dropwise adding; according to the palladium-carbon catalyst for the dehalogenation coupling reaction, provided by the invention, the conversion rate is increased, and the defects that the selectivity is not high, the catalytic activity is not strong and the catalyst is inactive and difficult to use mechanically in the preparation of 3, 3 ', 4, 4'-biphenyl tetraformate in the dehalogenation coupling reaction are overcome.

The invention relates to a preparation method and application of an AuPd alloy nanoparticle doped ZnO sensing material, and belongs to the field of gas sensing. According to the invention, sodium hydroxide is used as a solution to provide an alkaline environment, zinc nitrate hexahydrate is used as a zinc source, chloroauric acid and palladium chloride are used as a gold source and a palladium source, deionized water is used as a solvent, and the AuPd-ZnO gas-sensitive sensing material is prepared through the steps of mechanical stirring, microwave-assisted hydrothermal method synthesis, centrifugation, drying and the like. The sensor based on the AuPd-doped ZnO nano material has good gas-sensitive performance on acetone, and has high response, ideal stability and good selectivity. The response to 50 ppm ethanol is 32, the lower limit of detection is 5 ppm, and high stability is shown in a continuous peripheral gas-sensitive test. The method is simple in preparation process, low in equipment requirement and high in controllable degree, and the obtained product is uniform, has excellent gas-sensitive performance, can realize trace detection of ethanol and can be used as an ideal sensing device for ethanol detection.

The invention relates to the field of chemical production, and discloses a preparation device and method of bis (triphenylphosphine) palladium dichloride, the preparation device comprises a base, the top of the base is fixedly connected with a preparation cylinder, the front end of the preparation cylinder is fixedly connected with a window, and the top of the preparation cylinder is fixedly connected with a motor; the device comprises a preparation cylinder, the top of the preparation cylinder is fixedly connected with an arc-shaped supporting plate, the inner wall of the preparation cylinder is rotatably connected with a stirring rod, the outer side of the arc-shaped supporting plate is fixedly connected with a quantifying mechanism, the quantifying mechanism comprises a quantifying cylinder, and the outer wall of the quantifying cylinder is fixedly connected with the outer wall of the arc-shaped supporting plate. And the inner wall of the quantifying cylinder is in sliding connection with a partition plate. By arranging the quantifying mechanism, the adding amount of chemical agents can be accurately controlled, and the inner wall space of the three groups of quantifying cylinders is adjusted according to the total manufacturing amount, so that the quantifying effect is achieved, the proportion of the chemical agents is accurately controlled, and the problem that the adding amount is difficult to accurately control in a traditional mode is solved.

According to the method, aryl anhydride and aryl bromide are used as main raw materials, N, N-dimethylacetamide is used as a solvent, 5mol% of bis (triphenylphosphine) palladium dichloride and 5mol% of ethylene glycol dimethyl ether nickel bromide are used as catalysts, 10mol% of 2-(dicyclohexylphosphine) 3, 3 '-dicyclohexylphosphine is used as a catalyst, and the asymmetric diaryl ketone compound is prepared through a one-step reaction. The method comprises the following steps: by taking 2, 6-dimethoxy-2 ', 4', 6 '-triisopropyl-1, 1'-biphenyl and 5mol% alpha, alpha, alpha-terpyridyl as ligands, one equivalent of sodium sulfate as an additive and two equivalent of zinc powder as a reducing agent, putting the materials into a reaction container in a nitrogen atmosphere, heating to 40 DEG C, and reacting for 12 hours to obtain the asymmetric diaryl ketone compound I with high yield. The method has the advantages of simplicity and convenience in operation, mild reaction conditions, high yield, few additives, high selectivity and the like, and has certain feasibility for realizing industrial production.

The utility model discloses a blocky palladium chloride crushing device, which relates to the technical field of crushing devices and comprises a crushing bin, a feeding hopper is mounted at the upper end of the crushing bin, a rotating hole is formed in one end of the feeding hopper, a groove roller is mounted at the middle end of the rotating hole, and a convex groove roller is mounted at one end of the rotating hole. A roller connecting motor is installed at one end of the convex groove roller, a collecting hopper is installed at the lower end of the material crushing bin, a bottom motor is installed at the lower end of the collecting hopper, a hammer connecting shaft is installed at the upper end of the bottom motor, and a material crushing hammer is installed at the upper end of the hammer connecting shaft. Through the arrangement of the material crushing bin, the feeding hopper, the groove roller, the convex groove roller, the hammer connecting shaft and the material crushing hammer, blocky palladium chloride is fed into the hopper, the convex groove roller is driven by the roller connecting motor to rotate, and the blocky palladium chloride is primarily extruded and crushed through a gap between the convex groove roller and the groove roller; and then the bottom motor drives the hammer connecting shaft and the material crushing hammer to rotate and grind in the material crushing bin, so that the crushing efficiency of the device is improved.

The invention discloses a method for preparing a fluorine-containing compound and its application, and relates to the technical field of perovskite material additives. The preparation method is as follows: naphthaleneboric acid, potassium carbonate and bis(triphenylphosphine)palladium chloride are added to a drying container, the container is evacuated to a vacuum state and then filled with nitrogen, phenylacetylene and nine fluoro-4-iodobutane are added to the container, dichloromethane and distilled water are then added to the container, and heated for reaction; the obtained reaction mixture is subjected to extraction and drying, separation and purification, and a fluorine-containing compound is obtained. The fluorine-containing compound prepared by the present invention has good compatibility with the perovskite material, and there will be no heterogeneous phase generation; it is applied as an additive in the perovskite material to suppress the migration and loss of ions, reduce the defect state density at the perovskite grain boundary, extend the carrier lifetime, and improve the charge transfer efficiency; it can also promote the nucleation and growth of perovskite, and improve the quality and morphology of the perovskite film.

The application discloses a preparation method of a phenylacetic acid compound, and particularly, the application uses a substituted or unsubstituted aromatic hydrocarbon as a starting material, and under the action of a palladium catalyst (such as palladium acetate, palladium on carbon, palladium chloride, tetra-triphenyl palladium, etc.), the starting material is reacted with formaldehyde, HCl (aq) and CO to efficiently generate the phenylacetic acid compound. The method disclosed by the application only needs to start from the aromatic hydrocarbon, greatly reduces the difficulty and cost of obtaining the raw material, and avoids stimulating, sensitizing or toxic raw materials. Compared with the prior art, the method disclosed by the application has the advantages of simplicity and efficiency, cheap and easy-to-obtain raw materials, high atomic economy, high yield, green and pollution-free, easy industrialization and the like.

The application discloses a sulfuric acid acidified palladium carbon catalyst and a preparation method and application thereof, and the preparation process of the catalyst comprises the following steps: sulfuric acid acidification of activated carbon, washing, preparation of a palladium chloride hydrochloride solution as a precursor, preparation of a suspension of the sulfuric acid acidified activated carbon in deionized water, dropwise addition of the palladium chloride hydrochloride solution into the suspension of the sulfuric acid acidified activated carbon, vigorous stirring, filtration, vacuum drying, and obtaining of the sulfuric acid acidified palladium carbon catalyst, and application of the catalyst to preparation of 2,5-dimethyltetrahydrofuran. The application self-prepares a high-efficiency sulfuric acid acidified palladium carbon catalyst to catalyze a reaction, the catalyst has good circulation stability, and has the advantages of simple reaction, low reaction temperature, easy separation of a product, high yield and the like.

The invention discloses a novel C2 symmetric chiral bisamide ligand and a preparation method and application thereof, the ligand has a structure as shown in # imgabs0 #, Ar is aryl, the relative positions of two sulfur in the general formula are different, * represents a chiral center, R is 4-methylbenzyl, 4-bromobenzyl, 2, 6-dimethylbenzyl, methyl or benzyl, and n represents 1 or 2. Dithiophenol and (2S, 3S)-2, 3-diphenylaziridine react to obtain an intermediate, and the intermediate and nitrogen-substituted chiral cyclic amino acid or 2-diphenylphosphinobenzoic acid are subjected to dehydration condensation to obtain various ligands with novel structures. A catalyst formed by complexing the ligand and an allyl palladium chloride dimer can be used as a chiral ligand for efficiently catalyzing an asymmetric allyl alkylation reaction.

The invention provides a preparation process of palladium chloride dihydrate, which comprises the following steps: S1, respectively adding palladium powder, high-purity water and a reducing agent into a reactor, stirring and heating, and carrying out constant-temperature reaction and standing for layering to obtain activated palladium powder; s2, hydrochloric acid is added into the activated palladium powder, then stirring and heating are conducted, hydrogen peroxide is dropwise added, a reaction is conducted till the palladium powder is completely dissolved, and a dissolved solution is filtered; s3, transferring the filtrate into an evaporator for dissolving, and then carrying out vacuum concentration; s4, repeating the step S3 for 3-5 times until the pH value of the solution reaches 1-5.5; and S5, carrying out vacuum concentration on the solution, and obtaining palladium chloride dihydrate when the palladium content reaches a set value. The direct recovery rate of the preparation process is high, the raw material loss can be effectively reduced, the production benefit is improved, the operation process is simple, and the prepared palladium chloride dihydrate has the nitrate-free characteristic, also has good water solubility and can meet the use requirements in different scenes.

The invention provides a Pd-foamed nickel hydrogen evolution catalyst and a preparation method and application thereof.The preparation method of the Pd-foamed nickel hydrogen evolution catalyst comprises the following steps that a mixed solution containing sodium chloride and palladium chloride is used for conducting electric etching-deposition treatment on foamed nickel, and the Pd-foamed nickel hydrogen evolution catalyst is obtained; wherein the electric etching-deposition treatment is carried out by using a cyclic voltammetry method. According to the preparation method of the Pd-foamed nickel hydrogen evolution catalyst, the catalyst with low overpotential and high stability can be prepared, and the method has the advantages of being short in step, easy to operate, high in practical operability and the like.

The present application relates to the technical field of catalytic materials, and discloses a halloysite nanotube loaded palladium-platinum bimetallic alloy catalyst and a preparation method thereof, the catalyst comprising heat pretreated halloysite and uniformly dispersed palladium-platinum bimetallic alloy particles, and the mass ratio of palladium, platinum and heat pretreated halloysite being 0.012-0.022:0.012-0.022:1. The preparation method comprises mixing the heat pretreated halloysite with palladium chloride and chloroplatinic acid hexahydrate, adding concentrated ammonia water to adjust the pH to 9-11 to form an ammonia complex; obtaining a precursor through a hydrothermal reaction, and adding sodium borohydride for liquid phase reduction. The bimetallic alloy phase produces geometric and electronic synergistic effects, thereby reducing the reaction activation energy; the ammonia complex ion is chemically bonded with the hydroxyl group of the carrier to prevent the loss of active components in the hydrothermal environment. The catalyst is combined with glycerol to produce hydrogen in situ, thereby avoiding the safety hazards and equipment investment of external high-pressure hydrogenation, and realizing the high-yield conversion of green diesel under extremely low noble metal loading.

The invention relates to the technical field of waste liquid treatment, in particular to a cyclic utilization method and application of palladium in a circuit board ion palladium waste liquid. Comprising the following steps: S1, separating metal impurities from the palladium waste liquid to obtain feed liquid I; s2, carrying out palladium ion concentration on the feed liquid I to obtain feed liquid II; s3, reducing the feed liquid II to generate a palladium monomer, and collecting palladium powder; and S4, taking palladium powder to react with an oxidizing agent in an acidic medium to obtain a salt solution containing palladium ions. According to the method, an ion exchange resin adsorption separation method and a liquid membrane extraction method are combined, on one hand, the content of metal impurities in the palladium recovery process is reduced, and the recovery purity of the metal palladium is guaranteed; on the other hand, the recovery rate of metal palladium is effectively increased; the purity of the palladium chloride prepared by the method is up to 98% or above, the quality of the synthesized colloidal palladium activating solution is stable, a closed-loop recovery and utilization process mode can be realized, and the application prospect is wide.

The invention discloses an alpha-fluoro alpha, beta-unsaturated amide derivative as well as a synthesis method and application thereof. The preparation method comprises the following steps: by taking amyl-1, 1, 2-trifluoro-1, 4-diene which is simple and convenient to prepare and a cheap and abundant amine compound as raw materials, an allyl palladium chloride dimer as a transition metal catalyst, 1, 4-bis (diphenylphosphine) butane as a ligand and 2, 5-di-tert-butylbenzoquinone as an oxidant, reacting in an organic solvent at a proper temperature under a nitrogen condition, thereby obtaining the 1, 1, 2-trifluoro-1, 4-diene compound. The alpha-fluoro alpha, beta-unsaturated amide derivative is obtained with good yield, and the structural formula of the derivative is shown in the specification. The synthesis method disclosed by the invention has the characteristics of simplicity and convenience in operation, mild conditions, greenness, economy, wide substrate compatibility, high chemical selectivity and high regioselectivity, and solves the technical problem that the synthesis conditions of the alpha-fluoro-alpha, beta-unsaturated amide derivative are complicated and harsh. Meanwhile, the alpha-fluoro drug molecules can be efficiently and highly selectively obtained, and the method has a wide application prospect.

The invention discloses a catalytic synthesis method of methyl nitrite, belongs to the technical field of methyl nitrite synthesis, and is used for solving the technical problem that the selectivity of catalytic synthesis of methyl nitrite in the prior art needs to be further improved. The catalytic synthesis method specifically comprises the following steps: adding lanthanum nitrate, copper nitrate, palladium chloride and deionized water into a beaker; the preparation method comprises the following steps: adding amino graphene and aluminum silica gel into a reaction kettle, stirring at room temperature for 10-20 minutes, adding ethylene glycol, continuously stirring for 15-30 minutes, adding a composite carrier into a system, adjusting the pH value to 3-4 by using saturated dilute nitric acid, heating to 50 DEG C, reacting for 12-15 hours, and performing post-treatment to obtain the modified catalyst. The reaction conversion rate, selectivity and catalyst stability are improved.

The invention discloses a preparation method and application of a composite electrode for removing chlorinated PPCPs in water through electro-catalytic hydrodechlorination, and the preparation method of an electrochemical cathode comprises the following steps: placing foamed nickel in a mixed solution of nickel nitrate hexahydrate and manganese sulfate for electro-deposition, and after the reaction is finished, drying the foamed nickel to obtain a NiMn-LDH / NF electrode, and placing the NiMn-LDH / NF electrode and anhydrous sodium hypophosphite in a tubular furnace, carrying out calcination phosphorization in a nitrogen atmosphere, placing the electrode in a mixed solution of palladium chloride and sodium chloride, and carrying out electro-deposition palladium loading to finally obtain the Pd / NiMn-LDH-Ov / NF composite electrode. The Pd / NiMn-LDH-Ov / NF composite electrode prepared by the method has good electro-catalytic performance, the removal rate of losartan potassium can reach 96.45%, meanwhile, the Pd / NiMn-LDH-Ov / NF composite electrode has excellent recycling performance, and secondary pollution is avoided.

The present invention discloses a preparation method and application of a Pd v FeCoNiZn v LDH high-entropy catalytic material. Palladium chloride is dispersed in absolute ethanol to obtain solution A; ferric chloride hexahydrate, cobalt nitrate hexahydrate, nickel nitrate hexahydrate, zinc nitrate hexahydrate, ammonium fluoride and urea are added to deionized water, and then mixed with solution A to obtain solution B; nickel foam is placed in solution B for hydrothermal reaction to obtain nickel foam loaded with PdFeCoNiZn LDH; then it is placed in an alkaline solution and heated to react to obtain a flower-shaped Pd v FeCoNiZn v LDH high-entropy catalytic material assembled by nanosheets with abundant zinc and palladium bimetallic vacancies. The high-entropy catalytic material prepared by the present invention exhibits a fast mass transfer rate and reaction kinetics in electrocatalytic HER, and thus shows excellent electrocatalytic activity and stability, and can be used as an electrocatalytic water splitting hydrogen evolution catalyst.

The present invention discloses a vinyl acetate catalyst, its preparation method, and application. The method comprises the following steps: crushing a carbonized raw material, adding an acidic solution, soaking for a period of time, washing and drying, then adding an alkaline solution and stirring, isolating the mixture from air to obtain a base carbon material; mixing the base carbon material with a Y-type molecular sieve, then calcining the mixture in stages, and then introducing an appropriate amount of a mixed gas of water vapor, carbon dioxide, and nitrogen to obtain a composite catalyst carrier; mixing the composite catalyst carrier with sodium hydroxypropanesulfonic acid methacrylate, adding deionized water, and stirring to obtain a carrier suspension; simultaneously adding a palladium chloride solution and a tungsten chloride solution dropwise to the carrier suspension, stirring, centrifuging, drying, grinding, and calcining to obtain a modified catalyst carrier; and mixing the modified catalyst carrier with zinc acetate and an additive, stirring, insulating, filtering, and drying to obtain a vinyl acetate catalyst. The vinyl acetate catalyst provided by the present invention has a good conversion rate.

The invention discloses a concentrated crystallization device for preparing palladium chloride, comprising a frame, a machine head, a flask, a water bath heating structure, a transfer tube, a feed tube, a condenser, and a collecting bottle, and also comprising: a split connection structure, wherein the flask comprises a straight segment connected to the machine head, a side of the straight segment away from the machine head is connected with a flask segment, the split connection structure comprises a sealing cylinder nested on the outside of the straight portion of the flask segment, a sealing net is arranged at the opening of the flask segment, the straight segment and the flask segment are wrapped with a closed rubber sleeve on the outside, and a pressure dividing component is arranged on the outer movable sleeve of the closed rubber sleeve; a cantilevered accommodating structure, comprising a mounting cylinder arranged on the inner side of the sealing net, the end of the mounting cylinder is connected to a storage rack, the storage rack is cantilevered in a circular cavity of the flask segment, and the interior of the storage rack is filled with anti-boiling particles. The invention can allow the interior of the flask to be provided with the anti-boiling particles without affecting the normal formation of a liquid film, and can also better ensure the stability of the flask.