715 results about "Hydroxylamine" patented technology

The invention provides a low-cost flow battery and an application thereof, a redox active substance of a positive electrode electrolyte of the low-cost flow battery contains a hydroxylamine cyclic structure group with hindered amine, and the hydroxylamine cyclic structure group with hindered amine is preferably selected from 1-hydroxy-2, 2, 6, 7, 8-tetramethyl-1, 3, 5-tetramethyl-1, 3, 5-tetramethyl-1, 3, 5-tetramethyl-1, 3, 5-tetramethyl-1, 3, 5-tetramethyl-1, 3, 5-tetramethyl-1, 3, 5-tetramethyl-1, one or more of a 1-oxo-2, 2, 6, 6-tetrasubstituted piperidine group, a 1-oxo-2, 2, 6, 6-tetrasubstituted piperidine group, a 1-oxo-2, 2, 6, 6-tetrasubstituted piperidine group, and a 1-oxo-2, 2, 6, 6-tetrasubstituted piperidinium group; a redox active substance of the negative electrode electrolyte contains one or more of a titanium element, a vanadium element, a chromium element, an iron element and a zinc element. The low-cost flow battery has the advantages of high output voltage, high energy density, environment friendliness and low cost, and has good application prospects and large-scale popularization potential in the field of energy storage.

The invention belongs to the technical field of preparation of blocking removers, and particularly relates to a composite chelating blocking remover for an oil field and a preparation method of the composite chelating blocking remover. The composite chelating blocking remover for the oil field is prepared from the following raw materials in percentage by mass: 7 to 9 percent of 1-butyl-3-methylimidazole dodecyl sulfonate, 5 to 7 percent of erucamide propyl hydroxypropyl sulfobetaine, 3 to 4 percent of di-(2-ethylhexyl) sodium sulfosuccinate, 4 to 5 percent of ethylenediamine di-o-hydroxyphenylacetic acid, 5 to 7 percent of N, N '-di (2-hydroxybenzyl) ethylenediamine-N, N'-bis (2-hydroxybenzyl)-N, N '-bis (2-ethylhexyl)-N, N'-bis (2-hydroxybenzyl)-N, N '-bis (2-hydroxybenzyl)-N, N'-bis (2-hydroxyphenyl)-N, N '-bis (2-hydroxyphenyl)-N, N'-bis (2-hydroxyphenyl)-N The cleaning agent is prepared from the following components in percentage by weight: 3 to 4 percent of N, N '-diacetic acid, 2 to 3 percent of O-(3-(benzyloxy) propyl) hydroxylamine, 1 to 2 percent of heptadecenyl hydroxyethyl imidazoline quaternary ammonium salt, 1 to 1.5 percent of dimethyl diallyl ammonium chloride homopolymer and the balance of water. The composite chelating blocking remover for the oil field has excellent scale dissolution rate and paraffin inhibition rate when being applied to complex scale blocking removal of the oil field.

The invention relates to the field of caprolactam production, and discloses a green and efficient production process and device. The process comprises the following steps: continuously oximating cyclohexanone and hydroxylamine in a microreactor under the catalysis of mesoporous silica solid acid; carrying out gas phase rearrangement on cyclohexanone-oxime in the presence of a ZSM-5 molecular sieve under the assistance of microwaves; coupling, rectifying and purifying the crude product through a four-stage molecular sieve membrane; and performing catalytic cracking on the by-product to obtain N2 / H2O and recycling. The device comprises a micro-reaction unit, a microwave-radial reactor, a membrane coupling rectifying tower group and a tail gas cracking unit. Zero emission of ammonium sulfate is achieved, the product purity is larger than or equal to 99.95%, and energy consumption is reduced by 45%.

The invention discloses a preparation method of an ultra-pure hydroxylamine aqueous solution, and relates to the field of organic chemistry and chemical industry production. The method comprises the following steps: reacting electronic-grade hydroxylamine salt with organic alkali in a proper solvent to generate hydroxylamine, then separating and removing salt and unreacted hydroxylamine in a reaction solution through a mercaptopyridine ion exchange modified membrane, and finally concentrating the solution into 50wt% ultra-high-purity hydroxylamine aqueous solution by adopting reduced pressure evaporation or multi-effect evaporation. The process has the characteristics of high efficiency, environmental protection, simplicity and easiness in operation, effectively improves the purity, yield and separation efficiency of hydroxylamine, and meets the strict requirements of electronic grade hydroxylamine on purity and metal ion content.

The invention provides a photoacid generator, a preparation method thereof and a photoresist based on the photoacid generator. The photoacid generator is 4-alkyl-N-hydroxyl naphthalimide fluoroalkyl sulfonate, and the molecular structural formula of the photoacid generator is # imgabs 0 #, and in the formula, R is alkyl. The preparation method of the photoacid generator comprises the following steps: S1, dissolving 5-alkyl acenaphthene in a first solvent, heating, adding potassium permanganate in the heating process, then heating to reflux for reaction, and after the reaction is finished, purifying to obtain 4-alkyl-1, 8-naphthalic anhydride; s2, dissolving the 4-alkyl-1, 8-naphthalic anhydride, hydroxylamine hydrochloride and a first inorganic base in a second solvent for reaction, and after the reaction is finished, purifying to obtain 4-alkyl-N-hydroxy-1, 8-naphthalic imide; and S3, adding the 4-alkyl-N-hydroxy-1, 8-naphthalimide and an organic alkali into a third solvent, dropwise adding fluoroalkyl sulfonic anhydride, heating to react after dropwise adding is completed, and purifying after the reaction is completed to obtain the 4-alkyl-N-hydroxy-1, 8-naphthalimide. The photoresist based on the photoacid generator provided by the invention is large in ADR, and the negative photoresist development defect and the standing wave are improved.

The present application relates to the technical field of fine chemical synthesis, and in particular to an efficient preparation process of octanoyl hydroxamic acid, which comprises the following preparation steps: S1, preparation of ethyl n-octanoate: 90-110 parts by weight of n-octanoic acid and 35-40 parts by weight of ethanol are mixed, and then a solid acid catalyst is added, and the mixture is heated to reflux for reaction for 2.5-3 hours, filtered to obtain a precipitate and a filtrate, and the filtrate is decompressed and distilled to obtain ethyl n-octanoate; S2, preparation of octanoyl hydroxamic acid: 0.4-0.6 parts by weight of sodium acetate and 0.2-0.4 parts by weight of sodium carbonate are added to water, stirred until dissolved, ethanol is added, and after stirring, 24-32 parts by weight of hydroxylamine and ethyl n-octanoate prepared in S1 are added to react to obtain octanoyl hydroxamic acid; the process has the advantage of improving the reusability of the solid acid catalyst.

The invention discloses a preparation method of a high-purity ultra-clean hydroxylamine aqueous solution. A four-stage purification process comprises the following steps: 1) low-temperature chelation-ceramic membrane metal removal; 2) molecular sieve membrane rectification decomposition prevention; 3) pulse electrodialysis reversal deep desalination; and 4) gradient filtration terminal refining. According to the preparation method of the high-purity ultra-clean hydroxylamine aqueous solution, a low-temperature molecular sieve membrane rectification technology is adopted, hydroxylamine liquid-phase thermal decomposition is avoided through a vapor phase separation mechanism, and the decomposition rate is reduced to 1t from 15% of a traditional process; the method comprises the following steps of: removing metal through chelation-electrodialysis synergistically, ensuring that Fe and Cu ion residues are less than or equal to 0.05 ppb through a thiosemicarbazide-bipolar membrane system, ensuring the nitrogen environment in the whole process, ensuring that the dissolved oxygen is less than or equal to 5ppb, replacing liquid phase distillation with molecular sieve membrane vapor phase separation, solving hydroxylamine liquid phase thermal decomposition, and breaking through the trace metal removal limit by combining thiosemicarbazide-bipolar membrane synergistically removing impurities. And then through nanoscale terminal filtration, the metal / particle control reaches ppb-level limit which is superior to the SEMI standard, and double spanning of quality and cost is realized.

The invention relates to the field of phosphorus-nitrogen flame retardants, and discloses a preparation method and application of a novel phosphorus-containing nitrogen oxide flame retardant, the preparation method comprises the following steps: S1, under the protection of nitrogen, dissolving diphenylphosphinyl hydroxylamine and triethylamine in a tetrahydrofuran solvent to prepare a reaction substrate solution; s2, slowly dropwise adding a diphenylphosphinyl chloride solution into the solution, and then sufficiently carrying out the reaction in a staged heating and heating reflux mode; s3, cooling and filtering to remove solid byproducts generated by reaction, and concentrating filtrate to obtain a crude product solid; and S4, recrystallizing and purifying the crude product by using ethyl acetate, and finally heating and drying the obtained crystal under a vacuum condition to obtain the product. An N-O group is innovatively introduced into the molecular structure of the flame retardant, so that the effect of efficiently capturing gas-phase free radicals in cooperation with a phosphorus-containing group is achieved, and the substantive technical progress that the material can be endowed with excellent flame retardant property with extremely low addition amount is realized.

The invention belongs to the field of concrete admixtures and relates to a concrete foaming agent as well as a preparation method and application thereof. The concrete foaming agent contains a foaming component, a reinforcing agent, a conditioning agent, water and an optional foam stabilizer, wherein the foaming component is organic amine modified sulfonated alkyl glycoside; the organic amine modified sulfonated alkyl glycoside is prepared according to the following method: carrying out hydroxyamination reaction on polyether alkyl glycoside and organic amine, carrying out sulfonation reaction on the obtained hydroxyamination reaction product, and filtering, washing and drying the obtained crude product to obtain the organic amine modified sulfonated alkyl glycoside. The key point of the invention is that the organic amine modified sulfonated alkyl glycoside is introduced into the concrete foaming agent as a foaming component, and the organic amine modified sulfonated alkyl glycoside can enhance the temperature resistance of the concrete foaming agent and endow the concrete foaming agent with good weather resistance, so that the concrete foaming agent still has good foaming and foam stabilizing properties under a relatively high temperature condition.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of metaraminol bitartrate. The preparation method comprises the following steps: reacting benzyloxycarbonyl-L-alanine serving as a raw material with dimethylhydroxylamine hydrochloride, then reacting with 3-benzyloxybromobenzene, then carrying out one-step hydrogenation reaction to obtain m-hydroxylamine, and finally salifying to obtain the metaraminol bitartrate. The method adopts a one-step hydrogenation method to simultaneously realize dual effects of reduction and deprotection, reduces operation steps and material consumption, saves material cost, and reduces generation of reaction wastes; in the preparation process, reaction conditions are mild, safety and reliability are achieved, operation is easy, and the obtained target product is high in yield, good in selectivity and suitable for large-scale production.

The present invention belongs to the technical field of chemical separation and purification, and specifically relates to a method for removing impurities from a hydroxylamine aqueous solution. The method for removing impurities from a hydroxylamine aqueous solution provided by the present invention comprises the following steps: mixing a hydroxylamine aqueous solution and an alkaline compound for sedimentation and then performing solid-liquid separation to obtain a liquid phase; the alkaline compound comprises barium hydroxide or calcium hydroxide; the liquid phase is passed through an ion exchange column for ion exchange to obtain a purified hydroxylamine aqueous solution; the resin in the ion exchange column is a resin containing phenolic hydroxyl groups. The phenolic hydroxyl-containing resin used in the present invention is easy to obtain, has a wide range of sources, and has low cost. The present invention first uses an alkaline solution to remove sulfate or phosphate in a hydroxylamine aqueous solution, and then uses a phenolic hydroxyl-containing resin to efficiently, quickly, and conveniently remove metal ions in the hydroxylamine aqueous solution without reacting with hydroxylamine. The impurity removal method provided by the present invention has the advantages of simple operation and obvious purification effect, and has good industrial prospects.

The application discloses a method for preparing a CGRP receptor antagonistic intermediate, and belongs to the field of synthesis of medical intermediates. Compound 1 is used as a raw material, reacts with hydroxylamine hydrochloride in an organic solvent to generate an intermediate 2, and then reacts in the presence of a reducing agent to obtain a remikiren intermediate 3. The application is characterized in that a large steric hindrance silicon group is used as the R substituent in the compound 1, so that high stereoselectivity is ensured in the reduction reaction. The key intermediate obtained by using the method has high chiral purity, and the operation is simple, so that the industrial production of the product in the later stage can be realized.

The present invention relates to a process for the preparation of substituted 4-(N′-hydroxy-carbamimidoyl)benzoic acids, which can be obtained by nitrilase catalyzed hydration of substituted terephthalonitriles of formula (II) in an aqueous medium to afford (ammonium) 4-cyanobenzoic acids (IIa). The hydration is followed by treatment of the aqueous reaction medium with hydroxylamine or a salt thereof to afford amidoximes (I).

The invention discloses a two-phase absorbent for capturing CO2, which is characterized by being prepared from the following components in percentage by mass: 25%-30% of N-(2-ethoxyl) ethylenediamine, 0%-3% of N-aminoethyl piperazine, 0%-3% of 2-(1-ethoxyl) pyridine, 10%-13% of N, N '-diethyl ethylenediamine, 15%-20% of N, N'-diethylethylenediamine, 5%-10% of N, N '-diethylethylenediamine, 5%-10% of N, N'-diethylethylenediamine and the balance of water. The invention relates to a cleaning agent which is prepared from the following components in percentage by weight: 1 to 5 percent of N, N-diethylhydroxylamine, 1 to 5 percent of pentamethyldiethylenetriamine, 0 to 2 percent of tert-butylamine ethoxyethanol, 0 to 3 percent of 2-amino-2-methyl-propyl alcohol, 5 to 8 percent of sulfolane, 5 to 8 percent of dimethyl ether, 5 to 8 percent of p-xylene and 5 to 8 percent of n-butyl alcohol. The composition can be prepared by uniformly stirring the components. The preparation method is simple, and the prepared two-phase absorbent can improve the saturated absorption capacity, improve the desorption rate and optimize the performance of the phase change absorbent.

The invention relates to the technical field of catalysis, in particular to a Ru / WO3-x heterojunction catalyst, the chemical formula of the catalyst is Ru / WO3-x, and x represents oxygen vacancy; ru is loaded on the surface of a WO3-x support in the form of a metal simple substance, and the preparation method comprises the following steps: by taking tungstate as a tungsten source, ammonium sulfate as a morphology adjuvant and ruthenium trichloride as a ruthenium source, adjusting the pH value to 0-2, adding deionized water to prepare a hydrothermal reaction solution, performing hydrothermal reaction with a current collector, washing with deionized water, and drying, thereby obtaining the WO3-x support. And calcining in a reducing gas atmosphere to obtain the Ru / WO3-x heterojunction catalyst integrated electrode. Under the same test condition, nitrate can be effectively inhibited from being excessively hydrogenated into the final product ammonia, so that the product stays in the intermediate hydroxylamine.

The invention relates to the field of drug-resistant bacterium infection, and discloses a g-C3N4 / Bi2Se3 nano heterojunction and a preparation method thereof.The preparation method comprises the steps that firstly, melamine powder is heated and calcined at the constant temperature, after a tubular furnace is naturally cooled, spark plasma sintering is conducted, nitrogen vacancies are introduced at the same time, and a blocky high-defect g-C3N4 material is obtained; grinding into powder, adding deionized water for ultrasonic treatment to obtain a first suspension, performing centrifugal treatment, freeze-drying the supernatant, and adding into an ethylene glycol solvent to obtain a second suspension; eG, polyvinylpyrrolidone, Bi (NO3) 3.5 H2O and Na2SeO3 are mixed and stirred, and the second turbid liquid is added; the preparation method comprises the following steps: adding Bi2Se3 into a reaction kettle, heating while stirring, adding a hydroxylamine EG solution, cooling to room temperature after reaction, centrifuging, washing, and carrying out vacuum drying on a precipitate to obtain a g-C3N4 / Bi2Se3 nano heterojunction; the problems that in the prior art, the catalytic efficiency is low, a collaborative mechanism does not achieve structure-function integrated design, the performance of a key functional material is limited, and the structural stability and biological suitability of the material are insufficient are solved.

The invention relates to a corrosion-resistant polypropylene modified plastic and a preparation method thereof, and belongs to the technical field of polypropylene plastic modification. The modified plastic is prepared from isotactic polypropylene, exfoliated montmorillonite, polyvinylidene fluoride powder, anhydride grafted polypropylene, a beta-crystal nucleating agent, diethyl aluminum chloride, peroxide, hindered phenol, phosphite ester and N, N-distearoyl hydroxylamine. The preparation method comprises the steps of low-shear melting and blending, high-shear supercritical COviscosity reduction, vacuum exhaust, bidirectional orientation, infrared local crosslinking, co-extrusion cooling and the like. The obtained material is excellent in tensile strength, elongation at break, low-temperature impact strength, strong acid corrosion resistance and the like.

The application provides a low-cost flow battery and application thereof, and the low-cost flow battery contains a hydroxylamine cyclic structure group with a hindered amine in a redox active material of a positive electrolyte of the low-cost flow battery, the hydroxylamine cyclic structure group with the hindered amine is preferably one or more of a 1-hydroxyl-2,2,6,6-tetrasubstituted piperidine group, a 1-oxygen radical-2,2,6,6-tetrasubstituted piperidine group and a 1-oxo-2,2,6,6-tetrasubstituted piperidinium group; and the redox active material of a negative electrolyte of the low-cost flow battery contains one or more of titanium elements, vanadium elements, chromium elements, iron elements and zinc elements. The low-cost flow battery has the advantages of high output voltage, high energy density, environmental friendliness and low cost, and has good application prospect and large-scale promotion potential in the field of energy storage.

The invention discloses a copper-based catalyst for preparing propyl alcohol by electrocatalytic reduction of carbon dioxide and application of the copper-based catalyst. The preparation method of the copper-based catalyst comprises the following steps: adding a sodium hydroxide solution into an aqueous solution of a copper compound to obtain a turbid solution; adding a hydroxylamine hydrochloride aqueous solution into the turbid solution, carrying out a reaction, and carrying out centrifugal drying to obtain Cu (OH) 2 / CuO; cu (OH) 2 / CuO is prepared into a working electrode, and then the working electrode is reduced into the Cu / Cu2O nanosheet through an electrochemical reconstruction method. The Cu / Cu2O electrocatalyst with the bicontinuous nano-domain structure is obtained by using a two-step electrochemical reconstruction method, and the Cu / Cu2O electrocatalyst is used as a cathode for electrocatalytic reduction of carbon dioxide. The hydrogen evolution reaction is inhibited in a KOH or KHCO3 aqueous solution system, so that the activity of propyl alcohol preparation is remarkably improved. Experiments show that the Faraday efficiency of propyl alcohol exceeds 12.1% under the current density of 0.84 A cm <-2 >, and the Faraday efficiency of propyl alcohol is good. According to the analysis, the Cu / Cu2O catalyst obtained through the electrochemical reconstruction method serves as the cathode, and the propyl alcohol can be prepared through the carbon dioxide electrocatalytic reduction reaction.

The invention discloses a preparation method of 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole, which comprises the following steps: taking a hydroxylamine oxygen sulfonic acid aqueous solution and isopentenal as raw materials, carrying out oximation reaction in an organic solvent under an alkaline condition, then directly adding an acid or an organic base catalyst into the reaction system, and reacting for 2-4 hours to obtain 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole, thereby obtaining the 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole. Under the catalytic action of the catalyst, a cyclization reaction is carried out, after the reaction is finished, an intermediate solution containing 5, 5-dimethyl-4, 5-dihydroisoxazole is obtained, and the next step is directly carried out; and carrying out a chlorination reaction by taking the intermediate solution as a raw material and sodium hypochloride or chlorine as a chlorination reagent, and after the reaction is finished, carrying out post-treatment to obtain the 3-chloro-5, 5-dimethyl-4, 5-dihydroisoxazole. The hydroxylamine oxygen sulfonic acid is used for enabling the isopentenal to be subjected to oximation reaction under the alkaline condition, then cyclization is carried out under the catalytic action of acid or alkali, the 5, 5-dimethyl-4, 5-dihydroisoxazole is generated, and the process has the advantages that the yield is high, the production steps are simplified, and the production cost is reduced.

The utility model provides a rectifying tower device for preparing isopropyl hydroxylamine, which comprises an upper tower shell and a lower tower shell, the upper tower shell is arranged on the upper side of the lower tower shell, a connecting pipe is arranged between the upper tower shell and the lower tower shell, the outer end of the connecting pipe is integrally connected with a connecting ring, and the connecting ring is arranged between the upper tower shell and the lower tower shell. A first filler plate is fixedly connected in the connecting pipe, a second filler plate is arranged in the lower tower shell, a third filler plate is arranged in the upper tower shell, the second filler plate and the third filler plate are respectively arranged on the lower side and the upper side of the connecting pipe, and the second filler plate can move up and down along the lower tower shell; and the third filler plate can move up and down along the upper tower shell. By means of a combined assembly mode, the purpose of convenient disassembly and assembly is achieved, the packing can be disassembled and assembled conveniently, meanwhile, maintenance is convenient, and the distance and the height between the packing plates can be adjusted conveniently.

The invention relates to a treatment method of hydroxylamine-containing waste liquid. The treatment method comprises the following steps: (1) mixing a transition metal catalyst with hydroxylamine-containing waste liquid to obtain mixed liquid, and carrying out self-decomposition reaction; (2) maintaining the pH value of the mixed solution at 9.0-10.5 in the self-decomposition reaction process; and (3) after the self-decomposition reaction is finished, carrying out solid-liquid separation to obtain the hydroxylamine-removed waste liquid. The chemical environment during hydroxylamine decomposition reaction is alkaline, the condition is easy to realize, and the use amount of acid is greatly reduced. Meanwhile, the amount of added simple substances and compounds containing metal elements is small, and the amount of generated corresponding metal-containing reaction waste is small. And finally, the heat required by the reaction can be completely provided by the heat released by the decomposition of the hydroxylamine, and the self-decomposition of the hydroxylamine can be realized without additional energy.

The invention relates to the technical field of polyurethane, in particular to bio-based waterborne polyurethane and a preparation method thereof. The preparation method comprises the following steps: firstly, preparing dialdehyde cellulose by utilizing cellulose oxidation, then reacting the dialdehyde cellulose with hydroxylamine hydrochloride to prepare oximido modified cellulose, and finally introducing the oximido modified cellulose and dimethylglyoxime into a polyurethane system. Through the synergistic effect of the oximido modified cellulose and dimethylglyoxime, the bio-based waterborne polyurethane film has excellent self-repairing efficiency while keeping high tensile strength and elongation at break. The bio-based waterborne polyurethane is suitable for the fields of flexible electronic devices, coatings, biomedical materials and the like, and has wide application prospects and remarkable economic and social benefits.

The invention relates to a method for efficiently preparing hydroxylamine hydrochloride. The method comprises the following steps: mixing a diacetylmonoxime solution and a hydrochloric acid solution, pretreating through a pressurized nano-bubble fluidized bed, and carrying out reaction distillation under heating and pressurizing; after the reaction is finished, cooling reaction liquid, performing primary filtration and suction filtration through cross-flow filtration equipment, and collecting hydroxylamine hydrochloride crystals; and washing the crystal with absolute ethyl alcohol, recovering ethyl alcohol through cross-flow filtration equipment, and finally freeze-drying to obtain the high-purity hydroxylamine hydrochloride. The preparation method comprises the following steps: stirring quinoline-8-yl acrylate, tributyltin acrylate, 4-vinyl benzocyclobutene, ethanol and benzoyl peroxide to obtain a mixed solution; immersing the PTFE membrane subjected to low-temperature plasma pretreatment into the mixed solution, and then carrying out ultrasonic cleaning and vacuum drying to obtain a polymer modified PTFE membrane; the hydroxylamine hydrochloride prepared by the method disclosed by the invention has relatively high purity and yield, and meanwhile, the content of heavy metal ions and the content of water are effectively reduced.

The invention relates to the technical field of precious metal recovery, in particular to a method and system for recovering gold, silver, palladium and platinum from silver anode slime. S2, palladium precipitation: adding a potassium-magnesium mixture and sodium chlorate into the pre-impregnation liquid obtained in S1 to obtain palladium precipitation residues and platinum precipitation liquid; s3, separating gold; s4, platinum and palladium precipitation: adding a potassium-magnesium mixture and sodium chlorate into the gold separation liquid obtained in S3 to obtain platinum and palladium precipitation residues and platinum and palladium precipitation post-liquid; s5, gold is reduced; s6, platinum and palladium separation, wherein hydroxylamine hydrochloride is added into the platinum and palladium precipitation residues obtained in the step S4, and palladium separation liquid and platinum precipitation residues are obtained; 7, platinum purification, wherein hydroxylamine hydrochloride is added into the platinum precipitation residues obtained in the step 6, and platinum separation liquid is obtained; s8, carrying out primary palladium deposition; s9, carrying out secondary palladium deposition; and S10, palladium is reduced. The recovery rate of palladium is 99% or above, the recovery rate of platinum is 99% or above, the purity of platinum is 99.9%, the purity of palladium is 99.95%, the recovery rate of silver is 98.5% or above, and the recovery rate of gold is 99% or above.

The present invention relates to the preparation of cyantraniliprole, comprising the preparation of 8-methyl-2,4-dioxo-1,4-dihydro-2H-benzo[d][1,3]oxazine-6-carbonitrile key intermediate via 2-amino-5-((hydroxyimino)methyl)-3-methylbenzoic acid. Wherein hydroxylamine attacks a benzylic formyl group, to obtain the 2-amino-5-((hydroxyimino)methyl)-3-methylbenzoic acid, that undergoes simultaneously or by consecutive steps dehydrogenation and cyclization to obtain the benzo[d][1,3]oxazine group and the cyano group of the desired product. In addition, an improved method for the synthesis of the benzylic formyl group is also displayed.

The invention relates to a method for jointly determining plutonium 238, 239 + 240 and neptun-237 in aerosol by taking Pu-236 as a yield tracer agent, which comprises the following steps: step 1, sample pretreatment: cutting an aerosol sample into pieces, adding 236Pu, ashing, and leaching with a nitric acid solution A; step 2, valence state adjustment: adjusting the acidity of the leaching solution, and sequentially adding a hydroxylamine hydrochloride solution, a ferrous sulfamate solution and a sodium nitrite solution to adjust the valence state of nuclide; step 3, separation and purification: separating and purifying by adopting a TEVA resin column, leaching by using a nitric acid solution B and a hydrochloric acid solution, and desorbing by using an HCl-HF solution; and 4, the desorption solution is subjected to electro-deposition to prepare a source, and a low background alpha spectrometer is adopted for measurement of plutonium 238, 239 + 240 and neptun-237. The detection method is high in sensitivity, the recovery rate of the neptun-237 is high, and the blank of joint analysis of plutonium 238, 239 + 240 and neptun-237 is filled.

The invention provides a preparation method of a nano-gold star material, which comprises the following steps: stirring and heating a chloroauric acid solution, adding a sodium citrate solution, continuously stirring and heating, when the color of the solution is changed from colorless to dark red, adjusting the rotating speed to 600rpm, turning off a heating device, cooling at room temperature, filtering the reacted solution by using a water-based filter membrane, and drying to obtain the nano-gold star material. Removing impurities to obtain a gold seed solution; characterizing the gold seed solution and the gold seed particles; the preparation method comprises the following steps: adding a 4-hydroxyethyl piperazine ethanesulfonic acid solution, a gold seed solution, a hydroxylamine solution and a magnetic rotor into deionized water, dropwise adding a 22.5 mM chloroauric acid solution, adjusting the rotating speed to 700rpm, and reacting for 15 minutes at room temperature to obtain the nano gold star material. The prepared nano gold star material is uniform, stable, adjustable in particle size and high in dispersity, the material is in a three-dimensional multi-branch shape, and the diameter of the material is adjustable within 50-200 nm.

The invention provides a preparation method of milbemycin oxime A4, which comprises the following steps: under an acidic condition, carrying out hydrolysis disaccharide removal reaction on tenvermectin B to obtain tenvermectin B aglycone; the preparation method comprises the following steps: carrying out silicon-based protection on tenvermectin B aglycone by adopting a silicon-based protection reagent to obtain 5-hydroxyl silicon-based tenvermectin B aglycone; the preparation method comprises the following steps: brominating 5-hydroxyl silicon-based tenvermectin B aglycone by adopting a brominating reagent to obtain 13-bromine-5-hydroxyl silicon-based protected tenvermectin B aglycone; the preparation method comprises the following steps: reducing 13-bromo-5-hydroxyl silicon group protected tenvermectin B aglycone by using a reducing agent to obtain 5-hydroxyl silicon group protected milbemycins A4; the milbemycins A4 protected by the 5-hydroxyl silicon group is subjected to desilicication protection treatment, and the milbemycins A4 is obtained; oxidizing milbemycins A4 by adopting an oxidizing agent to obtain 5-ketomilbemycins A4; the preparation method comprises the following steps: reacting 5-ketomilbemycins A4 with hydroxylamine hydrochloride to obtain milbemycins A4, and efficiently preparing the active component milbemycins A4 single component by taking tenvermectin B as a raw material.

The invention relates to a method for simply and conveniently preparing high-purity lotinia, which comprises the following steps of: reacting 5-acetyl-3-methyl-2-thiophenecarboxylic acid with 2, 2, 2-trifluoro-1-trichlorophenyl ethyl-1-ketone to obtain 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-formic acid, and reacting the 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-formic acid with 2, 2, 2-trifluoro-1-trichlorophenyl ethyl-1-ketone to obtain 3-methyl-5-(4, 4, 4-trifluoro-3-trichlorophenyl butyl-2-enoyl) thiophene-2-carboxylic acid. Reacting the isoxazole thiophene formic acid compound with hydroxylamine hydrochloride to obtain an isoxazole thiophene formic acid compound; the preparation method comprises the following steps: reacting 5-[(5S)-5-trichlorophenyl-5-trifluoromethyl-4, 5-dihydro-isoxazole-3-yl]-3-methyl-thiophene-2-formic acid with (R)-1-(p-tolyl) ethyl-1-amine to obtain 5-[(5S)-5-trichlorophenyl-5-trifluoromethyl-4, 5-dihydro-isoxazole-3-yl]-3-methyl-thiophene-2-formic acid; and finally, carrying out condensation on the product and 2-amino-N-trifluoroethyl acetamide hydrochloride, so as to obtain the (5S)-configuration final product lotinib. The method has the advantages of short synthetic route, simple process, mild reaction and high chiral purity and HPLC purity, and is especially suitable for large-scale production.