464 results about "Hydroxylamine" patented technology

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 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 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 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 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 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 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 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 the technical field of palladium recovery, in particular to a method for recovering palladium. According to the technical scheme, the method comprises a precipitant pre-synthesis stage, a targeted palladium precipitation stage and a multi-stage reduction purification stage, and the precipitant pre-synthesis stage comprises the step of adding 10-15 parts by mass of butanedione, 18-30 parts by mass of hydroxylamine hydrochloride and 0.1-0.3 part by mass of iron phthalocyanine into a reaction kettle. Through a composite precipitator system and a multi-stage reduction process, the method has safety and high efficiency: flammable and explosive solvents such as ethanol and highly toxic reducing agents such as hydrazine hydrate are not needed, so that the potential safety hazard of production and the environment-friendly treatment cost are remarkably reduced; high-selectivity capture and efficient reduction of palladium are achieved through magnetic separation of magnetic nano-microspheres, induced precipitation of nitrogen-doped graphene quantum dots and a staged temperature-control and pressure-control reduction technology, the palladium recovery rate and purity are high, the process period is short, operation is controllable, and the method is suitable for industrial continuous production.

The invention discloses a preparation method of an electronic-grade hydroxylamine aqueous solution, and relates to the field of chemical preparation. The preparation method comprises the following steps: reacting electronic-grade ammonia water or organic alkali with electronic-grade hydroxylamine salt to generate a hydroxylamine aqueous solution; and after the reaction, separating through a POSS (Polyhedral Oligomeric Silsesquioxane) nano blending modified membrane, and removing salt, impurities and unreacted raw materials to obtain a high-purity hydroxylamine aqueous solution. And concentrating the solution into a 50% hydroxylamine aqueous solution by adopting a low-temperature vacuum concentration technology. The method can effectively remove metal ions and inorganic impurities, and ensures that the final product is high in purity and meets the electronic grade requirement.

The application provides a synthesis method of p-benzoquinone dioxime. The synthesis method comprises the following steps: (1) adding solid acid into an ethanol solution of phenol to obtain a mixed solution A, then vacuumizing and filling with inert gas; dissolving nitrite into ethanol, uniformly mixing to obtain an ethanol solution of nitrite, then vacuumizing and filling with inert gas; in an inert gas atmosphere, adding the ethanol solution of nitrite into the mixed solution A dropwise to perform nitrosation reaction, to obtain a reaction liquid B; in the inert gas atmosphere, adding an ethanol solution of hydroxylamine into the obtained reaction liquid B to perform oximation reaction; after the reaction is completed, filtering the obtained reaction liquid C, performing reduced pressure distillation on the obtained filtrate, and performing washing, filtering and drying on the obtained residual liquid of the reduced pressure distillation, to obtain p-benzoquinone dioxime. The method provided by the application reduces the occurrence of side reactions, improves the conversion rate of the reaction, and improves the yield and purity of p-benzoquinone dioxime.

The invention discloses a synthesis method of 9-dichloromethylene-5-amino-benzonorbornene and an intermediate product, the synthesis method comprises the following steps: firstly, synthesizing a cyclization compound 1 as shown in a formula 1 from a cold solution of 6, 6-dichlorofulvene and 1, 4-benzoquinone under the action of a solution of a catalyst I, carrying out oximation reaction on the cyclization compound 1 prepared in the step a and hydroxylamine salt under an alkaline condition, and carrying out post-treatment to obtain the 9-dichloromethylene-5-amino-benzonorbornene. Under the action of a catalyst II, adding the oximate 2 prepared in the step b into a closed container, carrying out hydrogenation reduction to obtain 9-dichloromethylene-5-amino-benzo norbornene, and directly treating the reduction product with acid to obtain 9-dichloromethylene-5-amino-benzo norbornene, namely the 9-dichloromethylene-5-amino-benzo norbornene, namely the 9-dichloromethylene-5-amino-benzo norbornene. According to the method, the cyclization compound is oximated firstly, then the residual carbonyl and two double bonds on the ring are subjected to one-step reduction through catalytic hydrogenation, the working procedure is optimized, meanwhile, reduction by using expensive sodium borohydride is avoided, the method is short in synthesis route and suitable for industrialization, and the production cost is reduced.

The invention discloses a preparation method of an arfamarana key intermediate, which comprises the following steps: carrying out nucleophilic addition reaction on a compound I and 1-[3-chloro-5-(trifluoromethyl) phenyl]-2, 2, 2-trifluoroethanone under the action of an organic solvent A and alkali to obtain a compound II; dissolving the compound II in an organic solvent B, adding concentrated sulfuric acid, carrying out intramolecular dehydration and cyanogen hydrolysis, and after the reaction is finished, cooling to room temperature for crystal growing to obtain a compound III; dissolving the compound III in an organic solvent C, carrying out intramolecular cyclization and ester hydrolysis reaction on the compound III and hydroxylamine hydrochloride under the action of a certain amount of sodium hydroxide aqueous solution, and after the reaction is finished, collecting a water phase and adjusting the pH value of the water phase, so as to obtain the key intermediate of arfampanaga. The reaction in each step has a high conversion rate, the purity of the prepared arfamarin intermediate is high, and powerful support and guarantee are provided for preparation of high-purity arfamarin.

The application discloses a synthesis method of afugan, which comprises the following steps: 1-[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroacetone and 4-acetylnaphthalene carboxylic acid are added into a solvent, a base is added, DMAP is added after complete reaction at 50-80 DEG C, acetic anhydride is added dropwise, tetrabutylammonium bromide is added after complete reaction, and an aqueous solution of sodium hydroxide and hydroxylamine hydrochloride is added, and reaction is carried out at 0-5 DEG C, so that an intermediate is obtained; the intermediate is reacted with acyl chloride under the action of DMF and dichloromethane, so that 4-(5-(3-chloro-5-(trifluoromethyl)phenyl)-5-(trifluoromethyl)-4,5-dihydroisoxazole-3-yl)-1-naphthalene carboxylic chloride is prepared; 2-amino-N-(2,2,2-trifluoroethyl)acetamide hydrochloride and a dichloromethane solution of a base are added dropwise, and reaction is carried out at 0-5 DEG C, so that afugan is obtained. The method has a short route, high yield and suitability for large-scale industrial production.

The invention discloses a method for coating pentazole hydroxylammonium salt with copper alginate, the pentazole hydroxylammonium salt is coated with a copper alginate gel network to form a composite material, the stirring rate and the dripping rate are strictly regulated and controlled by screening different mass ratios and drying modes, and the composite material is prepared. And an optimal experimental formula is screened out so as to achieve the purpose of reducing hygroscopicity and mechanical sensitivity. Compared with a pentazole hydroxylamine salt raw material synthesized in the early stage, the pentazole hydroxylamine-based composite energetic microsphere prepared by the preparation method disclosed by the invention is more regular in morphology, higher in sphericity degree, obviously reduced in sensitivity and hygroscopicity, easier to prepare medicines and capable of being popularized to preparation of composite microspheres of other energetic materials.

The invention relates to the technical field of uranium extraction fiber membranes, and discloses a preparation method of an MXene / PVDF / PAO photo-thermal-piezoelectric composite fiber membrane, and the preparation method comprises the following steps: S1, dissolving PAN in DMF, adding hydroxylamine hydrochloride and NaOH, and stirring to obtain a spinning solution I; s2, PVDF is dissolved in DMF, multiple layers of MXene materials are added, and a uniform spinning solution II is obtained through stirring; and S3, preparing the MXene / PVDF / PAO fiber membrane from the spinning solution I and the spinning solution II in a double-spinning form by using an electrostatic spinning device. And jointly assembling the PAO, the PVDF nano particles and the Mxene nano sheets into the electrostatic spinning membrane. Wave energy excites the piezoelectric effect of PVDF, and light energy is absorbed by Mxene. Compared with an existing scheme, water flow resistance is smaller, adsorption sites are more, and large-scale sea tests are better facilitated.

The invention discloses a metallocene polypropylene composite material as well as a preparation method and application thereof. The metallocene polypropylene composite material is prepared from the following components in parts by mass: 84.63 to 96.50 parts of metallocene isotactic polypropylene, 0 to 6 parts of polypropylene random copolymer, 3 to 9 parts of allyl elastomer, 0 to 3 parts of polypropylene wax, 0.10 to 0.55 part of organic peroxide degradation agent, 0 to 1.8 parts of hindered hydroxylamine ester degradation agent and 0 to 0.15 part of phosphate ester antioxidant. The metallocene polypropylene composite material is suitable for a melt-blowing processing technology, and the melt-blowing non-woven fabric of the metallocene polypropylene composite material has lasting filtering performance.

The invention discloses an electrolytic preheating-electrolytic ignition method for a three-electrode hydroxylamine nitrate liquid propellant, and belongs to the field of liquid rocket engines and electrochemistry. Three electrolysis electrodes are arranged in the electrolysis chamber and comprise two positive electrodes and one negative electrode, so that two groups of electrolysis electrode pairs are formed. The method comprises the following steps: injecting a nitric acid hydroxylamine-based liquid propellant into an electrolysis chamber, and electrifying a group of electrolysis electrodes to start electrolysis preheating; after the preset switching time is up, closing the current working electrolysis electrode pair, and switching to another group of non-working electrolysis electrodes to continue electrolysis; and low-voltage and rapid electrolytic ignition is realized. According to the three-electrode electrolysis structure, the time for ignition and reaction to reach the highest temperature can be shortened, and the system response speed is increased; the preheating and ignition voltage can be changed, and the large voltage adjusting and optimizing space is achieved; meanwhile, the electrolytic ignition current is relatively stable, and the instantaneous power consumption is small; and electrolysis power consumption can be saved, electrolysis electrode loss is reduced, and reuse of the electrode is facilitated.

This invention discloses a method for preparing a self-healing, antibacterial dynamic hydrogel and its coating application. The method includes: 1. Reacting konjac glucomannan with sodium periodate to achieve aldehyde functionalization, and mixing it with sodium alginate powder to prepare a precursor polymer solution A; 2. Mixing an acylhydrazide or hydroxylamine small molecule crosslinking agent with an aminoglycoside drug to prepare an amino crosslinking agent solution B, and preparing a calcium salt ionic crosslinking agent solution C; 3. Mixing the three solutions and allowing them to stand to obtain a hydrogel. The application involves coating a hydrogel mixture solution onto a biodegradable metal surface after preparing a polyethyleneimine auxiliary layer and then gelling it. This invention utilizes aldehyde-functionalized oxidized konjac glucomannan and two crosslinking agents to form acylhydrazone, oxime, and imine bond networks, endowing the hydrogel with self-healing, self-responsive, and long-term antibacterial properties. The hydrogel of this invention improves the biocompatibility, antibacterial properties, and stability of biodegradable metal substrates, making it suitable for biodegradable implantation applications.

The invention discloses a preparation method and application of a pydiflumetofen intermediate, and the method comprises the following step: in the presence of cuprous oxide or cuprous salt and acid, synthesizing 2, 4, 6-trichlorobenzene diazonium fluoroborate and isopropenyl acetate into the pydiflumetofen intermediate of formula I, according to the invention, 2, 4, 6-trichloroaniline which is cheap and easy to obtain is used as a raw material to improve a Meerwein arylation reaction method, and finally industrial cheap and mass production of the intermediate I is realized.

This invention provides a method for synthesizing a sulfonylpyrazole intermediate, belonging to the field of herbicide intermediate preparation technology. The method includes a condensation reaction of glyoxylic acid and hydroxylamine to generate 2-(hydroxyimino)acetic acid, followed by a chlorobromination reaction of the 2-(hydroxyimino)acetic acid to generate a chlorobromination intermediate. The chlorobromination intermediate then reacts with isobutylene to generate a sulfonylpyrazole intermediate. The key feature is that the chlorobromination reaction is carried out in the presence of sodium bromide and chlorine. This invention can maintain a stable reaction environment while improving the yield and purity of the intermediate product.

This invention discloses a synthetic process for 3-chloro-5,5-disubstituted-4,5-dihydroisoxazole. The process comprises the following steps: S1: Under acid catalysis, compound III undergoes a cyclization reaction with hydroxylamine and / or hydroxylamine salt to obtain compound V; S2: In a solvent, compound V undergoes a chlorination reaction with a chlorinating agent to obtain compound VI. This invention provides an economical, environmentally friendly synthetic process that improves the selectivity of 3-chloro-5,5-dimethyl-4,5-dihydroisoxazole, and has significant industrial application value.

The present application provides a chemical mechanical polishing liquid and a method for using the same. The chemical mechanical polishing liquid contains cerium oxide abrasive particles, hydroxylamine and its derivatives, and a pH adjuster, wherein the surface of the cerium oxide abrasive particles is positively charged. The chemical mechanical polishing liquid of the present application can reduce the polishing rate of the polishing liquid as the height of the pattern step on the wafer decreases, thereby achieving the function of automatic stop. The use conditions are relatively mild, and the chemical mechanical polishing liquid can be used in large-scale production, can be applied to pattern wafers with different patterns, and has a wide application prospect in the field.