283 results about "Hydroxylamine Hydrochloride" patented technology

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 invention relates to a preparation method of 2-(2-amino-5-bromo-benzoyl) pyridine, which comprises the following steps: (1) dissolving 2-amino-5-bromobenzoic acid in an organic solvent A, adding dimethyl hydroxylamine hydrochloride, a condensing agent and organic alkali, and carrying out condensation reaction to obtain 2-amino-5-bromo-N-methoxy-N-methyl benzamide; and (2) in an organic solvent B, enabling 2-bromopyridine to react with the 2-amino-5-bromo-N-methoxy-N-methyl benzamide in the step (1) under the action of an organic strong base, so as to obtain the 2-(2-amino-5-bromo-benzoyl) pyridine. The preparation method provided by the invention has the advantages of easily available synthesis raw materials, low cost, simple synthesis route, safe and controllable synthesis process and simple post-treatment method, has no amplification effect, and is suitable for industrial large-scale production.

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 invention relates to a method for synthesizing trifloxystrobin through a one-pot method, and belongs to the technical field of organic synthesis.The method comprises the following steps that 1, E-2-(2-halomethylphenyl)-2-methoxyiminoacetic acid methyl ester, m-trifluoromethyl acetophenone, hydroxylamine hydrochloride or hydroxylamine sulfate and a solvent are added into a reaction flask, then alkali is added, and after addition is completed, a heat preservation reaction is conducted; and Step 2, after the reaction is finished, filtering to remove salt, and concentrating filtrate under reduced pressure to obtain trifloxystrobin. Compared with a traditional synthesis method of the trifloxystrobin, the synthesis method of the trifloxystrobin has the advantages that the 3-trifluoromethyl acetophenone and the E-2-(2-halomethylphenyl)-2-methoxyiminoacetic acid methyl ester are used as raw materials, the trifloxystrobin is directly synthesized by a one-pot method, the reaction route is short, the raw material cost is low, and the synthesis method of the trifloxystrobin by the one-pot method has the advantages that the synthesis efficiency is high, and the synthesis cost is low. The preparation method has the advantages that the preparation of m-trifluoromethyl acetophenone oxime from m-trifluoromethyl acetophenone is not needed, the whole synthesis process is simpler and more efficient, the reaction conditions are mild, and the preparation method is suitable for industrial large-scale production.

The invention discloses a flame-retardant polyurethane composite material and a preparation process thereof, and relates to the field of high polymer materials. When the flame-retardant polyurethane composite material is prepared, tetramethyl tetravinyl cyclotetrasiloxane reacts with DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) to obtain phosphorus modified cyclotetrasiloxane; then, lignin sequentially reacts with 3-aminopropyldimethoxymethylsilane and phosphorus modified cyclotetrasiloxane, and modified lignin microspheres are obtained; the preparation method comprises the following steps: reacting 2, 4-pentanedione, 1, 5-dichloro and hydroxylamine hydrochloride to obtain a dioxime monomer; and uniformly mixing isophorone diisocyanate, 1, 4-butanediol, a dioxime monomer, N, N-dimethyl hexylamine, the modified lignin microspheres and deionized water, pouring into a mold, and curing to obtain the flame-retardant polyurethane composite material. The flame-retardant polyurethane composite material prepared by the preparation method disclosed by the invention has excellent antibacterial property, flame retardance and self-repairing property.

The invention relates to the technical field of benzamide, in particular to a preparation process of 4-hydroxythiobenzamide, which comprises the following steps: S1, preparing raw materials: preparing the 4-hydroxythiobenzamide from the following raw materials in parts by weight: 80-100 parts of formic acid, 80-100 parts of hydrochloric acid, 20-30 parts of 4-hydroxybenzaldehyde, 8-12 parts of hydroxylamine hydrochloride, 8-12 parts of thioacetamide and 4-6 parts of sodium hydroxide. According to the preparation method, after 4-hydroxybenzaldehyde is subjected to activating treatment reaction, part of positive charges on aldehyde carbon are dispersed, oxygen atoms in an acetal structure are connected with the aldehyde carbon through covalent bonds to generate an electron withdrawing induction effect, the reaction sequence and the reaction path of the 4-hydroxybenzaldehyde can be controlled through aldehyde activation, and the reaction efficiency of the 4-hydroxybenzaldehyde is improved. Therefore, the generation of byproducts is reduced, and the purity of a reaction product obtained from 4-hydroxybenzaldehyde is improved.

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 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 invention provides a water-phase preparation method of sodium citrate-mediated size-controllable gold layer-coated ferroferric oxide nanoparticles. The water-phase preparation method comprises the following steps: step 10, preparing a sodium citrate-modified ferroferric oxide nanoparticle solution; and step 20, adding a sodium citrate solution, a chloroauric acid solution and a hydroxylamine hydrochloride solution into the sodium citrate modified ferroferric oxide nano-particle solution to prepare the gold layer coated ferroferric oxide nano-particles. According to the water-phase preparation method of the sodium citrate-mediated size-controllable gold layer-coated ferroferric oxide nano-particles, provided by the invention, the preparation of the gold layer-coated ferroferric oxide nano-particles with controllable size, adjustable magnetic nucleus size, no intermediate layer and low cost can be realized.

The invention is applicable to the technical field of soil detection, and particularly provides an analysis method for gradually and continuously extracting a silicon form in soil, which adopts a step-by-step continuous extraction method and sequentially adopts an acetic acid-sodium acetate solution, hydrogen peroxide, an acetic acid-sodium acetate solution, a hydroxylamine hydrochloride solution and a sodium hydroxide solution as extracting agents. The method comprises the following steps: fully oscillating with a soil sample to extract different forms of silicon, and determining the silicon content by using a silicon molybdenum blue colorimetric method, so that the content of the silicon in each form, including effective silicon, organic combined silicon, iron and manganese oxide combined silicon and amorphous silicon, in the soil can be rapidly detected. And the content of amorphous silicon in the soil can be obtained. The soil silicon form analysis method is simplified, the detection efficiency is improved, and a theoretical basis is provided for knowing the soil silicon supply capacity and evaluating the silicon nutrition effect in the soil.

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 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.

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 belongs to the technical field of rare earth material analysis, and particularly relates to an ultra-trace analysis method for a copper element in a rare earth material based on an extraction principle, and the analysis method comprises the following steps: dissolving a rare earth oxide sample with 1: 1 hydrochloric acid, and drying by distillation to obtain a sample solution; sequentially adding an ammonium citrate solution, a hydroxylamine hydrochloride solution and a copper reagent solution into the sample solution, stirring for 1-2 minutes at the rotating speed of 150-200rpm, dropwise adding ammonia water with the ratio of 1: 5 to adjust the pH value to be 9-10, and forming a complex by Cu < 2 + > and a copper reagent to obtain a complex solution; adding an extracting agent into the complex solution, oscillating and extracting for 1-2 minutes, standing and layering for 10-15 minutes, and taking a lower layer organic phase; when ultra-trace analysis is carried out on the copper in the rare earth element, through specific chemical treatment, other elements or compounds which may interfere with determination are reduced, and through collaborative optimization of chemical extraction and spectrophotometry, the lower detection limit of the copper in the rare earth element is reduced to 0.1 ppm from traditional 2ppm.

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 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.

A synthesis method of 2-chloro-4-bromobenzonitrile comprises the following steps: S1, adding methylchloroaniline and hydrobromic acid into a solvent a, dropwise adding a sodium nitrite solution, rapidly cooling to room temperature after the reaction is completed, and filtering to obtain a compound I; s2, adding the compound I, bromine and a solvent b into a reaction kettle, stopping heating after the reaction is completed, naturally cooling to room temperature, and filtering to obtain a compound II; s3, adding the compound II, hydroxylamine hydrochloride and sodium hydroxide into the reaction kettle, stopping heating after the reaction is completed, naturally cooling to room temperature, and filtering to obtain a compound III; s4, adding the compound III into thionyl chloride and a solvent c, stopping heating after the reaction is completed, naturally cooling to room temperature, and filtering to obtain 2-chloro-4-bromophenoxybenzene; and (S5) carrying out cyclohexane refining on the 2-chloro-4-bromobenzonitrile. According to the synthetic method of the 2-chloro-4-bromobenzonitrile, the 2-chloro-4-bromobenzonitrile is synthesized through four-step reaction of diazotization, hydroformylation, oximation and nitrilation, and the method is simple in process, stable in quality, low in energy consumption and easy to produce.

The invention discloses a synthetic method of a substituted trans-dicyclohexyl alkenyl liquid crystal monomer, which comprises the following steps: reacting 4, 4 '-dicyclohexyl ketone with chloromethyl ether phosphine salt and potassium tert-butoxide at-10 DEG C to 0 DEG C to form 4, 4'-dicyclohexyl diene methyl ether; reacting with hydroxylamine hydrochloride under the action of a first catalyst to generate 4, 4 '-dicyclohexyl dioxime; under the action of a second catalyst, carrying out unilateral deprotection to generate 4-oxime 4 '-dicyclohexylformaldehyde; the preparation method comprises the following steps: reacting 4-oxime with R1BrPPh3 and potassium tert-butoxide at the temperature of 10 DEG C below zero to 0 DEG C to obtain 4-oxime 4 '-dicyclohexyl alkyl ethylene; reacting with formic acid to generate 4-formaldehyde-4 '-dicyclohexyl alkyl ethylene; the substituted trans-dicyclohexyl alkene liquid crystal monomer is prepared by reacting the substituted dicyclohexyl alkene with R2BrPPh3 and potassium tert-butoxide at the temperature of-10 DEG C to 0 DEG C to obtain a cis-trans mixture and carrying out transposition. The method comprises seven steps of reaction, transposition and purification are not needed in the early stage, transposition crystallization is only needed in the last step, and the total yield can reach 70% or above. The raw materials are cheap, easily available and low in cost.

The present invention relates to a corrosion gel for weld detection, a preparation method, a corrosion method and a weld surface crack detection method, belonging to the technical field of weld detection. The corrosion gel for weld detection comprises the following raw materials: agar, water, 98% sulfuric acid, 10% hydroxylamine hydrochloride solution, p-tolylthiourea, stannous sulfate, thiourea, 10% Triton X-100 solution and 0.05% ethanol solution of o-phenanthroline derivative. The preparation method of the corrosion gel for weld detection comprises the following steps: weighing agar and dissolving it in water; sequentially adding 98% sulfuric acid, hydroxylamine hydrochloride solution, p-tolylthiourea, stannous sulfate, thiourea, Triton X-100 solution and ethanol solution of o-phenanthroline derivative; adding 100 mL of ethanol solution of o-phenanthroline derivative and mixing evenly to obtain a hot corrosion gel. A weld surface crack detection method comprises the following steps: making an indicating electrode; preparing a corrosion gel; treating the weld with the corrosion gel; evaluating the weld crack.

This invention belongs to the field of soil manganese extraction technology, and discloses a stepwise extraction method and application for manganese species in soil. First, exchangeable manganese is extracted using magnesium chloride; then, manganese carbonate and sulfides are extracted using hydrochloric acid; next, active Mn(III) bound to organic matter is extracted using pyrophosphate solution under alkaline pH; then, manganese oxides are dissolved using hydroxylamine hydrochloride; and finally, manganese bound to crystalline iron and manganese oxides is extracted using sodium dithionite solution. This stepwise extraction scheme accurately quantifies the concentration of active Mn(III) species bound to organic matter in the soil. Experimental results show that the extraction method of this invention can effectively separate different forms of manganese in soil. In particular, PP extraction successfully distinguishes Mn(III) bound to organic matter without introducing interfering substances such as iron minerals that may interfere with dissolution.

The invention discloses an organic peroxide reaction endpoint rapid detection method and application thereof, and belongs to the technical field of organic chemistry. The invention aims to solve the technical problems that the reaction endpoint of an organic peroxide initiator is difficult to judge, the generated organic peroxide is easy to decompose due to too long reaction time, and the reaction is incomplete and raw materials are remained due to too short reaction time, and provides a rapid detection method for acyl chloride residues in the organic peroxide reaction process. Therefore, the reaction endpoint is determined. According to the technical scheme, the method for rapidly detecting the reaction endpoint of the organic peroxide is characterized in that in the reaction process of an organic peroxide initiator, acyl chloride is gradually consumed, the content is reduced, and the acyl chloride completely reacts when the reaction endpoint is reached. Through reaction of different acyl chloride concentrations and hydroxylamine hydrochloride, a standard curve or a color card is established, the residual amount of acyl chloride is judged, and the reaction endpoint is accurately judged.

The application discloses a hydroxylamine hydrochloride detection method in azithromycin dry suspension, and relates to the trace detection field. The method uses isoamyl aldehyde as a derivatizing agent, generates isoamyl aldoxime by performing derivatization treatment on a sample to be measured, and then uses N-nitrosodiisopropylamine as an internal standard substance to quantitatively determine the isoamyl aldoxime by using liquid chromatography-tandem mass spectrometry. The detection method adopts an isoamyl aldehyde derivatizing agent-N-nitrosodiisopropylamine internal standard substance system, can correct detection errors caused by factors such as matrix effect, pretreatment loss and derivatization efficiency fluctuation, and improves the accuracy and sensitivity of the trace hydroxylamine hydrochloride detection result, thereby guaranteeing the safety of the medicine.

The invention relates to the technical field of graphene modification, and particularly discloses a preparation method of modified graphene for lubricating oil, which comprises the following steps: ultrasonically dispersing graphene in water to obtain a graphene dispersion liquid; potassium octadecyl benzene sulfonate is added into the graphene dispersion liquid, and a stirring reaction is performed for 10-20 min; then adding ammonium molybdate and sodium sulfide into the system, adjusting the pH value of the reaction system to 4.5-6, and reacting for 1-2 hours under the reflux stirring action at 60-110 DEG C; adding hydroxylamine hydrochloride into the reaction system, and continuously stirring to react for 2-4 hours; and finally, carrying out centrifugal separation on the reaction liquid, washing with ethanol and distilled water for multiple times, and carrying out centrifugal separation to obtain the modified graphene. According to the preparation method of the modified graphene provided by the invention, a stable and uniform lubrication enhancement layer can be constructed on the surface of the graphene in situ, so that the graphene is endowed with excellent oil solubility and oil phase dispersion stability.

The present invention relates to an iron ore reverse flotation inhibitor and a preparation method thereof. In the first step, a mixture of the following components by weight is reacted at 40°C to 50°C for 1 to 6 hours to obtain an auxiliary agent (1): 100 parts of corn starch, mung bean starch, or potato starch, 0.5 to 4.0 parts of sodium hydroxide or sodium ethoxide, 5 to 15 parts of methyl chloroacetate, and 5 to 15 parts of hydroxylamine hydrochloride or hydroxylamine sulfate. In the second step, a mixture of the following components by weight is reacted at 20°C to 50°C for 1 to 3 hours to obtain a finished inhibitor: 100 parts of the auxiliary agent (1) obtained in the first step and 1 to 12 parts of sodium hypochlorite. The inhibitor has strong inhibitory ability, selectivity, and low-temperature adaptability and can be used for room-temperature flotation.

The invention relates to the technical field of organic synthesis, in particular to the field of IPC C07D239, and more particularly relates to a synthesis method of a phenyl isoxazoline compound. Comprising the following steps: step 1, using a benzaldehyde compound as an initial raw material, and reacting with hydroxylamine hydrochloride to generate a benzaldoxime compound; 2, carrying out a chlorination reaction on the benzaldoxime compound generated in the step 1 and liquid chlorine through a microchannel reactor to generate a chlorinated benzaldoxime compound; and 3, carrying out ring closing on the chlorobenzaldoxime compound generated in the step 2 and an alkene compound to obtain the phenyl isoxazoline compound. A metal catalyst is not used in the preparation method, so that the solid waste treatment cost is reduced; in the step 2, a continuous flow reaction technology of a microchannel reactor is adopted, the reaction time is shortened, compared with a kettle type intermittent process, the productivity is greatly improved, and the reaction safety is higher.

This invention relates to the field of bionanomaterials technology, and particularly to mitochondrial-targeting nanomaterials capable of releasing HNO, their preparation methods, and applications. The preparation method of the mitochondrial-targeting nanomaterials capable of releasing HNO includes the following steps: synthesis of a silanized HNO donor: hydroxylamine hydrochloride is dissolved in a mixed solvent of anhydrous tetrahydrofuran and anhydrous pyridine, and a dichloromethane solution of 2-(4-chlorosulfonylphenyl)ethyltrimethoxysilane is added. The mixture is stirred at room temperature, and after post-treatment, a silanized HNO donor is obtained; synthesis of aminated carbon dots: chitosan, ethylenediamine, and mercaptosuccinic acid are dispersed in deionized water, and concentrated hydrochloric acid is added and stirred until dissolved. This preparation method can prepare mitochondrial-targeting nanomaterials capable of releasing HNO, achieving precise delivery, controlled release, and visual tracking of HNO to cardiac mitochondria, solving the technical problems of traditional HNO donors' inability to achieve stable loading on carriers and lack of mitochondrial targeting ability.

The present invention discloses an N-aryl-N-alkyl-O-allylhydroxylamine compound and its synthesis method. The general structural formula is as follows: The synthesis method includes the following steps: Using cheap and easily available aldehydes or ketones as starting materials, reacting with hydroxylamine hydrochloride to form oximes, and then preparing N-alkylhydroxylamines under the action of a supported metal catalyst; N-alkylhydroxylamines react with (R4-substituted) allyl bromide, etc. in the presence of a weak base to prepare N-alkyl-N-allylhydroxylamines; N-alkyl-N-allylhydroxylamines react with aryl alkyne precursors under the action of an initiator fluoride at room temperature to prepare N-aryl-N-alkyl-O-allylhydroxylamine compounds. The method of the present invention can effectively avoid the use of toxic, harmful, and explosive strong oxidants, and at the same time solve the problems of limited raw material sources, high prices, harsh reaction conditions, and low reaction selectivity in the existing synthesis methods.

The invention provides a preparation process and system of N-benzyl hydroxylamine hydrochloride, and the preparation process utilizes a microchannel reactor and a film concentration device to realize synthesis of a target product through a two-step method. The method comprises the following steps: firstly, continuously pumping dibenzylamine, an auxiliary agent and hydrogen peroxide into a micro-channel reactor, and carrying out accurate temperature control and efficient mixing under a micro-scale to promote an oxidation reaction to be rapidly completed so as to generate a key nitrone intermediate; the step effectively avoids the dangerous thermal runaway phenomenon possibly occurring in a traditional reaction kettle, and the operation safety is improved. Then, introducing the nitrone intermediate and hydrochloric acid into a film concentration device; in the device, the nitrone intermediate is hydrolyzed under an acidic condition, and meanwhile, a reaction solution can be quickly evaporated by a film concentration technology, so that a solvent and byproducts generated along with the reaction are efficiently removed. The thin film concentration technology not only inhibits the occurrence of side reactions, but also ensures the high yield and high purity of the final product.