23 results about "Hydroxylamine Hydrochloride" patented technology

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 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.

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.

This invention relates to the field of bionanomaterials technology, and particularly to mitochondrial-targeting nanomaterials based on ZnO quantum dots, their preparation methods, and applications. The preparation method of mitochondrial-targeting nanomaterials based on ZnO quantum dots includes the following steps: synthesis of 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 reaction is carried out with stirring at room temperature, and after post-treatment, silanized HNO donor is obtained; synthesis of zinc oxide quantum dots: zinc acetate dihydrate is dissolved in anhydrous ethanol, diethanolamine is added, the reaction is carried out, and after post-treatment, zinc oxide quantum dots are obtained. The preparation method can prepare mitochondrial-targeting nanomaterials that achieve precise delivery, controlled release, and visual tracking of HNO into cardiac mitochondria, solving the technical problems of traditional HNO donors' inability to achieve stable loading on a carrier and lack of targeting ability to mitochondria.

This invention belongs to the field of organic chemical synthesis technology, specifically relating to a method for synthesizing 2-fluoro-3-aminobenzoic acid, an important chemical intermediate. Specifically, o-nitroaniline is condensed with hydrated trichloroacetaldehyde and hydroxylamine hydrochloride to obtain 2-(hydroxyimino)-N-(2-nitrophenyl)acetamide; the resulting product undergoes an intramolecular Beckmann rearrangement to generate 7-nitroindigo; 7-nitroindigo undergoes Bayer-Villedge oxidation to generate 2-amino-3-nitrobenzoic acid; 2-amino-3-nitrobenzoic acid undergoes diazotization and halogenation reactions to generate 2-fluoro-3-nitrobenzoic acid or 2-chloro-3-nitrobenzoic acid; 2-fluoro-3-nitrobenzoic acid can be further reduced by nitro to obtain 2-fluoro-3-aminobenzoic acid; or, 2-chloro-3-nitrobenzoic acid can be esterified to obtain 2-chloro-3-nitrobenzoic acid ester, which can then be fluorinated, saponified, and reduced to obtain 2-fluoro-3-aminobenzoic acid. The raw materials of this invention are low in cost and readily available, and the entire reaction route has specific regioselectivity, making it suitable for industrial production.

The present application relates to the chemical technology field, specifically to a kind of preparation method of high-purity o-vanillin.The method uses o-methoxyphenylamine as starting material, with chloral hydrate and hydroxylamine hydrochloride is condensed, hydroxylamine oximation reaction, and cyclization reaction is carried out under strong acid condition, and compound 2 is generated;Compound 2 is oxidized under strong base condition, and compound 3 is generated;Compound 3 is esterified with primary alcohol to generate corresponding ester, and then reduction hydrogenation reaction is carried out under the action of strong reducing agent, and compound 4 is generated;Compound 4 is reacted with oxidizing agent in the presence of nitroxyl radical catalyst, and compound 5 is generated;Compound 5 carries out diazotization hydrolysis reaction, and o-vanillin is generated.The method avoids the problem of regioselectivity of traditional formylation reaction through specific reaction sequence, eliminates the generation of isomer impurities from the source, realizes the efficient, environmentally friendly, economic synthesis of high-purity o-vanillin, and provides high-quality raw material guarantee for downstream pharmaceutical.

The application relates to a preparation method of a networked amidoxime beta cyclodextrin adsorbent, which comprises the following steps: first, carrying out a first step reaction of beta-cyclodextrin and epichlorohydrin; then, adding acrylonitrile to carry out a second step reaction under a nitrogen atmosphere to obtain a networked beta-cyclodextrin acrylonitrile polymer; and finally, carrying out a third step reaction of the networked beta-cyclodextrin acrylonitrile polymer and hydroxylamine hydrochloride to obtain a networked beta-cyclodextrin amidoxime polymer. The synthesis steps are simple, water is used as a reaction medium (avoiding the use of a large amount of organic solvents), and the environment is good; the prepared adsorbent has excellent selectivity for gallium in Bayer mother liquor; the adsorption capacity of the adsorbent for gallium ions reaches 41.6 mg / g or more, and the saturated adsorption time is extremely short, which is 6 minutes; the adsorbent has excellent adsorption kinetics; in addition, the adsorbent has a stable structure, the adsorbent can be made into a liquid filter paper, has a long service life in the Bayer mother liquor, and the adsorption capacity retention rate is not less than 90% after 5 adsorption-desorption cycles.

The application provides a temperature control method for a hydrolysis section in the preparation process of O-trans-(3-chloro-2-propenyl) hydroxylamine hydrochloride, and belongs to the technical field of safety temperature control in organic synthesis. The application converts the reaction heat into latent heat of vaporization of low-temperature liquid immediately by adopting a spraying instantaneous heat removal scheme on the existing hydrolysis tower; a multi-point temperature monitoring system is interlocked with a spraying system and a refrigeration unit to form three-parameter closed-loop control of "temperature-rate-flow", and the closed-loop interlocking ensures that the cooling intensity automatically increases with the temperature rise. Any parameter exceeding the limit triggers the maximum cooling mode, so that the temperature of any point in the whole hydrolysis process is less than or equal to 75 DEG C, the temperature is lowered by less than or equal to 67 DEG C within 60 s after starting within 30 s, the system temperature is prevented from being out of control, and local temperature runaway is prevented.

This invention belongs to the field of organic synthesis technology and discloses a method for preparing trans-3-chloro-2-propenylhydroxylamine hydrochloride. The method involves adding trans-1,3-dichloropropene to a ketoxime, a base, a phase transfer catalyst, and a first solvent for etherification. After the reaction, the mixture is first extracted with an extractant, and the resulting oil phase is then distilled to obtain the oxime ether. The oxime ether, an aqueous hydrochloric acid solution, and a second solvent are mixed and subjected to vacuum distillation in a distillation column to obtain trans-3-chloro-2-propenylhydroxylamine hydrochloride. This invention avoids the use of an aqueous base in the etherification stage, effectively preventing the hydrolysis of the ketoxime. The purified oxime ether obtained in the etherification step is purified by distillation, significantly reducing side reactions during the subsequent hydrolysis. Adding a solvent during the hydrolysis stage allows for better mixing of the aqueous hydrochloric acid solution and the oxime ether, resulting in more uniform acidification, a more complete reaction, and improved conversion and selectivity.

This invention belongs to the field of herbicide technology and aims to solve the problems of complex preparation processes for dichloroisoxaflubenzuron, high equipment requirements, and environmental disadvantages. To this end, this invention provides a green synthetic method for preparing dichloroisoxaflubenzuron and the application of the prepared product in herbicides. The method includes reacting 5-hydroxymethylfurfural with hydroxylamine hydrochloride to generate an oxime product, followed by the direct addition of a propynic acid derivative, and cyclization under a first bifunctional catalyst and a hydrogen atmosphere to generate intermediate I; dissolving or dispersing intermediate I in a chloride-containing electrolyte and anolyzing it to generate a dichloro intermediate II; reacting dichloro intermediate II with an acrylate compound under light conditions and a catalyst in a one-pot conversion reaction to directly obtain crude dichloroisoxaflubenzuron; and finally, introducing the crude product into a continuous crystallization and separation device to obtain a high-purity dichloroisoxaflubenzuron product. This invention features a simple process, reduces equipment requirements, and is environmentally friendly.

This invention discloses a method for preparing a high-efficiency uranium extraction hydrogel from seawater, comprising the following steps: Step I: Hydroxylamine hydrochloride is completely dissolved in dimethylformamide (DMF), then Na2CO3 and NaOH are added and stirred rapidly; Step II: Polyacrylonitrile (PAN) is added to the above mixture for reaction, and the resulting reaction mixture is filtered twice through a 0.22 μm filter membrane to obtain poly(aminoamine)oxime (PAO); Step III: A precursor solution containing Zn(NO3)2·6H2O and Cu(NO3)2·3H2O is added in batches to an aqueous solution of Na2CO3, and NaOH solution is gradually added dropwise to adjust the pH; Step IV: The suspension is continuously stirred in a water bath, filtered, thoroughly washed with acetone, and dried to obtain Zn-Cu layered hydroxide (ZnCu-LDH); Step V: The PAO solution and ZnCu-LDH are mixed in a certain proportion to rapidly form a hydrogel. Practical verification shows that the PAO-ZnCu-LDH hydrogel has an adsorption capacity of up to 282 mg / g for uranium. This invention features a simple, quick, and reliable preparation process with high adsorption performance, making it a promising candidate for application in the field of ion selective recovery.

The present invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-methoxy oxime ether. The method comprises the following steps: (1) chlorination reaction: adding a chlorinating agent into aniline as a raw material in a solvent at 0-10°C, and performing a chlorination reaction to obtain 2,4,6-trichloroaniline; (2) coupling reaction: subjecting 2,4,6-trichloroaniline, isopropenyl acetate and a catalyst to a coupling reaction in a solvent under the initiation of nitroxyl ions, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone; (3) oximation reaction: subjecting 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone and hydroxylamine hydrochloride to an oximation reaction in a solvent under the action of an alkali, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-oxime; and (4) methylation reaction: subjecting 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-oxime and chloromethane to a methylation reaction in a solvent under the action of an alkali, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-methoxy oxime ether.

A synthesis method for selamectin was developed, where doramectin is oxidized by manganese dioxide, oximated and de-sugared in one-step by an aqueous solution of hydroxylamine hydrochloride, and then selectively reduced in the presence of Wilkinson's catalyst and hydrogen to obtain selamectin. Doramectin is oxidized to a carbonyl group firstly, so that the generation of impurities during the subsequent reaction is reduced; t-butyl alcohol with a larger steric hindrance is used as a solvent, so that transesterification impurities are avoided; the hydrogenation is implemented in the final step, and the crude product is recrystallized before the hydrogenation reaction, so that the cost is greatly reduced. The method of the present application with an overall yield of 57%. The purity of product was 97.11%. All impurities meet the requirements of Pharmacopoeia. The present application is a simpler, more economical and more efficient synthesis method, and is suitable for industrial production.

The application belongs to the technical field of seawater uranium extraction, and particularly relates to a uranium adsorption fiber material and a preparation method and application thereof. The preparation method of the uranium adsorption fiber material comprises the following steps: mixing hydroxylamine hydrochloride, a carbonate, polyacrylonitrile powder and an organic solvent to perform an amidoxime reaction, so as to obtain polyacrylonitrile amidoxime spinning solution; mixing the polyacrylonitrile amidoxime spinning solution and capsaicin powder to obtain spinning solution doped with capsaicin; and performing electrostatic spinning on the spinning solution doped with capsaicin, and soaking the obtained electrostatic spinning film in lye to obtain the uranium adsorption fiber material. The uranium adsorption fiber material has improved biological adhesion resistance, and the prepared uranium adsorption fiber material has good antibacterial performance and good uranium adsorption capacity.

This invention discloses a chiral amination synthesis process for a pharmaceutical intermediate, comprising two steps: First, hydroxylamine hydrochloride and compound I are mixed in a 40-50 wt% aqueous ethanol solution, and an alkaline reagent is added to adjust the pH to 4-6. The mixture is then heated under reflux to generate an oxime ether compound II. Second, compound II is dissolved in THF or toluene, and a chiral spiroboroate catalyst derived from diphenylvaline is added. A BH3·THF reducing agent is then slowly added dropwise at room temperature to perform an asymmetric reduction to obtain a chiral primary amine compound III. The advantages of this invention are: the reaction route avoids high-risk reagents and harsh conditions, significantly improving process safety; and through process route optimization, efficient asymmetric reduction is achieved, resulting in a product with high chiral purity. The reaction route of this invention features mild reaction conditions, simple operation, and is easy to scale up industrially. The overall route is concise, with short steps and high yield, making it suitable for large-scale industrial production.

This invention relates to a method for enhancing in-situ oxidation of persulfate to remove petroleum hydrocarbons from soil, belonging to the field of soil remediation technology. The method for removing petroleum hydrocarbons from soil according to this invention includes the following steps: a) adding 3-6% (by weight of the soil) of sodium persulfate to the contaminated soil, mixing thoroughly, and reacting until the sodium persulfate content in the soil decreases to 40-60%; b) continuing to add hydroxylamine hydrochloride, the amount of hydroxylamine added being 2.4-3.6% of the mass of sodium persulfate added in step a; c) reacting until the sodium persulfate content in the soil decreases to 5-15%. Compared with existing methods, this method for removing petroleum hydrocarbons from soil has lower soil remediation costs and significantly better results.

This invention discloses a high-yield method for preparing hydroxamic acid, relating to the field of organic synthesis technology. The specific steps are as follows: Hydroxylamine hydrochloride is dissolved in water and cooled; liquid alkali is added dropwise to generate free hydroxylamine; a carboxylic acid ester is added, and the pH is adjusted to 8–10, reacting until the ester residue is ≤2%; a small amount of the corresponding acyl halide is added, and the pH is maintained to continue the reaction until complete; acidification and crystallization yield high-purity hydroxamic acid. This invention uses carboxylic acid ester as the main raw material and a small amount of acyl halide as a synergist, employing a staged reaction to overcome the later-stage kinetic bottleneck, significantly reducing ammonia nitrogen in wastewater. The process is mild, low-cost, and easily industrialized, suitable for the preparation of high-purity products such as benzoyl hydroxamic acid, salicylic acid, and octanoyl hydroxamic acid.

The application discloses a method for preparing a mesoporous hollow nanoscale spherical structure adsorbent based on emulsion and micelle assembly and application of the adsorbent in uranium extraction. The mesoporous hollow nanoscale spherical structure material is combined with an amidoxime group, and a green and efficient uranium extraction adsorbent is prepared through a soft template method, self-polymerization of dopamine and amidoximation reaction. First, a nonionic surfactant, dopamine hydrochloride and an expanding agent 1,3,5-trimethylbenzene are used to form an emulsion / micelle system, ammonia is added after stirring to initiate the oxidative self-polymerization reaction of dopamine, and a mesoporous hollow nanoscale spherical catecholamine polymer MHS is prepared; then, a functional monomer 2-amino-3,5-divinylbenzonitrile is grafted to the MHS under the initiation of AIBN, and a cyan-amino bifunctionalized nanosphere CN-NH2-MHS is obtained; finally, the CN-NH2-MHS is chemically modified by hydroxylamine hydrochloride, the cyan group is converted into an amidoxime AO group, and thus an amidoxime-amino synergistically functionalized high-stability mesoporous hollow nanoscale spherical structure adsorbent AO-NH2-MHS is prepared.

This invention discloses a graft-modified amylopyridine-oxime-modified copolymer resin porous microsphere. Acrylonitrile, methyl methacrylate, and styrene are used as comonomers, divinylbenzene as a crosslinking agent, and azobisisobutyronitrile as an initiator. The copolymer resin microspheres ANMA are formed by suspension polymerization, followed by amylopyridine oxime-modification reaction with hydroxylamine hydrochloride solution to obtain amylopyridine-oxime-modified microspheres AOMA. Finally, AOMA-PEI is obtained through ethylenediamine amination, glutaraldehyde activation, and graft modification with polyethyleneimine (PEI). AOMA-PEI contains amylopyridine-C(NH2)=N-OH and aliphatic amine C-N groups. Its microstructure is a micron-sized spherical structure with a specific surface area of ​​93-99 m². 2 / g, mesopore volume data is 0.30-0.40 cm³. 3 / g; strength is 31-35 MPa, tensile stress is 55-60 MPa. Its preparation method includes the following steps: 1. Synthesis of ANMA microspheres; 2. Amine oxime modification of ANMA; 3. Grafting of polyethyleneimine. When used as a column adsorption material in molybdenum technetium generators, the adsorption capacity remains at 350-440 mg / g under irradiation conditions with an absorbed dose of 50-500 kGy.

This invention discloses substituted isoxazoline carboxylic acid methyl ester compounds, their preparation methods, and applications. Using concentrated sulfuric acid as a solvent, concentrated nitric acid is reacted with compound (I) to generate compound (II), which then reacts with a saturated aqueous solution of hydroxylamine hydrochloride to generate compound (III). Compound (III) reacts with NCS and MMA to generate compound (IV). Iron powder is used as a reducing agent to reduce compound (IV) to generate compound (V). Using DCM and n-butanol as solvents, and EDCl and DMAP as condensing agents, compound (V) is reacted with compound (VI) to obtain the target product, the substituted isoxazoline carboxylic acid methyl ester compound. Herbicidal activity tests at 100 ppm show excellent herbicidal activity in dicotyledonous rapeseed and monocotyledonous wheat. Compound VII12, at a concentration of 10 ppm, also exhibits excellent herbicidal activity in dicotyledonous rapeseed and monocotyledonous wheat.

This invention provides a cerium valence regulator for high-abundance cerium magnets and a method for preparing high-abundance cerium magnets, belonging to the field of rare earth permanent magnet technology. The cerium valence regulator for high-abundance cerium magnets provided by this invention comprises the following components by volume percentage: hydroxylamine hydrochloride 1-10%; tributyl phosphate 5-8%; and the balance being hydrocarbon solvent. In this invention, hydroxylamine hydrochloride facilitates the regulation of cerium valence, while tributyl phosphate plays a stabilizing role in the cerium valence regulator. Using the cerium valence regulator provided by this invention, it is possible to prepare high-abundance, high-performance cerium magnets with a 50% cerium-to-praseodymium / neodymium weight percentage, remanence Br ≥ 12 kGs, and intrinsic coercivity Hcj ≥ 12 kOe. Compared with current technologies, the high-abundance cerium permanent magnets obtained by this invention have approximately 30% higher trivalent cerium content, approximately 1.5% higher remanence Br, and approximately 8% higher coercivity.

This invention relates to the field of indigo synthesis technology, specifically a method for synthesizing 6-chloro-7-fluoroindigo, including intermediate synthesis. 470 mL of water is added to a reaction flask, followed by the sequential addition of 5.5 mL of concentrated sulfuric acid, 28.64 g of hydroxylamine hydrochloride, 25 g of chloral hydrate, and 20 g of 3-chloro-2-fluoroaniline under stirring. After a white solid precipitates, 100-200 g of anhydrous sodium sulfate is added, and the mixture is heated to reflux for 1.5 hours. After monitoring the remaining raw material at less than 3% using online HPLC, the mixture is cooled to 0°C and filtered. The filter cake is recrystallized using an ethanol-water mixed solvent. The cyclization reaction utilizes a single or composite organic sulfonic acid catalyst, or a recyclable solid acid catalyst, to replace traditional concentrated sulfuric acid. This method has low equipment requirements, is equipped with temperature and pressure interlock devices for automatic cooling and pressure relief, and provides mild and safe reaction conditions, reducing safety risks. Through optimization of the catalyst system, reaction temperature, and time, the cyclization yield is increased from 25.4% to over 50%, significantly improving yield and production efficiency.

The application provides a gold-silver alloy nanoparticle and a preparation method and application thereof, and the preparation method comprises the following steps: reacting water, silver sulfide quantum dots and polyvinylpyrrolidone powder at 0 DEG C until the reaction is sufficient, centrifuging, and obtaining a silver sulfide supernatant; mixing chloroauric acid, a sodium citrate solution and a NaOH solution at room temperature until the reaction is sufficient, and obtaining a reaction liquid; mixing the obtained silver sulfide supernatant and the obtained reaction liquid, adding polyvinylpyrrolidone, adding a hydroxylamine hydrochloride solution and a NaOH solution in sequence after reaction, fully reacting, and obtaining gold-silver alloy ions; and purifying the obtained gold-silver alloy ions, so that the gold-silver alloy nanoparticle is obtained. The preparation method adopts an aqueous phase method to synthesize the gold-silver alloy nanoparticle, the synthesis process is simple, green and environment-friendly, and the synthesis means of the gold-silver alloy nanoparticle is enriched; and the gold-silver alloy nanoparticle has potential application in the research of Alzheimer's disease and can effectively inhibit the incorrect folding of A beta 40 protein.