67 results about "Acetone oxime" patented technology

The invention discloses a reduction method for graphene oxide. The method comprises the following steps: using acetone oxime, acetaldoxime or methyl ethyl ketoxime as a reducing agent, and then preparing the graphene by reducing the graphene oxide in a graphene oxide aqueous solution the pH value of which is 6-10, wherein the reaction temperature is 80-100 DEG C and the mass ratio of graphene oxide to the reducing agent acetone oxime, acetaldoxime or methyl ethyl ketoxime is 1: (0.2-5). The method is characterized in that the oximido having lower toxicity is used as the reducing agent and thegraphene is acquired by reducing the graphene oxide by using a chemical reduction method. The preparation method is simply and easily performed, the reaction process is easily controlled, no special requirement for equipment exists, the cost is low, the pollution is free, and the method is easily popularized and used.

The invention relates to a non-steroidal androgen receptor modulator compound containing 1, 3-diaryl-3-aromatic amine-1-acetoxime compound (I), or relative medical acceptable salt and a relative preparation method. The invention also relates to a drug compound of 1, 3-diaryl-3-aromatic amine-1-acetoxime compound (I) and relative medical acceptable salt. The1, 3-diaryl-3-aromatic amine-1-acetoxime compound (I) or relative medical acceptable salt has androgen receptor antagonistic activity, therefore, the compound can be used to prepare the non-steroidal drug for preventing or/treating prostatic hyperplasia, prostate cancer, hirsutism, serious androgen dependence alopecia and acne or the like.

The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of O-3-chloro-2-propenylhydroxylamine. The preparation method of the O-3-chloro-2-propenylhydroxylamine comprises the following steps: uniformly stirring hydroxylamine salt, water and acetone, adding a sodium hydroxide solution, reacting at room temperature for 1 to 2 hours, then adding 1,3-dichloropropene and a phase transfer catalyst, heating in water bath, controlling the temperature at 60 to 90 DEG C, reacting for 5 to 10 hours, standing still for stratification, separatingand collecting an oil phase, extracting the oil phase 2 to 3 times with an extractant, drying extract liquid with anhydrous sodium sulfate, and removing a solvent under reduced pressure to obtain theO-3-chloro-2-propenylhydroxylamine. According to the preparation method of the O-3-chloro-2-propenylhydroxylamine provided by the invention, acetone oxime is firstly prepared by taking the hydroxylamine salt and acetone as raw materials, and then 1,3-dichloropropene and the phase transfer catalyst are added for a reaction to prepare the O-3-chloro-2-propenylhydroxylamine; the O-3-chloro-2-propenylhydroxylamine prepared with the preparation method has the purity of 99% or more than 99% and the yield of 88% or more than 88%, and the method is suitable for industrial production.

The invention discloses a synthetic method of 2,3-dimethyl-2,3-dinitrobutane. The synthetic method comprises the following steps that 1, acetoxime, water, and catalyst modified titanium silicalite (TS)-1 are added into a reaction container at room temperature; 2, aqueous alkali and hydrogen peroxide are added dropwisely into the reaction system obtained by the previous step at a temperature of 60to 90 DEG C with stirring; the pH of the reaction system is kept in a range of 8 to 10; and a mol ratio of hydrogen peroxide and acetoxime is in a range of 1 to (3: 1); 3, after dropwiseaddition, themixture obtained from the step 2 undergoes a reaction at a temperature of 60 to 90 DEG C for 0 to 2 hours; 4, reaction products obtained from the step 3 is cooled to room temperature and then is subjected to a filtration or a centrifugation process thus modified TS-1 is separated from the cooled reaction product and mother liquor is obtained; the modified TS-1 is washed by acetone; washing liquidis collected; and the collected washing liquid is added into the mother liquor; and 5, the mother liquor containing the collected washing liquid is subjected to a distillation process at a temperature less than or equal to 80 DEG C so that acetone in the reaction system is removed; the mother liquor treated by the distillation process is cooled and filtrated; and filter residues are washed by water to form 2,3-dimethyl-2,3-dinitrobutane products. Raw materials adopted by the synthetic method have the advantages of good safety and low cost. 2,3-dimethyl-2,3-dinitrobutane synthesized by the synthetic method has the advantages of less impurities and high product quality.

The invention discloses preparation of substituted saturated hydrocarbon and particularly relates to a synthesizing method of 2-nitropropane. The 2-nitropropane is prepared by oxidizing isohydrazone. The synthesizing method includes the steps of S1, condensing acetone, water and ammonia in the presence of a catalyst to generate ketimine, wherein the mass ratio of the acetone to the water is 1:(1-5), and the use amount of the catalyst is 5-11% of the use amount of the acetone; S2, oxidizing the ketimine obtained in the step S1 to form the isohydrazone, wherein reaction system temperature is 30-60 DEG C and heat-preservation reaction time is 0.5-3 hours; S3, oxidizing the isohydrazone obtained in the step S2 to form the 2-nitropropane, wherein reaction system temperature is 50-80 DEG C and heat-preservation reaction time is 0.5-3 hours; rectifying obtained primary reaction liquid to obtain qualified 2-nitropropane products. The synthesizing method has the advantages that the acetone, the ammonia and the water are used as the initial raw materials, and the method is mild in catalytic oxidizing reaction condition, simple in process, convenient to operate, suitable for large-batch 2-nitropropane production, simple in post-processing and high in product purity and does not coproduce acetone oxime or acetone azine.

The invention discloses a modified zeolite functional material for fixing benzene degrading bacteria. Zeolite is modified by a mixed solution prepared from ammonium dihydrogen phosphate, tetrahydro-4H-pyran-4-one, 5-bromothiophen-2-formaldehyde, 2,5-dichloro-3-bromopyridine, tetrabromothiophene and 2-acetylene thiophene to obtain a substance B; the substance B is modified by a mixed solution prepared from 3-chloropyridazine, acetaldehyde phenylhydrazone, acetone oxime, guanidine nitrate and indole-6-carboxaldehyde to obtain a substance C; the substance C is modified by a mixed solution prepared from 3-formylthiophene, di-tert-amylbenzoquinone and 4-amino-3-hydroxy-1-naphthalene sulfonic acid to obtain a substance D; and the substance D is modified by a mixed solution prepared from propyl sulfate, 2-aminoanthraquinone and nitrourea to obtain a substance, namely the modified zeolite functional material for fixing the benzene degrading bacteria.

The invention provides a preparation method of ketoxime, which is characterized by comprising contact of ketone and oximation agent under oximation reaction conditions with solvents, oxidizing agents, surfactants and catalysts. The preparation method of the acetone oxime has the advantages that the reaction operation is simple, the process time is short and continuous production can be achieved. For example, by adopting the method, the acetone conversion rate, the hydrogen peroxide conversion rate and the acetone oxime selectivity can reach above 98 percent within 40 minutes. For comparison in Example 1, the acetone conversion rate, the hydrogen peroxide conversion rate and the acetone oxime selectivity can only reach about 96 percent within 600 minutes under the same condition except for surfactants. Therefore, the production efficiency can be greatly increased when the method is adopted.

The invention relates to a sterilizing algicide for circulating cooling water and a preparation method of the sterilizing algicide. The sterilizing algicide comprises the following components in parts by mass: 10-19 parts of chlorophenasic acid, 10-19 parts of parachlorophenol, 3-10 parts of dodecyl dimethyl benzyl ammonium chloride, 0.5-3 parts of dithiocyano-methane, 8-15 parts of sodium dodecyl benzene sulfonate, 1-5 parts of acetone oxime, 2-5 parts of methyl alcohol, 1-3 parts of diethyl ether, 4-8 parts of sodium hydroxide, and 19-37 parts of water. The sterilizing algicide has good sterilizing and algae removal effects, and has a long pesticide effect, the sterilizing rate reaches over 98%, and the pesticide effect time is more than 25 hours.

The invention discloses a method for reclaiming acetone oxime from carvone production wastewater. The method comprises the following steps: firstly, reclaiming of an extractant, namely collecting 120-150 DEG C/2mmHg after-cut under the condition of rectification during carvone production as the extractant, wherein the mass content of the carvone is less than 0.5 percent; secondly, extraction of the wastewater, namely mixing the wastewater containing the acetone oxime and the extractant according to the weight ratio of 3.4-3.8:1, raising the temperature to be between 40 and 50 DEG C, stirring for 30 to 45 minutes, cooling the mixture to the room temperature, performing standing and delamination, re-extracting a water phase until reaching the standards, introducing the water phase into a wastewater purification treatment system, and reclaiming the acetone oxime from an organic phase, wherein the mass content of the acetone oxime in the water phase is less than 1.5 percent; thirdly, rectification, namely performing vacuum rectification on the organic phase, and collecting 80-85 DEG C/300mmHg acetone oxime cut fractions; and fourthly, recrystallization, namely dissolving the acetone oxime cut fractions into water according to the mass ratio of 1.5:1, reducing the temperature to be between 3 and 5 DEG C for crystallization and centrifugal separation, recycling a mother liquor, drying solid under vacuum and obtaining the acetone oxime. The method has simple technique, is convenient to operate and easy in industrial implementation, and changes the prior mode of no products after environment-friendly investment, and has high economic efficiency and social efficiency.

The invention discloses a purification method of acetone oxime, and relates to the technical field of organic compound purification. The method comprises the steps that acetone, ammonia gas or ammonia water, hydrogen peroxide, a solvent and a catalyst make contact with one another, and an acetone ammoximation reaction is conducted to obtain an acetone oxime reaction solution, wherein the solvent is a mixture of water and an organic solvent; for the purification process, the acetone oxime reaction solution is filtered at first, a filtrate is subjected to rectification to remove the organic solvent, tower kettle water and oxime mixed liquid is extracted with an extraction agent to obtain extraction liquid, the extraction liquid is subjected to rectification, the extraction agent is rectified out, and then pure acetone oxime is rectified out, wherein the extraction agent is ethyl acetate or dichloromethane or trichloromethane or methylbenzene. The method has the advantages of being capable of obtaining the extraction agent easily, high in extraction rate, capable of separating the extraction agent easily, simple in process, low in energy consumption, mild in separation condition, high in product purity and the like.

The invention belongs to the field of chemical technology, and in particular relates to a synthetic method of azithromycin genotoxic impurities, wherein the impurity is acetone oxime-O-p-methyl sulfonic acid ester. The preparation method comprises the following main steps: firstly, preparing a compound with acetone and hydroxylamine through oximation, then conducting esterification reaction with the compound and p-toluenesulfonyl chloride, and finally refining the substance to obtain the acetone oxime-methyl sulfonic acid ester impurities with purity of higher than 99.5%. The high purity synthetic acetone oxime-methyl sulfonic acid ester serves as the impurity standard for azithromycin finished products testing, facilitates the enhancement of positioning and qualitative identification of the genotoxic impurities in the testing of the azithromycin finished products, and improves the quality control of the azithromycin crude drugs.

The invention relates to a preparation method for acetoxime. The preparation method comprises the following steps: a) preparation of a reaction system: adding ketoxime and acetone in a molar ratio of1.0: (5.0-35.0) into a reactor, then adding an acid catalyst and a solvent, and carrying out uniform mixing in the reactor under stirring to form the reaction system which has a pH value of 1 to 5; b)a synthetic reaction of acetoxime: heating the reaction system obtained in step a) and carrying out the reaction for 5 to 10 h with reaction temperature controlled to be 5 to 100 DEG C and a pressurecontrolled to be 0 to 2 atm; and c) purification of acetoxime: purifying a product obtained in step b) so as to obtain acetoxime. The method of the invention has the advantages of high reaction conversion rate, high acetoxime selectivity, simple reaction process, environmental friendliness, reduced environmental pollution and easy industrial production.

The invention discloses a preservative for marine pipe pigging pressure testing and sealing and a production method thereof. The preservative comprises 8-35 weight parts of polyhydric alcohol phosphate ester, 25-75 weight parts of clear water, 5-25 weight parts of inorganic compounds, 1-12 weight parts of polymers, 0.5-10 weight parts of sterilization components and 2-10 weight parts of deoxidation components, which are fully stirred and dissolved in a synthesis kettle under normal temperature and are uniformly dissolved for split charging to form a finished product. Inorganic compounds are one or mixtures of more than two of zinc gluconate, sodium gluconate, sodium tripolyphosphate and sodium hexametaphosphate; the polymers are one or mixtures of more than two of polyaspartic acid, polyepoxysuccinic acid, hydrolytic polymaleic anhydride, polyacrylic acid and copolymers; the sterilization components are one or mixtures of more than two of dodecyl dimethyl benzyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl benzyl dimethyl ammonium chloride and glutaraldehyde; and the deoxidation components are one or mixtures of more than two of methyl ethyl ketoxime, acetone oxime and sodium sulfite.

The invention relates to the technical field of acetone oxime production processes, in particular to a preparation method of acetone oxime. The preparation method of acetone oxime comprises the following steps: 1) dissolving acetone in an organic solvent to prepare an acetone solution and then adding a TS-1 molecular sieve catalyst and ammonia water into the acetone solution to be mixed to obtaina prereaction liquid; and 2) heating the prereaction liquid to 40-80 DEG C, and adding a hydrogen peroxide solution to react for 3-10 hours under the condition that the temperature is 40-80 DEG C andthe pressure is 0-1.0MPa, then carrying out filtration and rectification, extracting the solution with an extraction agent to obtain an extraction solution, and rectifying the extraction solution to obtain acetone oxime. The preparation method is simple in production process. Acetone is dissolved by isopropanol or cyclohexane, so that the solubility is good and the conversion ratio of acetone is improved. Isopropanol or cyclohexane is easily separated from a mixture of acetone oxime separately in the later period. The extraction agent is used for acetone oxime, so that the extraction rate is high, and in the whole process course, environmental pollution caused by a conventional process is avoided.

The invention provides a synthesis method of 2-hydroxy-5-nonylpropiophenone and an application of the 2-hydroxy-5-nonylpropiophenone in a copper extraction agent. The synthesis method of the 2-hydroxy-5-nonylpropiophenone comprises the following steps: esterification reaction, rearrangement reaction, hydrolysis reaction and distillation purification. The method has the beneficial effects that thebrand-new synthetic route of the 2-hydroxy-5-nonylpropiophenone has the advantages that TiCl4 is adopted as a Lewis acid catalyst to carry out the rearrangement reaction of 4-nonylphenol ester, side reactions are fewer, and higher conversion rate and product purity can be obtained; according to the application of the 2-hydroxy-5-nonylpropiophenone oxime in the efficient copper extraction agent, the efficient copper extraction agent can be obtained after the 2-hydroxy-5-nonylpropiophenone oxime and the 2-hydroxy-5-nonylbenzaldoxime are compounded according to the ratio of 1:1, the product performance exceeds that of a Lix984N product, and the use stability and the unit consumption are lower.

The invention discloses a pickling compound corrosion inhibitor for thermal equipment and a preparation method thereof. The compound corrosion inhibitor is prepared from a tea seed shell ethanol extract, quaternary ammonium bis-imidazoline, acetone oxime, sodium alkyl benzene sulfonate, and an EDTA disodium salt. The compound corrosion inhibitor has a good corrosion inhibition effect in the temperature range of a hydrochloric acid pickling technology for the thermal equipment, and the corrosion inhibition rate can reach 96%.

The invention relates to a composite water treatment agent for a thickened oil thermal recovery boiler and a preparation method thereof. The composite water treatment agent for the thickened oil thermal recovery boiler comprises the following components according to weight percentage: 10%-25% of DTPMP (diethylene triamine penta methylene phosphonic acid), 10%-15% of sodium polyacrylate, 10%-12% of maleic acid acrylic copolymer, 5%-10% of 2-hydroxyphosphonoacetic acid, 5%-10% of acetone oxime, and the balance of water. The preparation method of the composite water treatment agent for the thickened oil thermal recovery boiler comprises the following steps of adding water into a reaction kettle, then stirring and simultaneously adding the DTPMP, the sodium polyacrylate, the maleic acid acrylic copolymer, the 2-hydroxyphosphonoacetic acid and the acetone oxime, then reacting for 30-40 minutes, and obtaining the composite water treatment agent for the thickened oil thermal recovery boiler. According to the composite water treatment agent for the thickened oil thermal recovery boiler, problems of corrosion and scaling of a steam drive thermal recovery are solved, and the requirement on production on site is met.

The invention relates to an organic synthesis intermediate acetone oxime synthesis method, which mainly comprises: dissolving 0.5 mol hydroxylamine phosphate in 20 L of a potassium chloride solution,slowly adding 0.6-0.8 mol of an acetone solution, controlling the solution temperature at 35-39 DEG C, standing for 90-110 min after the adding, reducing the solution temperature to 31-34 DEG C, adding 0.9 mol of a potassium bicarbonate solution, adjusting the pH value of the solution to 8.5-9, controlling the solution temperature at 41-45 DEG C, layering after cooling, extracting the obtained oillayer, carrying out pressure reducing distillation, collecting the distillate at a temperature of 90-95 DEG C, washing with a cyclohexane solution, washing with an isopropanol solution, dehydrating with a dehydrating agent, and carrying out cooling crystallization to obtain the finished product acetone oxime.