1101results about "Oximes preparation" patented technology

A process for producing an oxime is provided, wherein the process comprises the step of reacting a ketone, hydrogen peroxide and ammonia in the presence of a crystalline titanosilicate having MWW structure under the condition that the ammonia concentration in the liquid portion of the reaction mixture is about 1% by weight or more. By the process, an ammoximation reaction of the ketone can be carried out with a high conversion of the ketone and a high selectivity to the oxime corresponding to the ketone, thereby producing the oxime with a high yield.

The invention discloses a titanium silicalite TS-1 catalyst preparation method. Cheap inorganic Titanium silicalite is used as raw material, low quantity of tetrapropylammonium hydroxide or tetrapropylammonium bromide is adopted as template agent, and inorganic alkali such as ammonia water is used as alkali source so that the raw materials for preparation have low price and the production cost isgreatly reduced. The precursor preparation process is simple and easy to control, seed crystal is added to reduce the crystallization time and the repeatability is good. As secondary crystallization is adopted, the non-framework titanium is further reduced, and the acid site of the molecular sieve is reduced, the grain size is controllable within certain range, the molecular sieve channel becomessmoother to facilitate direct membrane separation of micrometer crystalline grains, and the obtained Titanium silicalite TS-1 catalyst has large grains, high activity, stable catalytic performance and broad industrial application prospect.

The present invention relates to methods of using amidoxime compositions for cleaning polishing pads, particularly after chemical mechanical planarization or polishing is provided. A polishing pad is cleaned of Cu CMP by-products, subsequent to or during planarizing a wafer, to reduce pad-glazing by applying to the polishing pad surface a composition comprising an aqueous amidoxime compound solution in water.

The invention relates to a one-step molding method of a titanium silicalite molecular sieve. The method comprises the following steps of crystallizing the titanium silicalite molecular sieve subjected to hydro-thermal synthesis; directly adding a matrix substance, a binder, a peptizing agent and a pore-enlarging agent without separating, washing and calcining; pulping; performing spray forming; and calcining the formed microspheres to remove a template agent to obtain large formed titanium silicalite molecular sieve particles which can be applied to ammoximation of cyclohexanone and epoxidation of olefin.

The invention discloses a method for preparing and modifying a titanium silicalite molecular sieve catalyst and application of the titanium silicalite molecular sieve catalyst in ketone oximation. The method comprises the following steps: (1) adding seed crystal into a titanium source, a silicon source, a first template agent, a first alkali source, water and additive which serve as raw materials to prepare a titanium silicalite molecular sieve A by adopting a hydrothermal synthesis method; (2) modifying the titanium silicalite molecular sieve A by using an acidic mixed solution to obtain a molecular sieve B; (3) modifying the molecular sieve B by using a second template agent and a second alkali source or mixed liquid of the second template agent and ammonium salt to obtain a molecular sieve C. The titanium silicalite molecular sieve catalyst prepared by the method can be applied to ketone oximation. According to the method, the synthesis cost of the titanium silicalite molecular sieve can be reduced, non-framework titanium in the molecular sieve can be effectively removed, and the catalyzing performance of the molecular sieve synthesized by a low-price system in a ketone oximation reaction can be remarkably improved.

The invention provides apple-shaped hollow molecular sieve microspheres and a preparation method and application thereof. The preparation method includes: homogenizing a molecular sieve, a binder, a pore forming agent and water, and mixing colloidal grout with a surfactant for emulsifying to form a spherical emulsion under action of surface tension of the surfactant, wherein at the moment of sprayforming, the pore forming agent pyrolyzes at a point inside the spherical emulsion in a centralized manner to form a cavity from the surface to the inside of the microsphere emulsion, and in the process of spray forming, the cavity contracts to a certain degree to form macropores on the surface to be communicated with a hollow structure inside; combining with the subsequent calcining process to obtain large-grained hollow molecular sieve microspheres. Results of embodiments show that by the preparation method, hollow microspheres with macropores in the surface can be prepared, particle size distribution is 50-300um; hollow structure diameter reaches 10-150um, a macropore of 5-30um is formed in the surface of each molecular sieve microsphere, thickness of a shell layer reaches 10-80um, andthe shell layer is provided with mesopores of 70-200nm.

The invention relates to a titanium-silicon molecular sieve TS-1 catalyst for catalyzing ketone oximation reaction. In order to solve the problems of small particles, difficult separation and reutilization, high synthesis cost, strict and complex requirements in the process of gluing, poor repeatability and stability and the like in the prior art, the invention provides a new titanium-silicon molecular sieve TS-1 catalyst for the catalyzing ketone oximation reaction, which is prepared from the following steps: mixing the titanium-silicon molecular sieve TS-1 with one or more solutions of organic amine, ammonium salt, ammonia water and urea, carrying out crystallization again under the self-generating hydro-thermal pressure, and filtering, washing, drying and roasting to obtain the product. The prepared titanium-silicon molecular sieve TS-1 catalyst has large particles and easy separation and recovery after reaction, can improve the reutilization ratio, is especially suitable for ketone oximation reaction using hydrogen peroxide as an oxidizing agent, and can not produce byproducts, thereby protecting the environment and being beneficial to industrial application.

A cyclohexanone oxime is produced in a method comprising the step of reacting a cyclohexanone with a hydrogen peroxide and an ammonia in the presence of a titanium silicate and a silicon compound other than the titanium silicate. In the method, the reaction is conducted with suppressing the inactivation of the titanium silicate as a catalyst, to produce the cyclohexanone oxime with a high yield.

The present invention relates to a process for working up an ammoximation reaction mixture, by separating a catalyst from the reaction mixture, removing the ketone oxime product, discharging the water of the reaction, and recirculating a solvent, where the ketone oxime formed is removed in a liquid phase with at least one liquid-liquid extraction in a ternary solvent system.

The invention discloses a metal fiber / molecular sieve composite material and its preparation method and application. The composite material is formed by an integral sintered metal fibrous matrix and an MFI type molecular sieve layer uniformly coated on the outer surface of the each metal fiber of the matrix, and is prepared by using a sol precoated layer and a hydrothermal crystallization growth method. The metal fiber / molecular sieve composite material possesses a three dimensional opening style continuous network structure, the void ratio can reach 68%-85%, the permeability is high, the thermal conductivity is good and the structure is stable, the composite material possesses excellent catalytic effects of catalytic reaction of methanol prepared by olefin and catalytic reaction of a cyclohexanone peroxide ammoximation fixed bed, and the invention has the advantages of simple preparation method and controllable structure, is suitable for industrial production, and has the practical value and application prospect.

The invention discloses a fluorine-containing titanium-silicon molecular sieve with a MWW (Manual Wire Wrap) structure and a preparation method and an application thereof. In the molecular sieve, a fluorine atom is connected with a framework silicon atom in the form of a chemical bond, an XRD (X-Ray Diffraction) spectrogram contains a characteristic spectral line of the molecular sieve with the MWW structure, and characteristic peaks of -150+ / -5ppm and -143+ / -5ppm appear in a 19FMAS-NMR (19 File Management Assistant For Server-Nuclear Magnetic Resonance) spectrogram; the preparation method comprises the following steps of: synthesizing a boron-containing parent body, post-treating, baking and the like; and the molecular sieve serving as a catalyst is applied to catalytic oxidation reactions of compounds containing carbon-carbon double bonds and at least one other functional group as well as reactions for catalytically synthesizing oxime. The molecular sieve has a complete crystalline state structure; according to the electronic effect of framework fluorine, the molecular sieve and higher catalytic oxidation capability; a preparation process is simple, and is easy for industrial production; synthesis of corresponding epoxides or catalytic synthesis of oxime from compounds containing carbon-carbon double bonds and at least one other functional group can be catalyzed at higher activity and high selectivity; and a reaction process is environmentally-friendly.

Certain known and novel pyruvate derivatives are particularly active in restoring or preserving metabolic integrity in oxidatively competent cells that have been subjected to oxygen deprivation. These pyruvate-derived compounds include, but are not limited to oximes, amides, pyruvate analogues, modified pyruvate analogues, esters of pyruvate (e.g., polyol-pyruvate esters, pyruvate thioesters, glycerol-pyruvate esters and dihydroxyacetone-pyruvate esters). Such pyruvate derivatives (including single tautomers, single stereoisomers and mixtures of tautomers and / or stereoisomers, and the pharmaceutically acceptable salts thereof) are useful in the manufacture of pharmaceutical compositions for treating a number of conditions characterized by oxidative stress.

The invention relates to an ammoximation method of ketone or aldehyde, which comprises the step of making ketone or aldehyde, ammonia and peroxide take the ammoximation reaction in a reaction vessel in the existence of titanium silicon catalysts and reaction solvents. The invention is characterized in that in the method, the reaction pulp carries out the multi-stage liquid-solid separation through a hydraulic cyclone and an inorganic membrane or a metal sintering pipe, and the separated titanium silicon catalysts are sent back to the reaction vessel for recycled use. The method improves the solid-liquid separation efficiency, prolongs the regeneration period of separation assemblies, improves the permeation flux of separation components, and lowers the energy consumption and the investment of a solid-liquid separation system.

The invention relates to a nitrocyclohexane hydrogenation catalyst and a preparation method thereof, and relates to a method for nitrocyclohexane hydrogenation by using the catalyst. Carbon nano tubes are used as a carrier in the catalyst and carry the following components: at least one VIII family metal and at least one alkali metal in the element periodic table. The catalyst can be used for preparing cyclohexane oxime by nitrocyclohexane hydrogenation; and according to the method, the preparation flow is short, the yield is high, comprehensive cost is low, resources are saved and no waste slag, waste gas or waste liquid is discharged; and the method is a pollution-free production process.

The invention relates to a lamellar catalyst containing mesoporous titanium-silicate molecular sieves and a preparation method and application of the stratiform catalyst. The stratiform catalyst is provided with a 12-membered ring hole and sine reticulation hole system of an MWW high-silicon molecular sieve, wherein the interlayer is provided with a 2-10 nm mesoporous structure, 4-coordinated titanium or 4-coordinated and 6-coordinated titanium. The preparation method comprises the following steps: an MWW high-silicon molecular sieve containing a template agent serves as a precursor for swelling, then filtering, washing and drying are carried out, pillaring, filtering and drying are performed, then hydrolysis reaction is realized to form an inorganic wall and a mesoporous structure in the interlayer of the MWW high-silicon molecular sieve, re-filtering, re-washing and re-drying are carried out, and high-temperature calcination is carried out to obtain titanium-containing MCM-36 of a microporous-mesoporous composite structure. According to the invention, as a new silicone source and titanium source hybrid pillaring agent is used for pillaring to prepare the titanium-containing mesoporous pure titanium silicate molecular sieve, Bronsted acid site of boron or aluminium in the molecular sieve precursor is eliminated.

A process is described for the preparation of substantially pure fluvoxamine maleate, an important antidepressant drug of the formula I, for use as an active pharmaceutical ingredient (API), from the corresponding oxime viz 5-methoxy-4'-trifluoromethylvalerophenone oxime of formula II.

The present invention relates a method for preparation of ketoxime compound, comprising: feeding a ketone compound, hydrogen peroxide, water, and ammonia into a reactor for contact reaction under the conditions of oximation reaction of ketone and ammonia, in the presence of a titanium-silicon molecular sieve catalyst, wherein, the molar ratio of the hydrogen peroxide to the ketone compound is 0.1 or more and less than 1. The present invention also relates to method for preparation of alkoxy-amine hydrochloride, comprising the following steps: preparing ketoxime compound by using the method for preparation of ketoxime compound described above, preparing ketoxime ether compound from the ketoxime compound, and then feeding the ketoxime ether compound and hydrochloric acid solution respectively into a rectification tower continuously for catalytic distillation, and separating alkoxy-amine hydrochloride from the liquid of the tower bottom of the rectification tower. In the method for preparation of ketoxime compound provided in the present invention, the titanium-silicon molecular sieve catalyst has a long useful life; using the method for preparation of alkoxy-amine hydrochloride provided in the present invention, the target product can be obtained at high purity and high yield.

The invention relates to a method for preparing strobilurin fungicide. The method comprises the following steps: (1) mixing the compound in formula (II) with the compound in formula (III) for reaction for 5 to 10 h at the temperature of 90 to 120 DEG C to obtain the compound in formula (IV), wherein the compound in formula (III) is acetal of formamides compound, R1, R2 and R3 are substituted alkyl or aryl; and (2) hydrolyzing the compound in formula (IV) under an acidic condition, and then stirring the hydrolyzed product at the room temperature for 2 to 4 h under the condition of alkali, methylating reagent and phase transfer catalyst to obtain the product, wherein X is 6-(2'-cyanophenoxyl) pyrimidine-4-oxy or 6-trifluoromethylpyridine-2-oxymethyl; 6-(2'-cyanophenoxyl) pyrimidine-4-oxy or 6-trifluoromethylpyridine-2-oxymethyl;[2-[[[[4-(4-chlorophenyl)-but-3-en-2-yl]imido]oxy]methyl]phenyl]; and 2-(2-((3-butyl-4-methyl-coumarin-7-yloxy)metyl)phenyl). The total yield of the method reaches above 85%.

The preparation method of the fungicide intermediate (E)-2-(2'-chloromethyl)-2-methicillin imino acetic methyl ester is: 1) the phenyl phthalate and the thionyl dihalide react with the influence of a catalyst; the catalyst is the Louis acid and phosphonic derivative; 2) the product of the first step and the alkali metal cyanide react with the influence of the organic solvent and phase transfer catalyst; the organic solvent is selected from the non-polar aromatic solvent or the halogen hydrocarbon; the phase transfer catalyst is selected from the halide of the four-level nitride or the ammonium salt; the alkali metal cyanide is selected from the sodium cyanide and potassium cyanide; 3) the products of the second step and the methanol react under the condition with the organic solvent and the chlorinated hydrogen; 4) the products of the third step and the methicillin amine hydrochloride under the condition with the organic solvent; thus, the target product can be got. The energy consumption and production risk of the present invention are obviously lowered; the relative collection rate is high; the safety in the production process is improved; and the present invention has no drawbacks such as the obstruction.

The invention discloses a 1,5-disubstituted aryl-1,4-pentadiene-3-ketoxime ether compound (I) and a preparation method thereof and insecticidal activity application. In the formula, Ar is aryl and can be substituted by one or more groups, and R1O can be in o, m and p positions. R1 and R2 are respectively C1-6 alkyl, C2-6 chain alkenyl or C2-6 chain alkynyl, benzyl, acyl and heterocyclic ring radical and can be substituted by one or more groups, wherein n is 0-3. In the invention, a series of novel curcumin derivatives 1,5-disubstituted aryl-1,4-pentadiene-3-ketoxime ether prepared by the oxime ether structure based on the structure of curcumin derivative 1,5-disubstituted aryl-1,4-pentadiene-3-ketone is prepared and the compounds and preparations have the function of preventing and treating crop pests, in particular a highly preventing and treating effect for plutella xylostella, nilaparvata lugens, snout moth's larva, sogatella furcifera, cnaphalocrocis medinalis, cabbage caterpillar, beet armyworm and aphid.

Certain known and novel pyruvate derivatives are particularly active in restoring or preserving metabolic integrity in oxidatively competent cells that have been subjected to oxygen deprivation. These pyruvate-derived compounds include, but are not limited to oximes, amides, pyruvate analogues, modified pyruvate analogues, esters of pyruvate (e.g., polyol-pyruvate esters, pyruvate thioesters, glycerol-pyruvate esters and dihydroxyacetone-pyruvate esters). Such pyruvate derivatives (including single tautomers, single stereoisomers and mixtures of tautomers and / or stereoisomers, and the pharmaceutically acceptable salts thereof) are useful in the manufacture of pharmaceutical compositions for treating a number of conditions characterized by oxidative stress.

The invention discloses an ammoximation reaction and separation coupling process which comprises the following steps: continuously adding reaction raw materials and a solvent in different groups outside a reaction kettle into a pipeline reactor for reaction, mixing the components in a mixer, and subsequently feeding the mixture into the reaction kettle for sufficient reaction, wherein the upper part of the reaction kettle is a reaction zone, and the lower part of the reaction kettle is a filtration separation zone; separating a reaction product, namely, cyclohexanone-oxime from a catalyst in the filtration separation zone, feeding the separated cyclohexanone-oxime into a later process, and circulating the catalyst back to the reaction kettle for continuous reaction through equipment such as the pipeline reactor outside the reaction kettle. Backwashing is performed once every 10-300 seconds, so that the continuity of reaction separation is ensured. As the raw materials sufficiently contact the catalyst, the reaction is complete, and the conversion rate of cyclohexanone can be 99.9-100%. The whole set of reaction separation devices is reasonable in arrangement and stable in reaction.

The liquid phase cyclohexanone-oxime producing process with reaction system comprising cyclohexanone, ammonia and hydrogen peroxide and Ti-MWW molecular sieve as catalyst belongs to the field of organic chemical synthesis. Reactants cyclohexanone, ammonia and hydrogen peroxide are added successively into the reaction system with Ti-MWW molecular sieve as catalyst and solvent through stirring, and heated through heating to obtain the product cyclohexanone-oxime. The present invention has the following obvious advantages: excellent catalytic activity of the Ti-MWW molecular sieve as catalyst, high cyclohexanone converting rate, high cyclohexanone-oxime selectivity, high utilization of hydrogen peroxide, simple post-treatment and environment friendship.

The invention relates to a synthesis method of oxime, which belongs to the technical field of organic synthesis. At present, the oxime is synthesized mainly by utilizing the reaction between hydroxylamine salt and ketone and aldehyde, and defects are the high dosage of hydroxylamine salt and the production of a large amount of byproduct (inorganic salt). The technique is an environment-friendly process. In the technical scheme of the invention, reactant (ketone or aldehyde), ammonia and hydrogen peroxide are ordinally added into the reaction system of catalyst containing Ti-MWW-F molecular sieve and solvent, and after stiring, temperature raising and reaction are finished, an oxime product is produced by filtering, distillation, liquor filtering and separation. The invention has the advantages of high conversion rate of ketone or aldehyde, high utilization rate of hydrogen peroxide, usage of water as resolvent, simple post-processing procedure and environment-friendly reaction procedure.

The invention relates to a synthesized multilevel structure ZSM-5 zeolite molecular sieve with intracrystalline meso pores and intercrystalline meso pores, as well as a synthetic method and an application thereof. Except micropores of the zeolite structure, the multilevel structure ZSM-5 zeolite molecular sieve comprises the intracrystalline mesoporous and intercrystalline mesoporous structure, wherein primary nanometer crystal grain size is 40-500nm, and secondary accumulated particle size is 500nm-5[mu]m. The structure greatly improves diffusion performance and the catalyst activity of the molecular sieve, reduces possibility of generation of side reaction and carbon deposit, improves carbon accommodating capability of the molecular sieve catalyst, and prolongs life of the catalyst.

The invention discloses a fluorine-containing oxime ester photoinitiator as shown in a formula (I) which is described in the specification. The fluorine-containing oxime ester photoinitiator has excellent film forming ability when applied to photocured compositions, is good in surface curing effect and not prone to yellowing, and presents good usage effect when compounded with other conventional photoinitiators.

The invention discloses a method for catalyzing ammoximation of cyclohexanone. The method comprises the steps as follows: subjecting cyclohexanone, ammonia, oxygen, hydrogen, diluent gas and a solvent to coming in contact with a catalyst. The mole ratio of cyclohexanone, to ammonia, oxygen, hydrogen and diluent gas is 1:(0.1-10.0):(0.1-10.0):(0.1-10.0):(0-100). The mass ratio of the solvent to the catalyst is (20-1000):1. The catalyst is a microporous titanium-silicon material or a compound containing the microporous titanium-silicon material. The composition of the microporous titanium-silicon material is expressed as xTiO2*100SiO2*yEmOn*zE in an oxide form, wherein x ranges from 0.001 to 50.0; the sum of y plus z ranges from 0.005 to 20.0; the ratio of y to z is smaller than 1; E is one or more metal noble metals selected from Ru, Rh, Pd, Re, Os, Ir, P and Au; m and n are numbers required for meeting the oxidation state of the E; and material grains are partially or totally hollow-structured. The method has the advantages of high selectivity of cyclohexanone oxime, high product activity and stability, environment friendliness and low cost.

Certain known and novel pyruvate derivatives are particularly active in restoring or preserving metabolic integrity in oxidatively competent cells that have been subjected to oxygen deprivation. These pyruvate-derived compounds include, but are not limited to oximes, amides, pyruvate analogues, modified pyruvate analogues, esters of pyruvate (e.g., polyol-pyruvate esters, pyruvate thioesters, glycerol-pyruvate esters and dihydroxyacetone-pyruvate esters). Such pyruvate derivatives (including single tautomers, single stereoisomers and mixtures of tautomers and / or stereoisomers, and the pharmaceutically acceptable salts thereof) are useful in the manufacture of pharmaceutical compositions for treating a number of conditions characterized by oxidative stress.