562 results about "Dimethyldichlorosilane" patented technology

The invention relates to a method preparing a copper catalyzer used for dimethyldichlorosilance synthetic reaction through a liquid phase ball-milling partial reduction method. The method includes the steps of taking copper oxide as raw material, adding solvent media containing reducing substances, enabling copper oxide particles to become small and achieve partial reduction through mechanical ball-milling, obtaining the copper-based catalyzer containing the ternary components of copper, cuprous oxide, copper oxide after suction filtration, drying and smashing, and obtaining the ternary copper catalyzer with adjustable components and controllable particles through adjusting the parameters of reducing agent types, concentration and ball-milling conditions. In catalytic reaction of organosilicone monomer synthesis, the catalyzer is high in catalytic activity and selectivity and helpful for improving the processing ability of an existing organosilicone monomer device, reduces production cost, and improves the yield of target products. The method preparing the catalyzer through the liquid phase ball-milling partial reduction method is simple in process, mild in condition and convenient to operate, and brings convenience to achieve large scale production.

The invention relates to the organosilicon monomer synthesis field, and particularly relates to a Cu-Cu2O-CuO ternary copper-based solid solution catalyst and its preparation method. The method comprises the following steps of: 1) taking a mixture composed of 0.5-40wt% of metal copper powder and 20-80wt% of copper oxide as a raw material, conducting heat treatment at a temperature of 600-1000DEG C for 0.5-12h under inert gas protection, and then carrying out ageing at a temperature of 300-600DEG C for 1-15h so as to obtain a ternary copper-based solid solution; and 2) subjecting the ternary copper-based solid solution from step 1) to shattering and milling to obtain the Cu-Cu2O-CuO ternary copper-based solid solution catalyst. The copper-based solid solution catalyst prepared in the invention shows high dimethyldichlorosilane selectivity and silicon power raw material conversion rate.

A process for preparing dimethyl dichlorosilane from the high-boiling-point residue generated in synthesizing methyl chlorosilane includes filling catalyst in gas preheater, passing chloromethane (or hydrogen chloride) gas through it, carrying catalyst into reactor while introducing said residue to it, and separating dimethyl dichlorosilane from the cooled substance at tower top.

The invention relates to a flower-shaped copper oxide catalyst and a preparation method and application thereof to the direct synthesis of an organic silicon monomer. The preparation method of the flower-shaped copper oxide catalyst comprises the following steps: (1) adding copper salt to ethanol or mixed solvent of ethanol and water to form solution; and (2) stirring and adding ammonia, strong alkali and nitrate to the solution in sequence to obtain a homogeneous solution, transferring the homogeneous solution to a reactor to carry out the thermal reaction of a solvent, and controlling the amount of the product of reaction, the reaction temperature and the reaction time to obtain the lower-shaped copper oxide catalyst. The preparation process of the flower-shaped copper oxide catalyst has simple experiment procedures and low cost, is convenient to operate, is environment-friendly and can be produced on a large scale. The prepared flower-shaped copper oxide powder can be used as the catalyst to the field of the direct synthesis of the organic silicon monomer, and particularly, the flower-shaped copper oxide powder is highly selective for the dimethyldichlorosilane monomer.

The invention discloses a method for hydrolyzing dimethyl dichlorosilane with concentrated acid. The method comprises the following steps: mixing the dimethyl dichlorosilane with hydrochloric acid to carry out hydrolytic reaction; mixing the obtained reaction liquid with a solvent; finally, performing separating operation on the obtained mixed solution to obtain hydrolysis product and hydrogen chloride gas. Through the adoption of the method, the content of cyclic polysiloxane in hydrolysate obtained from the dimethyl dichlorosilane through the concentrated acid hydrolyzing method is effectively increased; the design is reasonable, hydrolysate with low chlorine ion content can be obtained in no need of multi-stage phase separation procedures, and the hydrochloric acid and solvent obtained after separation can be recycled, so that the resource use ratio is improved, and the production cost is saved.

The invention discloses a methyl chlorosilane parallel double-effect distillation method. The method comprises the following steps: the synthetic product of methyl chlorosilane passes through a heavy component removing tower for removing heavy components and a light component removing tower for removing light components, the mixture of dimethyldichlorosilane and methyltrichlorosilane can be obtained, the mixture is divided to two parts to be sent to two parallel distillation systems of high-pressure refining and low-pressure refining, wherein one part enters in a high-pressure refining distillation system composed of a methyltrichlorosilane high-pressure tower and a dimethyldichlorosilane high-pressure tower, the other part enters in a low-pressure refining distillation system composed of a methyltrichlorosilane low-pressure tower and a dimethyldichlorosilane low-pressure tower, and the overhead gas phases of the methyltrichlorosilane high-pressure tower and the dimethyldichlorosilane high-pressure tower are separately used as the heat sources of the tower bottom reboilers of the methyltrichlorosilane low-pressure tower and the dimethyldichlorosilane low-pressure tower. By adopting two parallel processing lines, energy consumption can be reduced by more than 20%- 40% and the amount of circulating water can be saved.

A surface treated particle comprising a plurality of inorganic, metallic, semi-metallic, and/or metallic oxide particles and a star-graft copolymer with looped and/or linear polymeric structure on a star-graft copolymer, obtainable by a heterogeneous polymerization reaction in the particle surface proximity, encapsulating at least a portion of said particles and a method for making the same. The surface treatment comprises: Si (w, x, y, z), where: w, x, y, and z are mole percent tetrafunctional, trifunctional, difunctional, and monofunctional monomeric units, respectively; w, x, y, and z are about 0-50, 0-50, 5-99, and 0-5, respectively; w is tetraethylorthosilicate; x is selected from the group consisting of γ-glycidoxypropyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, methyltrimethoxysilane, n-propyltrimethoxysilane, isobutyltrimethoxysilane, n-hexyltrimethoxysilane, n-octyltrimethoxysilane, n-octadecyltrimethoxysilane, phenyltrimethoxysilane, 3-(trimethoxysilyl)propylsuccinic anhydride, heptadecafluorotrimethoxysilane, 3-isocyanatopropyltrimethoxysilane, 2-(diphenylphosphino)ethyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane, n-(trimethoxysilylpropyl)EDTA, pentafluorophenylpropyltrimethoxysilane, trifluoropropyltrimethoxysilane, and the triethoxy-containing counterparts of these monomers; y is selected from the group consisting of dicyclohexyldimethoxysilane, diethyldiethoxysilane, dimethyldichlorosilane, dimethyldiethoxysilane, dimethyldimethoxysilane, diphenyldiethoxysilane, diphenyldimethoxysilane, di-n-hexyldichlorosilane, n-hexylmethyldichlorosilane, methyldodecyldiethoxysilane, n-octylmethyldimethoxysilane, and the diethoxy-containing counterparts of these monomers; and z is selected form the group consisting of n-octadecyldimethylmethoxysilane, triethylsilanol, trimethylethoxysilane, trimethylmethoxysilane, and the ethoxy-containing counterparts of these monomers. Product(s) per se, defined as surface treated ZnO and/or TiO₂, and the use of the product(s) per se in personal care formulations are excluded.

The invention relates to a method for generating dimethyldichlorosilance by utilizing disproportionation reaction, which belongs to the technical field of the comprehensive utilization of three wastes in the production process of methyl chlorosilane. The invention is characterized by comprising the following steps: generating the dimethyldichlorosilance by using methyl trichlorosilane and trimethylchlorosilane as organic silicon monomers, or a high boiling object and a low boiling object as the organic silicon monomers, or the mixture of the methyl trichlorosilane, the trimethylchlorosilane, the high boiling object and the low boiling object as the organic silicon monomers as raw materials under the single or combined catalytic action of aluminum powder and anhydrous aluminum trichloride as catalysts. In the invention, reaction is generated in a high-pressure agitating kettle at the temperature of 180 to 350 DEG C, and in the reaction, the reaction pressure is controlled by the reaction temperature, i.e. the higher the reaction temperature is, the higher the reaction pressure is, and the maximum conversion rate of a target product can reach more than 70 percent. The invention improves the resource utilization level of methyl organic silicon monomer production, the dimethyldichlorosilance is produced in lower cost, and the invention has simple and easy operation and is suitable for large-scale popularization and utilization.

The invention relates to the field of organic chemistry, in particular to a method for processing and recovering contacts in the synthetic process of methyl chlorosilane, which is characterized by comprising the following steps: adding an intermediate storage tank of the contacts in the process of synthesizing the methyl chlorosilane; when the selectivity of a target product is reduced to between 70 and 90 percent, transferring the contacts in the reaction system to the intermediate storage tank; re-adding new contacts to react in a fluidized bed, and mixing the transferred contacts with fresh silicon powder; and returning the mixture to the fluidized bed to use the mixture as new contacts to be added to the reaction. In the invention, the production method is used to not only ensure the stability of the selectivity for dimethyl dichlorosilane in the synthetic process of the methyl chlorosilane, and prolong the synthetic cycle of organochlorosilane simultaneously. The effective production time of the production device can be up to over 50 days.

The invention discloses a preparation method for thermoset high temperature resistant methyl phenyl silicone resin, which relates to the technical field of resin preparation and comprises the steps of utilizing toluene or dimethylbenzene or mixed solution of the toluene and dimethylbenzene to serve as a solvent, utilizing methyl trichlorosilane, dichlorodimethylsilane and methylphenyldichloros as monomer raw materials, dropping mixed solution of acetone and water into the raw materials under the condition of ice-water bath, ensuring that the dropping is finished within 3-5 hours, obtaining a prepolymer of the methyl phenyl silicone resin, performing condensation and curing on the obtained prepolymer above 150 DEG C after pressure of the prepolymer is reduced and the prepolyme is concentrated, the adopted condensation catalyst is caprylate or naphthenate, particularly is stannous octoate, zinc isoocatanoate, cobalt naphthenate and dibutyltin dilaurate. The resin is semi-transparent hard or elastic solid, can not be dissolved or fused, and can be resistant to high temperature above 200 DEG C, and can be used as silicon rubber or a plastic filler.

The invention relates to method for the cracking treatment of waste residues slurry produced in a synthesis process of an organic silicone monomer. The comehtod comprises: adding a high-boiling material of the same mass into a organic silicon waste residue slurry liquid and solid mixture containing 20 percent of solid to prepare a cracking feed solution, wherein a catalyst is tri-n-butylamine andthe cracking reaction temperature is 80 to 160 DEG C; and introducing HCl gas, wherein the ratio of the feed speeds of the hydrogen chloride and the raw material mixed liquid is 1:1.05-1:1.12. The method has the advantages that: the residue slurry containing 20 percent of solid is used in combination with the high-boiling material, so a monosilane product can be separated directly in a cracking process; the conversion rate is over 70 percent; the selectivity of dimethyldichlorosilane is over 35 percent; the selectivity of methylsilane is over 40 percent; and the slurry residue obtained after cracking having certain liquidity and can be further treated.

The invention discloses a preparation method of carboxyl silicone oil. Undecylenic acid and methyl hydrogen dichlorosilane are taken as raw materials to be subjected to direct hydrosilylation in the presence of a platinum/carbon catalyst to obtain 11-carboxyl undecyl methyl dichlorosilane; and the carboxyl silane monomer 11-carboxyl undecyl methyl dichlorosilane and dimethyldichlorosilane are subjected to co-hydrolysis and equilibrium polycondensation to obtain 11-carboxyl undecyl methyl silicone oil. The preparation method has the following advantages: the preparation process of carboxyl silicone oil is simplified by adopting the method for preparing the carboxyl silane monomer by one step through the direct addition reaction; the raw materials adopted for synthesis are industrial raw materials and are suitable for industrial large-scale production; and after being prepared into emulsion and compounded with amino silicone oil emulsion, the prepared carboxyl silicone oil can provide very good softness and full hand feel when being applied to textile finishing.

The invention discloses a method for preparing inertia high-boiling silicone oil from organic silicone high-boiling residues. With organic silicone high-boiling residues as the reaction raw material, the method includes the four steps of hydrolysis, hydrosilylation, neutralization, and devolatiligation and decoloration. The organic silicone high-boiling residues as the raw material are rectified high-boiling residues or decomposed high-boiling residues. The rectified high-boiling residues are high-boiling residues obtained by separating dimethyldichlorosilance out of the organic silicone high-boiling residues in advance through rectification. The decomposed high-boiling residues are high-boiling residues obtained by decomposing the organic silicone high-boiling residues in advance through a decomposing device and separating out monosilane. The decomposed high-boiling residues or rectified high-boiling residues which are difficult to process and use are used as the raw material, and the inertia high-boiling silicone oil which is controllable in viscosity, low in activity and high in stability is prepared through hydrolysis, addition and other reaction. The method is controllable in reaction process, simple in post-processing method, conventional in reaction device, high in production efficiency, stable in product quality and suitable for large-scale industrial production.

A continuous hydrolysis process for organic dichlorosilane in order to prepare low-viscosity linear or cyclic organic siloxane includes at least three stages of cyclic hydrolysis reaction system. Each cyclic hydrolysis reaction system includes internal and external cyclic units.

The invention provides a processing and recycling process for silicon slurry, which comprises the steps as follows: silicon slurry is evaporated for gas and solid separation; high boiling point substances are obtained after the gas phase is condensed; the high boiling point substances react with hydrogen chloride to be cracked into mixed monomers such as methyl trichloro silicane, trimethyl chloro silicane, methyl silane, dimethyl dichloro silicane and the like; and after the fractionation, each pure monomer product can be obtained. The solid phase separated through evaporation mainly contains cuprous oxide, silicon, silicon dioxide and the like; hydrochloric acid (or sulfuric acid) is added into the solid phase to extract copper chloride (or copper sulfate, which can be sold directly) by a chemical method; and silicon and silicon dioxide are separated out. Iron powder is added into a copper chloride solution for extracting copper and ferrous chloride, and sodium hydroxide is added into the ferrous chloride solution for extracting ferrous oxide. The processing and recycling process is environment-friendly and can eliminate pollution, and meanwhile can recover various by-products from silicon slurry, thereby having well economic benefits.

A cationic organic silicon compound of reaction type color-fixing agent, is obtained by: react hydroxy silicone oil, dimethyl dichlorosilicane, amine, siloxane, together with quaternary ammonium agent. The durable color-fixing agent is of environmental protection. It improves color-fixing effect of active dyes in difficulty for color fixing and low fastness for washing. Besides those advantages, it is helpful for softening and has bactericidal effect. It can be used in direct dye and acidic dye to increase the wet fastness in fabrics, improve wear and sunshine tolerance, less influence in colors and tones of fabrics and have brighten and strengthen fuscous.

The invention relates to the field of catalysts used for synthesis of dimethyldichlorosilane, in particular to a ternary copper catalyst CuO-Cu2O-Cu for synthesis of dimethyldichlorosilane and its preparation method. The method comprises the following steps of: 1) taking copper oxide powder as a raw material, adding a reducing gas, controlling its flow to make the flow of the reducing gas introduced into per gram of CuO particles at 0.1ml/min-100ml/min, maintaining the temperature at 100DEG C-600DEG C, carrying out a reduction reaction for 0.5h-6h, thus obtaining partially reduced copper oxide; and 2) subjecting the partially reduced copper oxide obtained in step 1) to breaking and ball-milling, thus obtaining the ternary copper catalyst for synthesis of dimethyldichlorosilane. With copper oxide as the raw material, the method prepares the ternary copper catalyst CuO-Cu2O-Cu through a one-step reaction, and has the advantages of simple technological process, convenient operation, strong process controllability, and easy mass production. The prepared catalyst shows high dimethyldichlorosilane selectivity and silicon powder material conversion rate.

The invention relates to a method for preparing polysiloxane by hydrolyzing dimethyl dichlorosilane, which comprises two continuous hydrolysis steps (1) and (2) and a neutralization step (3): step (1), dimethyl dichlorosilane, concentrated hydrochloric acid of the concentration greater than 35 percent and dilute generated by secondary hydrolysis are hydrolyzed at 10-60DEG C and under the pressure of 0-0.3MPa according to the weight ratio of 1: 1.5: 0.5-1: 1.5: 3; step (2), hydrolysis is carried out in excess water, and the reaction temperature is normal temperature; and step (3), the neutralization reaction is carried out, resin is adopted to adsorb a filter unit, the stuffing is cation-base exchange resin with large surface area, and the height of the stuffing is 2-4 meters; the content of the hydrolysate Cl- is less than 10ppm, the product siloxane prepared in the method has the viscosity less than 50mPa.S, and the content of impurity in hydrogen chloride gas is less than 10ppm.

The invention relates to a cracking process of organosilicon high-boiling components.. The cracking process is characterized in that organosilicon high-boiling components are used as raw materials and are subjected to impurity removal, N,N-dimethylaniline, N,N-diethylformamide or tri-n-butylamine are selected as a catalyst, the catalytic cracking is performed inside a reaction vessel to which hydrogen chloride gas is introduced, and finally, dimethyldichlorosilane, monomethyltrichlorosilane, monomethyldichlorosilane and trimethylchlorosilane are respectively recovered through a layered cooling tower at different temperatures. The cracking process has the advantages that the matching is reasonable, the operation is simple, the recovery ratio is high, and more than 60% of dimethyldichlorosilane product with high added value can be obtained.

The invention relates to an improvement of the producing method of methylchlorosilane, adding methylchlorodisilane, and a catalyst N, N-dimethylaniline1 accounting for 1-2% of the weight of methylchlorodisilane into a cracking kettle, making the materials a certain quantity, where the kettle is installed with a fractionating tower. It controls temperature at 90-110 deg.C, charging hydrogen chloride into the materials, making the molar ratio of methylchlorodisilane to hydrogen chloride 1 to 0.9-5.5, and its characteristic: the ratio of the height of the crackling kettle to the diameter = 1.0-2.0; the flux of the hydrogen chloride is 16 cu m/h; reacting for 5 hours, and then supplementing methylchlorodisilane into the kettle, and later supplementing once at 2h intervals, supplementing the hydrogen chloride once 200 kg, and completing in 0.5 h; supplementing the catalyst 2 kg at 4h intervals and completing in 10 minutes. It continuously reacts for 28-36 h, and collects condensate. It does not preprocess raw materials, and the sum of methylhydrodichlorosilane and dimethyldichlorosilane higher than that of existing techniques.

The invention discloses a synthetic method for avibactam sodium salt. The method comprises the following steps: taking (2S, 5R)-5-[(benzyl oxyl) amino] piperidine-2-formamide as a starting material; constructing a urea ring by carbonyl diimidazole under the effect of dimethyldichlorosilance to obtain (2S, 5R)-6-(benzyl oxyl)-7-oxo-1,6-diazabicyclo [3.2.1] octane-2-formamide; then carrying out hydrogenation to remove benzyl; carrying out sulfonation reaction on the compound and a sulfonated reagent; synthesizing into a quaternary ammonium salt intermediate by using quaternary ammonium salt; and finally carrying out ion exchange to obtain the avibactam sodium salt. The improved process is low in cost, simple and convenient to operate, good in product quality and suitable for industrial production. In a process of synthesizing the intermediate (2S, 5R)-6-(benzyl oxyl)-7-oxo-1,6-diazabicyclo [3.2.1] octane-2-formamide, dimethyldichlorosilance which is low in price is used, and therefore, the production cost is greatly reduced.

The invention discloses a dimethyl dichlorosilane hydrolysis method for directly producing gaseous hydrogen chloride, and belongs to the technical field of hydrolysis during the production of methyl chlorosilane. The method comprises the following steps of: pre-mixing the dimethyl dichlorosilane and concentrated hydrochloric acid through a jet mixer and then feeding the mixture into a static mixer for hydrolysis of concentrated hydrochloric acid with pressure so as to obtain a reaction mixture; introducing the reaction mixture into a combined separator with a plate type tower; separating the acid oil, acid and gas from the reaction mixture; and processing the acid oil, the acid and the gas respectively. The method ensures complete reaction and complete separation so as to obtain relatively pure hydrogen chloride gas and ensure difficult blockage of a methyl chloride synthesizer and pipelines thereof through forcible hydrolysis of the static mixer and separation of the combined separator with the plate tower in coordination with water removal by condensation; and the hydrogen chloride per se has pressure so as to realize the gravity feed of the hydrogen chloride. The method can obviously improve the product yield; and the unit consumption of the dimethyl dichlorosilane per ton of methyl siloxane is below 1.7 tons.

The invention discloses fluorosilicon oil with a high-efficiency defoaming performance and a preparation method thereof. Acroleic acid and fluorine-containing fatty alcohol generate esterification reaction under the effect of a catalyst to synthesize fluorine-containing fatty alcohol acrylate; the fluorine-containing fatty alcohol acrylate and dichloromethyl silane generate silicon hydrogen addition reaction to obtain fluorine-containing dichlorosilane; the fluorine-containing dichlorosilane and dimethyl dichlorosilane generate dechlorination cyclization reaction under the effect of a metal oxide; and finally, under the effect of a blocking agent hexamethyl disiloxane, the fluorosilicon oil is obtained by ring-opening polymerization reaction. The fluorosilicon oil has low surface tension and good defoaming and foam inhibiting effects as an oil defoamer.

The invention discloses modified fluorine-containing silicone oil and a preparation method thereof. The preparation method of the modified fluorine-containing silicone oil comprises the following steps: firstly reacting hydrogen-containing dichloromethylsilane which serves as a starting material, chloroplatinic acid which serves as a catalyst and octavinyl polyhedral oligomeric silsesquioxane (POSS) to synthesize a vinyl polyhedral oligomeric silsesquioxane dichloromethylsilane monomer; then carrying out hydrolysis co-balance by the monomer, dimethyldichlorosilance and trimethylchlorosilane to prepare vinyl polyhedral oligomeric silsesquioxane side group silicone oil; and finally carrying out single electron transfer reaction (SET) by vinyl and perfluoroalky iodide in a vinyl polyhedral oligomeric silsesquioxane structure of the side group to prepare the modified fluorine-containing silicone oil. According to the modified fluorine-containing silicone oil, octavinyl polyhedral oligomeric silsesquioxane is added in a side chain of the silicone oil, so that the heat resistance of the silicon oil is improved; by virtue of the fluoroalkylation reaction, the surface tension of the fluorine-containing silicone oil is reduced. The modified fluorine-containing silicone oil is excellent in water and oil repellency and resistance to high temperature; the high-temperature-resistant fluorine-containing silicone oil is mild in reaction conditions, simple and convenient tin preparation process and easily available in raw materials, and is suitable for industrial production.