Method of producing alkoxysilanes

FIELD: chemistry.

SUBSTANCE: one-step method of producing tri- and tetraalkoxysilanes is proposed, involving direct interaction of silicon with an appropriate aliphatic alcohol containing 1 to 4 carbon atoms, in the presence of a catalyst such as copper or copper chloride at a temperature of 200-300°C, which is carried out in the vibrating bed of milling bodies in the acceleration range of oscillations of 26.6 to 985.9 m/s2.

EFFECT: method is chlorine-free process that meets modern environmental requirements, and ensures the production of the desired product in high yield and high conversion of the starting materials.

8 cl, 7 ex



Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to methods of purification of alkoxysilanes and deals with obtaining highly pure tetraethoxysilane. Claimed is a method of tetraethoxysilane purification, including the initial processing of a product to be purified with a 0.3-1.5% water ammonia solution, added with intensive mixing to tetraethoxysilane which must be purified in a volume ratio (4-6):1, further rectification of the preliminarily purified product and its purification by distillation without boiling at a rate of evaporation from the surface of 0.5-1.5 ml/cm2·hour. The technical result consists in the following: the method makes it possible to obtain a highly pure product with the content of limited metal admixtures at the level of 10-6 wt %, chlorine less than 10-3 wt % and suspended particles with the diameter of 0.3 mcm about 200 particles/cm3.

EFFECT: indices of the obtained tetraethoxysilane quality satisfy the requirements for initial products for highly technological materials.

3 cl, 1 tbl, 4 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to biologically active compounds. What is presented is a new compound of meglumine orthosilicate having new biological activity noncharacteristic for silicic acid esters, increasing body resistance to physical activity. There are also presented versions of a method for preparing meglumine of meglumine and tetraethoxysilane.

EFFECT: what is prepared and characterised is a new hydrolysis-resistant compound which can be applied in medicine, and may be also used as a biologically active additive to compensate for silicon deficiency.

4 cl, 3 dwg, 2 tbl, 11 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing alkoxysilanes of general formula Si(OR)4, where R is an alkyl group. Disclosed is a method of producing alkoxysilanes by reacting aliphatic asymmetrical ethers of general formula R1OR2, where R1=butyl, iso-butyl, tert-butyl, tert-amyl and R2=methyl, ethyl, with finely dispersed silicon metal in gas-vapour phase in a closed reactor at temperature 200-270°C in the presence of copper monochloride as a catalyst, taken in amount of 10-20% of the weight of silicon metal.

EFFECT: improved method of producing alkoxy silanes, which enables to replace chlorosilanes and alcohols with aliphatic ethers, as well as increasing output of alkoxysilanes and purity of the end product.

1 cl, 9 ex

FIELD: chemistry.

SUBSTANCE: method of obtaining alkylalkoxysylanes, namely octyltriethoxysylane, can be used for creating compositions, possessing water-repellent, electro-insulating and other properties, as well as intermediate product for obtaining other silicon-organic compounds. Claimed is method of obtaining octyltriethoxysylane by interaction of octane with trichlorsylane at temperature on reaction mass boiling in presence of Spier catalyst (0.1 "н" solution of platinum hydrochloric acid in isopropyl alcohol) and etherification of obtained octyltriethoxysylane with excess of absolutised alcohol with further target product separation by known methods. Invention allows to reduce time of interaction of octane with trichlorsylane (hydrosylation reaction) to 5 hours with platinum catalyst expenditure 0.0002-0.0003% of charged reagents weight, as well as eliminate application of solvent.

EFFECT: increase of hydrosylation process efficiency with minimal expenditure of platinum catalyst, reduction of reaction time and elimination of solvent application.

7 cl, 1 tbl, 11 ex

FIELD: synthesis of biologically active compounds.

SUBSTANCE: invention provides novel biologically active compounds, notably solvate complexes of silicon and titanium glycerates imparting transcutan impermeability to medicaments, which can have utility as ointment base for transdermal therapeutic systems characterized by high penetration ability. There are described solvate complexes of silicon and titanium glycerates depicted by following formula: 2Si(C3H7O3)4·Ti(C3H7O3)4·xC3H8O3, wherein 9≤ x≤ 30, and hydrogels based thereon, containing water and gel-forming additive at following proportions of components: solvate complexes 48.4-65.2%, gel-forming additive 0.1-0.6%, and water the rest.

EFFECT: enlarged resource of transcutan-active materials.

2 cl, 3 tbl, 5 ex

FIELD: synthesis of organosilicon compounds.

SUBSTANCE: invention relates to production of alkoxysilanes of general formula RnSi(OR1)4-n, wherein R and R1 are lower alkyls and n = 0 or 1, which can be used in manufacture of silane-linking agents, organosilicon varnishes, resins, and the like. Invention proposes production of alkoxysilanes via etherification of chlorosilane at 0-30°C followed by two-step desorption of hydrogen chloride. First-step desorption is carried out at 40-80°C. Second-step desorption is carried out in reactor-desorber, which is tubular apparatus constituted by seven in series connected heating jacket-equipped sections, wherein alcohol is fed to sections 2-5 in amount 25-30% of the weight of reaction mass while maintaining temperature 70°C in the first section rising to 150°C in the last section. From hydrogen chloride released in etherification and desorption stages, acid alcohol can be condensed and then recycled to process.

EFFECT: increased productivity of process and stabilized quality of product.

2 cl, 3 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for synthesis of alkoxysilanes. Invention describes a method for synthesis of alkoxysilanes of the general formula: R'nSi(OR)m wherein n = 0-3; m = 1-4 and n + m = 4. Method involves reaction of chlorosilanes of the general formula: R'nSiClm wherein R' means hydrogen atom (H), CH3, C2H4, C2H or C6H6 with alcohols of the general formula: ROH wherein R means (C2-C8)-alkyl or (C2-C8)-aryl. Chlorosilane solution in an inert volatile nonpolar solvent is added to boiling alcohol solution in the same solvent at temperature 75-95°C, solvent is distilled off and evolving dry hydrogen chloride is captured. Method provides increasing yield, simplified process and decreasing time during the reaction carrying out.

EFFECT: improved method of synthesis.

6 cl, 1 tbl, 11 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes a method for preparing tetraalkoxysilanes. Method involves the interaction of ground silicon with alcohol in the high-boiling solvent medium in the presence of a copper-containing catalyst at enhanced temperature to obtain trialkoxysilane and its the following dehydrocondensation with alcohol in the presence of a catalyst. Products formed in reaction of silicon with alcohol as a vapor-gaseous mixture are fed to dehydrocondensation with alcohol in the presence of calcium oxide or hydroxide as a catalyst. Method provides simplifying process and reducing energy consumption.

EFFECT: improved preparing method.

4 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes a new chemical compound polyethoxysiloxane of the general formula: where R are similar or different organooxy-groups representing residues of aromatic alcohols: 2-phenylethyl, cinnamic, thymol, vanillin, vanilla, salicylic aldehyde, eugenol, santanol, santalidol, menthol, isobutyl; n = 3, 4, 5; x = 1-6, and a method for their preparing. Invention provides synthesis of polyethoxysiloxanes comprising pharmacophore organooxysilyl ligands that can be used as modifying agents of textile materials and able to confer to them stable aroma odor useful for aromatization, and antibacterial properties and enhanced deformation-strengthening properties to nonwoven materials simultaneously.

EFFECT: improved preparing method, valuable properties of compounds.

3 cl, 3 tbl, 4 dwg, 9 ex

FIELD: silicon-containing substances, medicine, pharmacy.

SUBSTANCE: invention describes silicon glycerates eliciting transcutaneous conductivity of medicinal agents with the composition of the formula: Si(C3H7O3)4 x xC3H8O3 wherein 3 ≤ x ≤ 10 with dynamic viscosity 4.6-28.5 Pa x s (20 ± 0.5°C). Compounds are prepared by interaction of tetraethoxysilane with glycerol in the mole ratio = 1:(7-14) in the presence of tetrabutoxy-titanium (0.06 mole/mole of tetraethoxysilane) and removal of formed ethyl alcohol in heating of reaction mass to 120-130°C and keeping at this temperature for 3 h, not less. Also, invention describes glycerohydrogels based on element-organic glycerates containing water and gel-forming additive that contain as element-organic glycerates silicon glycerates with the composition of the formula Si(C3H7O3)4 x xC3H8O3 wherein 3 ≤ x ≤ 10 as they contain electrolyte as a gel-forming additive in the following ratio of components, wt.-%: silicon glycerates, 8.2-65.1; electrolyte, 0.1-0.6, and water, the balance. Proposed compounds - silicon glycerates and glycerohydrogels based on thereof are physiologically active substances eliciting transcutaneous conductivity of medicinal agents with possible broad spectrum of their applying in medicine.

EFFECT: valuable medicinal properties of compounds.

2 cl, 2 tbl, 2 dwg, 7 ex

Aluminium oxide // 2550368

FIELD: metallurgy.

SUBSTANCE: particles porosity is 60-80%, and porous structure is presented by long, parallel channels with close packing, with channels cross-section size 0.3-1.0 mcm and length up to 50 mcm.

EFFECT: structure of suggested aluminium oxide simplifies passage of the substances participating in various processes inside the particle ensuring access to the internal surface of the aluminium oxide, where both catalytic reactions and adsorption can occur.

2 dwg

FIELD: medicine.

SUBSTANCE: invention refers to ophthalmic devices and methods for preparing them. What is presented is a soft silicone hydrogel contact lens which possesses an ability to deliver a hydrophobic comfort-maintaining agent (phospholipid, glycolipid, glyceroglycolipid, sphingolipid, sphingoglycolipid, fatty alcohol containing 8 to 36 carbon atoms, or a mixture thereof) into the user's eye gradually releasing it from a polymer matrix consisting of hydrophobic chains formed of a silicon monomer or macromere, and hydrophilic chains formed of a hydrophilic monomer or macromere when in use. What is also presented is a method for making the above contact lens.

EFFECT: in the presented soft silicone contact lens, the hydrophobic comfort-maintaining agent is not covalently bond to the polymer matrix wherein it is distributed and can be released from the soft hydrogel contact lens into the user's eye when in use reliably for a long period of time and thereby reinforcing and stabilising a lipid layer of the lachrymal fluid film and reducing eye dryness.

16 cl, 2 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing triethoxysilane which is suitable for producing monosilane for semiconductor engineering and solar power, as well as for various organosilicon liquids and polymers. Disclosed is a method of producing triethoxysilane by directly reacting metallurgical silicon with dry ethyl alcohol in a medium of a high-boiling solvent in the presence of a copper (I) chloride catalyst, where higher efficiency of the process is achieved through two-step activation of the mixture of silicon, solvent and catalyst. At the first step, the mixture is held in a hydrogen current at 180-250°C for 0.5-2.5 hours while stirring. At the second step, the reaction mass is held in the same conditions in an atmosphere of an inert gas without stirring.

EFFECT: disclosed method of activating the reaction mass enables to achieve silicon conversion of more than 75% and triethoxysilane selectivity of over 80%.

1 cl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing alkoxy silanes using microwave energy. Disclosed is a method wherein silicon metal, a suitable hydroxy compound and a copper catalyst are exposed to microwave radiation to form a corresponding trialkoxy silane.

EFFECT: disclosed method enables to obtain desired alkoxy silanes with high selectivity, at low temperatures and over a shorter period of time compared to traditional methods.

29 cl, 16 ex

FIELD: electricity.

SUBSTANCE: invention relates to light-radiating devices using non-stoichiometric tetragonal rare-earth silicate luminophors. The proposed light-radiating device comprises a light-emitting diode, which emits light in an ultraviolet or visible part of spectrum, and a non-stoichiometric luminescent material arranged around the light-emitting diode. The luminescent material absorbs at least some light emitted by the light-emitting diode, and radiates light with a wavelength differing from the absorbed light. The non-stoichiometric luminescent material has a tetragonal crystalline structure and comprises more silicon in a crystalline grid compared to its content in the crystalline grid of silicate luminophors, having a stoichiometric crystalline structure.

EFFECT: due to usage of non-stoichiometric tetragonal rare-earth silicate luminophors, light-radiating devices may be produced, which have higher resistance to impact of temperature and moisture.

19 cl, 12 dwg, 3 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing silicon-furan-containing monomers which are stable over time, can be combined with epoxy resins and can modify physical-mechanical and thermomechanical properties of cured epoxide compositions. The method involves reaction of tetrachlorosilane with furfuryl alcohol in a medium of pure acetone while cooling to 0-5°C in the presence of triethylamine. Molar ratio of tetrachlorosilane:furfuryl alcohol:triethylamine is equal to 1:4:4.

EFFECT: obtaining silicon-furan-containing monomers which are stable over time, can be combined with epoxy resins and can modify physical-mechanical and thermomechanical properties of cured epoxide compositions.

1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemistry of organosilicon compounds, namely to elaboration of efficient sulphur-containing catalyst, applied for direct synthesis of triethoxysilane from metallurgical silicon and ethyl alcohol, as well as to method of obtaining said catalyst. Described is catalyst of direct synthesis of triethoxysilane based on copper chloride (1), representing ultrafine copper powders (1), whose spherical aggregates have diameter from 600 nm to 3 mcm and consist of globules with diameter to 200 nm, which, in their turn, represent nanoparticles of copper chloride (1) with size to 20 nm. Also described is method of obtaining described above catalyst by reductive thermolysis of chelate copper complex, obtained in situ from copper chloride dehydrate (11) in polyol medium.

EFFECT: obtaining target product with selectivity above 80%.

2 cl, 11 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: polycrystalline silicon powder with mean grain size of about 5 mcm is put into a chemical etching solution consisting of a mixture of hydrofluoric and nitric acid and water in ratio 2:1:10, and held therein for 60-90 minutes while stirring continuously until the end of porosification of silicon. The powder of porous silicon is then filtered, dried for 30 minutes at temperature of about 100°C and mixed with a solution of a photosensitiser from the class of cyclic tetrapyrroles with concentration from 5×10-5 to 3×10-3 mol/l. The obtained suspension is filtered and dried on air.

EFFECT: obtaining a novel hybrid photosensitiser, which widens the range of agents for action on cancer cells through photodynamic therapy.

1 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention claims compound of the formula I, where R1 is alkyl; phenylalkyl optionally substituted by halogen; phenyl optionally substituted by halogen, halogen alkyl or alkoxy; thienyl optionally substituted by halogen; or benzo[b]thienyl optionally substituted by halogen; R2 is pyridyl or pyrimidinyl; R3 is alkyl; halogen alkyl; phenyloxylalkyl optionally substituted by halogen or alkyl; phenyl optionally substituted by halogen, alkyl or alkoxy; thienyl or alkylsilyl; R4 is H; or its salt, and methods of obtainment thereof. Additionally invention claims intermediate compound of the formula VI and method of its obtainment, composition for control of pathogenic microbes, and various methods of pathogenic microbe control.

EFFECT: improved efficiency of application.

29 cl, 1 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: invention concerns obtaining powder material of transitional aluminium oxide. First version involves powder material with inoculation particles of transitional aluminium oxide with form factor 3:1 or more and average particle size approximately over 110 nm and under 1000 nm. Second version involves powder material with needle-shaped inoculation particles containing transitional aluminium oxide, with form factor 3:1 or more, secondary form factor 3:1 or less, and average particle size approximately over 75 nm. Third version involves powder material with plate-shaped inoculation particles containing transitional aluminium oxide, with form factor 3:1 or more, secondary form factor 3:1 or more, and average particle size approximately over 125 nm. Method of obtaining involves use of aluminium metahydroxide precursor and aluminium metahydroxide inoculation in suspension, thermal processing of suspension to transform aluminium metahydroxide precursor into aluminium metahydroxide powder material at temperature over 120°C, and burning.

EFFECT: production of aluminium oxide powder with novel morphological properties.

60 cl, 3 dwg, 3 ex

FIELD: elimination of malodorous elements from silicone solvents used in dry chemical cleaning procedures.

SUBSTANCE: method involves providing contacting of silicone solvent with adsorbent in order to eliminate odor; separating silicone solvent; performing dry cleaning procedure with the use of silicone solvent free of malodorous elements.

EFFECT: effective removal of undesired odors from volatile silicone.

18 cl, 4 tbl, 4 ex