Composition based on complex oxides of zirconium, phosphorus and calcium for coating obtaining. RU patent 2502667.
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Method of producing amorphous carbon-coated nanoparticles and method of producing transition metal carbide in nanocrystallite form / 2485052 Invention relates to a method of producing nanoparticles of a transition metal oxide coated with amorphous carbon. A liquid mixture containing as precursors at least one alkoxide of a transition metal selected from Ti, Zr, Hf, V, Nb and Ta, an alcohol and excess acetic acid with respect to the transition metal is diluted with water to obtain an aqueous solution. Precursors are contained in the solution in a molar ratio which is sufficient to prevent or significantly limit sol formation. The transition metal, carbon and oxygen are contained in said solution in a stoichiometric ratio which corresponds to the composition of nanoparticles. The aqueous solution is freeze-dried and the freeze-dried product undergoes pyrolysis in a vacuum or an inert atmosphere to obtain nanoparticles. The obtained nanoparticles can be subjected to carbothermal reduction to obtain carbide nanoparticles. |
 Composition based on zirconium oxide, titanium oxide or mixed zirconium and titanium oxide, applied on aluminium oxide or aluminium oxyhydroxide carrier, methods of its obtaining and its application as catalyst / 2476381Invention relates to field of chemistry, in particular, to catalytic compositions, applied as catalyst. Claimed are catalytic composition, methods of its application and catalytic system. Catalytic system, which contains at least one oxide on carrier, selected from zirconium oxide, titanium oxide or mixed zirconium and titanium oxide, applied on aluminium oxide or aluminium oxyhydroxide carrier, and which has after burning at 900°C for 4 hours size of particles of oxide on carrier not larger than 10 nm, if oxide on carrier is obtained on zirconium oxide base or not larger than 15 nm, if oxide on carrier is obtained on the base of titanium oxide or mixed zirconium and titanium oxide. Catalytic system contains claimed catalytic composition. |
 Filler and composite materials with zirconium and silica nanoparticles / 2472708Invention relates to filler materials made of nanoparticles for use in composite materials, including dental composite materials. The filler materials contain clusters of silica and zirconium dioxide nanoparticles. The filler materials can be obtained by mixing a sol of silica nanoparticles with a sol of pre-formed crystalline particles of zirconium nano-oxide. |
 Method of processing zirconium tetrachloride to obtain zirconium dioxide and hydrochloric acid / 2466095Invention relates to methods of processing zirconium tetrachloride and can be used in chlorine metallurgy when producing zirconium dioxide and hydrochloric acid. The method involves mixing zirconium tetrachloride with water in molar ratio ZrCL4:H2O=1:(1.0-1.2), obtaining zirconium oxychloride and hydrogen chloride gas, dissolving zirconium oxychloride in water, adding sulphuric acid with distillation of the HCl-H2O azeotropic mixture and precipitation of basic zirconium sulphate, filtering the suspension, washing and calcining the residue to obtain zirconium dioxide. Hydrogen chloride gas formed when producing zirconium oxychloride is taken for absorption, where the absorbent used is the HCl-H2O azeotropic mixture obtained during precipitation of basic zirconium sulphate. Concentrated hydrochloric obtained from absorption can be used in non-ferrous metallurgy when leaching concentrates and ores, etching metal surfaces of equipment, metal-roll and for other purposes. |
 Zircon concentrate processing method / 2450974Method involves chlorination of zircon concentrate, separate condensation of chlorinates, cleaning of silicon and zirconium tetrachlorides, aqueous hydrolysis of zirconium tetrachloride and deposition of zirconyl sulphate with distillation of azeotropic HCl-H2O mixture, filtration, washing and calcination of deposition so that zirconium dioxide is obtained, high-temperature vapour-phase hydrolysis of silicon tetrachloride in hydrogen-air flame so that pyrogenic silicon dioxide and HCl-bearing exhaust gases are obtained; absorption of hydrogen chloride by using azeotropic HCl-H2O mixture as absorbent, which is formed during hydrolytic separation of zirconyl sulphate. |
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Composition based on zirconium oxide, titanium oxide or mixed zirconium and titanium oxide, deposited on silicon oxide support, methods of producing said composition and use thereof as catalyst / 2448908 Invention can be used in inorganic chemistry. The catalytic composition contains at least one oxide on a support, which is based on zirconium oxide, titanium oxide or a mixed zirconium and titanium oxide, deposited on a silicon oxide-based support. After firing at 900°C for 4 hours, the oxide on the support has the form of particles deposited on a support and size of said particles is not greater than 5 nm if the oxide on the support is based on zirconium oxide, not greater than 10 nm if the oxide on the support is based on titanium oxide and not greater than 8 nm if the oxide on the support is based on a mixed zirconium and titanium oxide. After firing at 1000°C for 4 hours, particle size is not greater than 7 nm if the oxide on the support is based on zirconium oxide, not greater than 19 nm if the oxide on the support is based on titanium oxide and not greater than 10 nm if the oxide on the support is based on a mixed zirconium and titanium oxide. |
 Zirconium oxide and way of its production / 2442752invention refers to powdered zirconium oxide, way of its production and its application in fuel cells, notably for production of electrolyte substances for ceramic fuel cells. The powdered zirconium oxide containing up to 10 mole % of at least one metal oxide from the scandium, yttrium groups, the group of rare-earth elements and/or their mixtures is characterized by the extension density from 1.2 to 2.5 g/cm³ measured according to ASTM B 417. |
 Composition based on zirconium oxide, yttrium oxide and tungsten oxide, method of production and use as catalyst or catalyst support / 2440299Composition contains 1-20% yttrium oxide, 1-30% tungsten oxide and zirconium oxide - the rest. The specific surface area of the composition is at least equal to 20 m2/g after calcination for 4 hours at 900°C. |
 Zirconium hydroxide / 2434810Invention relates to chemistry and can be used in catalytic processes. Amorphous zirconium hydroxide has surface area of at least 300 m2/g, total pore volume of at least 0.70 cm3/g and average pore size from 5 nm to 15 nm. First, an aqueous solution containing sulphate anions and a zirconium salt with the ratio ZrC2:SO3 ranging from 1:0.40 to 1:0.52 are obtained. The solution is then cooled to temperature lower than 25°C. Alkali is then added to precipitate amorphous zirconium hydroxide which is then filtered and washed with water or alkali to remove residual sulphate and chloride. The washed residue undergoes thermal treatment at excess pressure of not less than 3 bars and dried. |
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Method of producing mineral material using zirconium oxide grinding beads containing cerium oxide, obtained products and use thereof / 2432376 In order to obtain ground mineral material a) at least one mineral material which is optionally in form of aqueous suspension is taken, b) said material is ground, c) the ground material obtained at step (b) is optionally sieved and/or concentrated, d) the ground material obtained at step (b) or (c) is optionally dried. The grinding step (b) is carried out in the presence of zirconium oxide grinding beads containing cerium oxide, having cerium oxide content between 14 and 20% of the total weight of said beads, preferably between 15 and 18% of the total weight of said beads, and more preferably approximately 16% of the total weight of said beads. The average size of grains after sintering grains which form said beads with average diameter less than 1 mcm is preferably less than 0.5 mcm and more preferably less than 0.3 mcm. The obtained ground mineral material is in form of aqueous suspension, wherein the weight ratio ZrO2/CeO2 is equal to 4-6.5, preferably 4.6-5.7 and more preferably 5.3. |
 Method and device for hydration of cao containing material in form of particles or powder, hydrated product and use of hydrated product / 2370442Invention can be used for producing hydrated material for reducing content of SO2 in waste gases. In the method of hydrating CaO containing material in form of particles or powder, water is added in an amount sufficient for maintaining partial pressure PH2O, as a function of temperature, within a range defined by the formula |
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Method of production of the pigment for manufacture of the cardboard and paper / 2283392 The invention is pertaining to the method of production of the pigment for manufacture of the cardboard and paper and may be used in pulp and paper industry at production of the filled paper, the coated paper and the cardboard. Calcium hydroxide suspension is treated with aluminum sulfate solution in the aqueous medium at stirring. The treatment is conducted in the aqueous medium containing the binding in the dissolved state. The binding is chosen from the group, which includes starch and polyvinyl alcohol in the amount of 0.5-5.0 mass % from the mass of the absolutely dry pigment, and-or the colorant in the amount of 0.1-0.5 mass % from the mass of the absolutely dry pigment. The technical result of the invention is the improved quality of the pigment and expansion of its field of application. |
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Method of production of the composite pigment for manufacture of the cardboard and paper / 2283391 The invention is pertaining to the method of production of the composite pigment for manufacture of the cardboard and paper and may be used in pulp and paper industry at production of the filled paper, the coated paper and the cardboard. Calcium hydroxide is mixed with kaolin and added with aluminum sulfate in the aqueous medium at stirring. The aqueous medium contains the binding chosen from the group, which includes starch and polyvinyl alcohol in amount of 1.5-5.0 % from the mass of the absolutely dry pigment, and-or the water soluble colorant in amount of 0.1-0.5 % from the mass of the absolutely dry pigment. The technical result of the invention is the improvement of the composite pigment quality and expansion of its field of application. |
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Method of production of the pigment for manufacture of the cardboard and paper / 2283390 The invention is pertaining to the method of production of the pigment for manufacture of the cardboard and paper and may be used in pulp and paper industry at production of the filled paper, the coated paper and the cardboard. In the water at intense stirring feed powders of calcium hydrate and calcium carbonate at the ratio of the indicated components accordingly from 1.0:2.2 up to 1.0:12.9. The produced suspension is gradually added with aluminum sulfate at its ratio to the total mass of the calcium hydroxide and calcium carbonate from 1.0:0.85 up to 1.0:4.30. Then the temperature of the mixture is increased up to 8О-85°С and the produced reaction mixture is kept at stirring within 90-180 minutes with formation of the dispersion of the pigment with the share of the dry substances in it equal to 20-35 %. Then the dispersion is dried and grinded into the powder. The powder is dispersed in the water containing the given amount of the dissolved coolant and-or binding - starch or polyvinyl alcohol. The technical result of the invention production of the pigment with the new properties, that allow to expand the field of its application at manufacture of various types of the cardboard and the paper. |
 Method of preparing pigment for manufacturing paper and cardboard / 2274693Invention relates to pigment, which can be used in manufacture of paper with filler, coated paper, and cardboard. Calcium hydroxide and calcium carbonate powders taken in proportion between 1.0:2.2 and 1.0:23.5 are added to vigorously stirred water, after which temperature of mixture is raised to 80-85°C and resulting reaction mixture is kept being stirred for 90-180 min to form dispersion of pigment containing 20-35% solids. |
 Method of processing phosphogypsum / 2402488Invention relates to chemistry and can be used to process environmentally hazardous phosphogypsum. Phosphogypsum is mixed with used cooling and hydraulic fluids containing ethylene glycol. The mixture undergoes deep dehydration to form a powdered product at temperature of 100-170°C while stirring constantly and then subjected to high-temperature burning. |
 Method of producing highly porous coating based on silicon and manganese double oxides / 2496712Invention relates to the technology of producing highly porous coatings based on double oxide systems used in the fast growing fields of electronics and lighting engineering, production of catalyst materials, as functionally sensitive, decorative, filter and radiation redirecting coatings. The method involves preparing a film-forming solution, followed by deposition thereof onto the surface of substrates, drying, annealing and cooling. The freshly prepared film-forming solution is held for 8-13 days at temperature of 6-8°C; drying is carried out at temperature of 60°C for 30-40 minutes, followed by nonlinear heating to 800-900°C in an air atmosphere; in the first 15-20 minutes, the rate of heating is maximum and is equal to 22°C/min; in the next 17 minutes, the rate of heating is kept at 18°C/min; and then for 12 minutes, the rate of heating is 12°C/min; in the last 40-20 minutes, the rate of heating is kept at 0.5°C/min; and holding is carried out at 800-900°C for 1 hour, with gradual cooling in natural cooling conditions of a muffle furnace, with the following ratio of components of the film-forming solution, wt %: tetraethoxysilane 22.4-21.6, hydrochloric acid 1.3·10-4-1.2·10-4, distilled water 3.2-1, metal salt MnCl2·4H2O 0.8-6.6, ethyl alcohol (98 vol. %) - the balance. |
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Method of producing metal products / 2478566 Method for industrial cleaning of a stream of a low-grade polyvalent cation with purity P1 by forming a precipitate of a double salt of the polyvalent cation with purity P2 and a solution of the polyvalent cation with purity P3, where P2>P1>P3, comprises the following steps: (a) forming from said stream a medium which contains water, the polyvalent cation, a cation selected from a group consisting of ammonia, alkali metal cations, protons and any combination thereof, and anions, wherein the formed medium is further characterised by presence of (i) a precipitate of a double salt which contains a polyvalent cation, at least one of said cations and at least one of said anions; and (ii) a solution of the polyvalent cation; wherein concentration of said anions is higher than 10% and the ratio of concentration of said cation and said anion in said solution of the polyvalent cation is in the range of the DS zone, which is defined in the present document; and (b) separating at least a portion of said precipitate from said solution. |
 Method and device for continuous production of metal oxide catalyst / 2477653Invention relates to production of metal oxide materials, including metal hydroxides and/or metal oxides and catalysts. Proposed method comprises the following steps: dissolving metals in nitric acid to produce metal nitride and releasing NOX and water vapor. Hydrolysis of metal nitride solution by introducing compressed superheated water vapor in metal nitride solution to produce suspension of hydroxide suspension and acid gas. Main components of acid gas are NO2, NO, O2 and water vapor. Suspension filtration and drying to produce metal hydroxides and/or metal oxides. Further recovery of produced metal hydroxides and/or metal oxides and production of metal oxide catalyst in traditional process. Released gas NOX may be used for production of reusable nitric acid. Proposed device consists of system to produce metal salt solution, metal salt solution hydrolysis system, product production system, and system to produce and recycle nitric acid. |
 Method for production of pure nanodispersed powder of titanium dioxide / 2470855Invention relates to a technology for production of nanodispersed materials and may be used in chemical industry, electronics, powder metallurgy. The method includes mixing of a pure solution of a precursor with alcohols supporting burning, spraying and combustion of a mixture in flame, at the same time the pure solution of the precursor is a pure acidulous aqueous solution of titanium tetrachloride, and alcohol content in a sprayed mixture makes at least 80% (wt), water - not more than 15% (wt). The size of drops of the sprayed mixture makes not more than 2 mcm. |
 Method of producing copper oxide nanowhisker structures / 2464224Invention relates to high-temperature electrochemistry, particularly to electrolytic production of copper oxide nanowhisker structures, and can be used in catalyst engineering. Molten polytungstate, containing 10 mol % K2WO4, 55 mol % LI2WO4 and 35 mol % WO3, undergoes electrolysis in a pulsed potentiostatic mode. The voltage is equal to 1060-1090 mV and pulse duration is equal to 0.1 s. A platinum anode is used. The cathode used is copper foil. |
FIELD: chemistry.
SUBSTANCE: invention can be used in chemical industry. Composition for obtaining thin film of complex oxides of zirconium, phosphorus and calcium contains ethyl alcohol, preliminarily distilled and dried to 96 wt %, zirconium oxochloride, calcium chloride and orthophosphoric acid with the following component ratio, wt %: zirconium oxochloride - 4.7-6.8; calcium chloride - 2.6-4.4; orthophosphoric acid - 0.5, ethyl alcohol - the remaining part.
EFFECT: claimed invention makes it possible to obtain thin films, possessing high refractive indices.
3 ex
The invention relates to the technology of thin-film materials based on complex oxide systems used in the rapidly developing fields of electronics and lighting industry, construction industry, including the technology of integrated circuits; as a corrosion-resistant, decorative, filter, and distributes radiation coatings.
Known composition to obtain a film of zirconium dioxide (application for invention No. 93014629/33, 6 C04B 41/65, C04B 35/48, publ. 1995.06.09)used for coating on the glass. The composition to obtain a film of Zirconia includes hydrated of oxochloride zirconium and contains 0,1...1 wt.% nitrate of cobalt. The invention allows to reduce energy consumption and improve the performance of the coating process on the basis of when the coating thickness over 100 nm.
The disadvantages of this structure should include the instability properties of the proposed film over time, due to structural transformations polymorphs of Zirconia.
Known composition to obtain a thin film based on a system of double oxides of zirconium and zinc (RF Patent 2411187, publ. 10.02.2011, C01G 25/02), which includes the preparation of film-forming solution containing ethyl alcohol, previously distilled and about Osenniy to 96 mass %, and it of oxochloride zirconium, followed by the application by centrifuging this solution on a substrate and a stepped heat treatment in the following ratio of components, mass %: oxochloride zirconium - 4,0-8,6, nitrate zinc - 3,8-7,6, ethyl alcohol - the rest.
The disadvantages of known composition include low adhesion of the film material to the substrates.
As a prototype of the selected article (L.P. Barilo, I.E. Petrovskaya, Y.S. Lutova, LN. Spivakov "Synthesis and physico-chemical properties of thin-film and dispersed functional silicophosphate materials" // Bulletin of the Tomsk Polytechnic University. Chemistry. 2011. - T. No. 3. P.41-47.), in which a method of obtaining thin-film and dispersed compositions based on complex oxides SiO2-P2O5-CaO. To obtain a thin-film oxide materials used film-forming solutions (ERP), which was prepared on the basis of 96% ethyl alcohol, tetraethoxysilane, phosphoric acid, calcium chloride given composition. Coating was obtained on the silicon substrates of centrifuging, the film formation was carried out in two stages: in the air in a drying Cabinet at 60°C in a muffle furnace at a temperature of 600°C. the resulting films have refractive indices from of 1.41 to 1.45. The disadvantage of the prototype I have is the low value of the refractive index.
The task of the claimed invention to provide a composition based on zirconium, phosphorus and calcium, providing stability to the structure, physico-chemical and target properties in a wide range of concentrations, as well as achieve high values of refractive index when using them as a redistributive radiation coatings.
The problem is solved in that a composition based on complex oxides by the Sol-gel method involves the preparation of a solution of the film-forming component and ethyl alcohol in the presence of inorganic acids and their salts, providing the processes of hydrolysis and polycondensation in solution, with subsequent deposition on the surface of the substrate by centrifuging and holding step of heat treatment, the oxide coating, but unlike the prototype as a film-forming substance used oxochloride zirconium as an additive - phosphoric acid and calcium chloride in the following ratio of components, mass %:
Oxochloride zirconium - 4,7-6,8
Calcium chloride - 2,6-4,4
Orthophoria acid - 0.5
Ethyl alcohol - the rest
To obtain thin films based on a system of complex oxides of zirconium, phosphorus and calcium are preparing film-forming solution, using as solvent e is silt alcohol 96 mass %, pre-distilled, and add oxochloride zirconium in the form of hydrated ZrOCl2·8SH2O. At room temperature ZrOCl2·SH2O and CaCl2dissolved separately in ethanol with periodic stirring for 1-3 hours depending on the concentration of oxochloride zirconium. Then the solutions merge and add phosphoric acid. After maturation, the film-forming solution for 1-2 days, depending on the concentration of oxochloride zirconium, it is applied by centrifuging in a centrifuge MPW-340 with the speed of 3000-5000 rpm for poloski of silicon, then perform step heat treatment before the formation of oxides in thin film.
The most appropriate temperature for storage THEN you should consider temperature in the range of 22-25°C for 6-8 months, depending on the concentration of oxochloride Zirconia.
For the preparation of solutions used utensils second accuracy class.
Below are examples illustrating the invention.
Example 1.
To prepare 100 ml of a film-forming solution, you need to take to 6.8 g of crystalline oxochloride zirconium and dissolve it in 40 ml of 96 mass % of ethyl alcohol, then take 2.6 g of calcium chloride to dissolve it in 40 ml of 96 mass % of ethyl alcohol, then the solution is drained, add 0.3 ml of phosphoric acid is density 1,685 g/cm 3and bring to volume of 100 ml ethyl alcohol. After maturation, the solution for 24 hours THEN put on a silicon substrate by the method of centrifugation and subjected to a stepwise heat treatment at temperatures of 60°C for 20 min and at temperatures of 800°C for 1 hour, resulting in a thin film of the composition ZrO2-P2O5-CaO with a refractive index of 1.9 and a thickness of 75 nm.
Example 2.
To prepare 100 ml of a film-forming solution should take 5.5 g of crystalline of oxochloride zirconium and dissolve it in 40 ml of 96 mass % of ethyl alcohol, then take 3.2 g of calcium chloride to dissolve it in 40 ml of 96 mass % of ethyl alcohol, then the solution is drained, add 0.5 ml of phosphoric acid with a density of 1,685 g/cm3and bring to volume of 100 ml ethyl alcohol. After maturation, the solution for 24 hours THEN put on a silicon substrate by the method of centrifugation and subjected to a stepwise heat treatment at temperatures of 60°C for 20 min and at temperatures of 800°C for 1 hour, resulting in a thin film of the composition ZrO2-P2O5-CaO with a refractive index of 2.1 and a thickness of 78 nm
Example 3.
To prepare 100 ml of a film-forming solution, you must take the 4.7 g of crystalline oxochloride zirconium and dissolve it in 40 ml of 96 mass % of ethyl alcohol, then take 4.4 g chloride is calcium dissolve it in 40 ml of 96 mass % of ethyl alcohol, then the solution is drained, add 0.5 ml of phosphoric acid with a density of 1,685 g/cm3and bring to volume of 100 ml ethyl alcohol. After maturation, the solution for 24 hours THEN put on a silicon substrate by the method of centrifugation and subjected to a stepwise heat treatment at temperatures of 60°C for 20 min and at temperatures of 800°C for 1 hour, resulting in a thin film of the composition ZrO2-P2O5-CaO with a refractive index of 2.0 and a thickness of 70 nm.
Composition for obtaining thin films of complex oxides of zirconium, phosphorus and calcium containing ethyl alcohol, previously distilled and dried to 96 wt.%, and oxochloride zirconium, characterized in that it additionally contains calcium chloride and phosphoric acid in the following ratio, wt.%:
| Oxochloride Zirconia | 4,7-6,8 |
| Calcium chloride | 2,6-4,4 |
| Phosphoric acid | 0,5 |
| Ethanol | Rest |