Method of obtaining complex yttrium, barium and copper oxide. RU patent 2503621.
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Method of obtaining basic chloride or copper (ii) nitrate / 2476380 Invention relates to technology of obtaining copper (II) salts. Method includes direct interaction of metal oxide with water solutions of hydrochloric or nitric acid with intensive mixing, including in presence of glass beads as grinding agent. Process is carried out with range of initial concentrations of acids from 0.4 to 2.7 mol/kg and mole ratio with copper (II) oxide in the range from (0.8:1) and to (1.8:1), with weight ratio of initial charge and glass beads (1:0.2)÷(1:1), at temperatures 15-50°C to the moment of process self-termination under current control over amount of accumulated copper (II) salts and acid spent on said purposes. After that, reaction mixture is separated from glass beads and filtered. Separated hard phase of reaction mixture is washed with 0.2-0.5 mol/kg solution of acid-reagent, after which it is returned for charge of repeated process. Washing solution is combined with reaction mixture filtrate. Obtained mixture is neutralised with 1.2-3.3 mol/kg water ammonia, dosed in small portions in such a way that pH does not exceed value 6.5-7.1. Product hard phase, precipitated during neutralisation, is left in contact with liquid phase for 12-24 hours, after which it is filtered, washed with distilled water and dried. Water solution of ammonium nitrate or chloride is used for other purpose. |
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Method of producing heteronuclear acetates of palladium with non-ferrous metals / 2458039 Invention relates to chemistry of platinum metals, particularly synthesis of palladium compounds, specifically synthesis of heteronuclear acetates of palladium with non-ferrous metals. The method of producing heteronuclear acetates of palladium with non-ferrous metals involves reaction of an acetate compound of palladium and a non-ferrous metal compound in a glacial acetic acid solution, where the reaction of compounds, taken in molar ratio palladium: non-ferrous metal of 1:(0.90-0.97), takes place in glacial acetic acid used in amount of (600-800)% of the molar amount of palladium, at temperature (70-90)°C with evaporation of the solvent to wet or dry residue, with repeated addition of glacial acetic acid in amount of (200-600)% of the molar amount of palladium, repeated evaporation of the solvent at temperature (80-120)°C, with treatment of the dry residue, pre-heated to (70-90)°C, with a solution of a mixture of benzene or toluene and acetic acid anhydride with volume ratio thereof equal to (4-8):1 respectively, the amount of the acetic acid anhydride being equal to (20-60)% of the molar amount of palladium, at temperature (70-100)°C for (2-30) minutes, cooling the obtained suspension to temperature (40-70)°C and filtering the desired compound. In another version, the method involves reaction of a palladium acetate and an acetate compound of a non-ferrous metal in glacial acetic acid solution with solvent evaporation, where the reaction of compounds, taken in molar ratio palladium: non-ferrous metal equal to 1:(0.90-0.97), takes place in glacial acetic acid used in amount of (400-600)% of the molar amount of palladium, at temperature (80-120)°C with solvent evaporation to a dry residue, with subsequent treatment thereof with a solution of a mixture of benzene or toluene and acetic acid anhydride, pre-heated to (70-90)°C, with volume ratio thereof equal to (4-8):1 respectively, the acetic acid anhydride being in amount of (20-60)% of the molar amount of palladium, at temperature (70-100)°C for (2-30) minutes, cooling the obtained suspension to temperature (40-70)°C and filtering the desired compound. |
 Method of producing copper (ii) ferrite / 2451638Invention relates to a method of producing copper (II) ferrite with a tetragonal spinel structure and can be used in chemical industry in sulphuric acid production processes. Initial iron (III) and copper (II) oxides are homogenised with addition of a mineralising agent - potassium chloride in amount of 0.5-1.5 wt % to the mixture of oxides, the mixture is briquetted at pressure 10 MPa and then thermally treated at temperature 850-1000°C. |
 Method of extracting copper (ii) ions from ammonia media using beta-n-oxyethylhydrazides of aliphatic carboxylic acids / 2422437Invention relates to a novel method of removing copper (II) ions from water in the presence of ammonia, which is based on using a floatation reagent in form of β-N-oxyethylhydrazides of aliphatic carboxylic acids of formula |
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Method of producing aqueous copper-silver compositions / 2420298 Invention relates to producing aqueous copper-silver compositions. Proposed method comprises dissolving silver oxide in distilled water in amount of 13·10-3 g per litre, cooling or heating of obtained solution to 20°C, solution settling and filtering. Then, obtained solution is used partially for producing copper ions by chemical rejection of silver from solution by metallic copper, filtration of copper solution, combining two solutions in one and additional filtration of prepared compositions. |
 Magnetic semiconductor material / 2400850Magnetic semiconductor material is a compound of chromium, gallium and copper selenide having chemical formula CuGaCr2Se5 and characterised by Curie point of 318K. |
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Method for removing copper from nickel-63 / 2323885 Method implies precipitation of Cu (I) iodide from nitric acid solution containing copper and nickel-63, in acidity range of 1 · 10-5 - 3 mol/l, by adding excess amount of an alkali metal iodide and sulphite mixture. Precipitate is isolated from mother liquor and washed, mother liquor and washing solution are combined, to the resulting solution ammonia is added, and nickel is precipitated from the ammonia solution by adding an alkali metal iodide or ammonium iodide. |
 Di-cuprous oxalate complexes as precursor materials for depositing metallic copper / 2322447invention relates to di-cuprous oxalate complexes stabilized with components of neutral Lewis base. There are described compounds of general formula (I) wherein copper is oxidation state +1 and R represents R-C≡C-R', which has at least one silyl group, R'HC=CHR containing at least one silyl group, or R'Si-C=C-R', where R represents A or at least one group SiR'3, R' represents R, H, or A, wherein L, R, and R', independently of each other, each can assume identical or different significances in different molecule positions, and A represents C1-C30-alkyl with nonbranched or branched chain. Described is also a method of preparing compounds of general formula (I) and a method of preparing high-cleaned thin copper layers. |
 Synthetic malachite producing method / 2308554Method comprises steps of dissolving basic copper carbonate in solution of ammonium carbonate containing excess molar concentration of ammonium per molar content of carbonic acid; dividing volume of initial working volume of solution by two parts by means of partition permeable for liquid and gaseous phases. In upper part there is dissolving zone where solid basic copper carbonate is placed. In lower part there is crystallization zone where preliminarily metallic or polymeric members of articles to be made are placed and where further evaporation of solution at temperature 40 - 95°C is realized. Formed after evaporation vapor-gas mixture is condensed and prepared condensate in the form of aqueous solution of ammonium carbonate is returned to dissolving zone for depositing from evaporated solution crystals of synthetic malachite onto surface of metallic or polymeric members arranged in crystallization zone. In dissolving zone temperature less by 20 - 30°C than temperature in crystallization zone is sustained. Concentration of Cu(II) in initial working solution is set equal to 45 - 60 g/l. |
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Method of production of cupper (i) thiocyonate (i)the lump sugar massecuite out of the cane-sugar raw / 2289545 The invention is pertaining to the field of chemical industry, in particular, to chemical technology of inorganic substances. The product produced by this method can be used as a pigment for the antifouling compositions of the catalytic agent of the processes of the organic synthesis, the stabilizing agent for the artificial fibers, for preparation of the electrolytes of the galvanic copper plating, for production of other copper compounds. Copper (I) thiocyonate is produced by the crystallization from the reactionary water solution containing copper (II), thiocyanide, the reactant- reducer. As the source of copper (II) uses the waste solutions of pickling of the printed-circuit boards or the waste electrolytes of the galvanic copper plating of the various chemical compositions. At that pH in the reactionary water solution is set from 0.0 up to 9.5. The presented invention allows to reduce the materials inputs for production of the cupper (I) thiocyonate, to expand the arsenal of the copper- containing materials used for production of cupper (I) thiocyonate, to increase efficiency of the process of production of cupper (I) thiocyonate, to utilize the toxic wastes and to reduce expenditures on the environmental protection at production of printed-circuit boards and electroplated coatings. |
 Method of obtaining stabilised water sol of nanocrystalline cerium dioxide, doped with gadolinium / 2503620Invention relates to technologies of nanomaterials production for obtaining of oxide fuel elements, thin coatings, films, which have high ionic conductivity. Method includes preparation of water solution of cerium and gadolinium salts, in which total concentration of rare earth elements constitutes 0.005÷0.02 mole per litre of water, and molar ratio of Ce:Gd constitutes from 19:1 to 4:1, addition of anion-exchange resin in OH-form to obtained solution until pH 9.0÷10.0 is reached, separation of formed colloidal solution from anion-exchange resin by filtering, hydrothermal processing at 120÷210°C for 1.5÷4 h and cooling to room temperature. Obtained unstable sol of nanocrystalline cerium dioxide, doped with gadolinium, is additionally stabilised with salt of polybasic acid (citric or polyacrylic) with molar ratio of rare earth elements in acid, equal 1:1÷4, and following slow drop-by-drop addition of ammonia water solution until pH 7÷8 is obtained. |
 Complex processing of coal combustion flue ash / 2502568Invention relates to processing of wastes, particularly, to ash-and-slag wastes of thermal electric power stations. Coal combustion ash is placed in reaction zone to add carbon sorbent thereto in amount of 10-25 kg per ton of ash. Then, it is processed by the mix of ammonium fluoride and sulfuric acid, heated to 120-125°C and held thereat for 30-40 minutes. Tetrafluorosilane resulted from said processing is absorbed by ammonium fluoride. Solution of ammonium hydroxide is introduced into that of ammonium tetrafluorosilicate to precipitation of silicon dioxide. Then, concentrated sulfuric acid in double surplus is added to aluminium residue, held at 250°C for 1.5 h and processed by water. Solid residue is calcined at 800°C. |
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Method of production of rare-earth element fluorosulphide powders / 2500502 Invention relates to inorganic chemistry, particularly to production of powders to be used in laser technology and optical instrument making. Proposed method comprises preparation of blend and its thermal treatment. Said blend is prepared from the powder of sesquialteral rare-earth element sulphides with particle size of 1-30 mcm and powder of rare-earth element trifluorides with particle size of 10-70 nm at molar ratio of 1:1.Thermal treatment of the blend is conducted at 650-800 °C for 20-30 minutes in atmosphere of argon, sulfiding gases H2S+CS2 and fluoridiser gases C2F4, CF4 obtained in Teflon pyrolysis. |
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Method of obtaining complex scandium chloride and alkali metal / 2497755 Invention relates to inorganic chemistry and deals with method of obtaining complex scandium chloride and alkali metal. Metallic scandium is mixed with lead dichloride and salt of alkali metal. Obtained charge is placed into crucible with inert atmosphere, heated to reaction temperature in presence of metallic lead and kept at temperature, exceeding melting temperature of mixture of salts by 50-100°, for 10-30 minutes. Metallic scandium is applied in compact form in from of pieces. As salt of alkali metal, metals chlorides are applied. In initial charge mixture of chloride salts of alkali metals is applied. |
 Method of producing powder of solid solutions of lanthanum, neodymium, praseodymium and samarium oxysulphides / 2496718Invention relates to inorganic chemistry and specifically to a method of producing powder of solid solutions of rare-earth oxysulphides for making ceramic articles, phosphors and laser materials. The method of producing powder of solid solutions of lanthanum, neodymium, praseodymium and samarium oxysulphides involves preparing a mixture of given mass of weighted forms of rare-earth oxides dissolved in nitric acid, precipitating rare-earth sulphates from the obtained solution using concentrated sulphuric acid, evaporating the formed suspension on air at 70 - 90°C to a dry state, grinding and calcining at 600°C for 1.5 hours, further grinding to a fine state and treating in a hydrogen stream with gas feed rate of 6 eq/h with respect to the weight of rare-earth sulphates at the following temperatures and duration of heat treatment: 600°C - 10 hours, 700°C - 5 hours and 850°C - 1 hour. |
 Molybdate-based inorganic pigment / 2492198Invention can be used in paint-and-varnish industry, in making plastic, ceramics and construction materials. The molybdate-based pigment, which contains cerium and an alkali-earth metal, is a complex molybdate with a scheelite structure of the composition Ca1-3/2XCexMoO4, where 0.10≥x≥0.02. |
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Method for synthesis of cuprates of barium and rare-earth elements / 2489356 Invention can be used in chemical industry. The method involves calcining a heteropolynuclear complex of nitrates of rare-earth elements, copper (II), barium and quinoline, after preliminary calcining, cooling and homogenisation. Basic calcining is carried out at temperature of 850°C for the yttrium subgroup, and at 750°C for the cerium subgroup. |
 Synthesis of cerium oxide nanoparticles in supercritical water / 2488560Invention can be used in chemical industry. Cerium oxide CeO2 nanoparticles are obtained by mixing 0.2 M Ce(NO3)3 · 6H2O solution with supercritical water. The reaction is carried out at temperature of 370-390°C and pressure of 240-260 atm. The ratio of the volume of the cerium salt solution to the volume of supercritical water is preferably equal to 2:10. |
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Method of extracting rare-earth metals from phosphogypsum / 2487834 Invention can be used in chemical industry and production of construction materials. Proposed method comprises processing phosphogypsum by sulfuric solution, filtration, extraction of precipitate of rare-earth metal insoluble compounds and separation of precipitate by filtration. Rare-earth metals are extracted from solution by oxalic acid or its soluble salts at consumption of 250-300 mol % while solution is neutralised to pH=1.0-2.5. Obtained precipitate of oxalates is separated from mother solution, rinsed, dried and calcined. |
 Fuel additive containing cerium dioxide nanoparticles with altered structure / 2487753Invention relates to a method of producing cerium dioxide nanoparticles and use thereof. Described is a method of producing cerium dioxide nanoparticles with a given lattice, which contain at least one transition metal (M), wherein: (a) an aqueous reaction mixture is prepared, said mixture containing a source of Ce3+ ions, a source of ions of one or more transition metals (M), a source of hydroxide ions, at least one nanoparticle stabiliser and an oxidant which oxidises the Ce3+ ion to a Ce4+ ion, at initial temperature ranging from about 20°C to about 95°C; (b) mechanical shearing of said mixture and passing said mixture through a perforated sieve to form a homogeneously distributed suspension of cerium hydroxide nanoparticles; and (c) creating temperature conditions that are effective for oxidation of the Ce3+ ion to a Ce4+ ion to form a product stream containing cerium dioxide nanoparticles, containing a transition metal Ce1-xMxO2, where x assumes a value from about 0.3 to about 0.8, said nanoparticles have a cubic fluorite structure, average hydrodynamic diameter ranging from about 1 nm to about 10 nm and geometric diameter from about 1 nm to about 4 nm, wherein the nanoparticle stabiliser is water-soluble and has a value Log KBC ranging from 1 to 14, where KBC denotes a constant for binding the nanoparticle stabiliser to a cerium ion in water and said temperature conditions that are effective for oxidation of the Ce3+ ion to a Ce4+ ion include temperature from about 50°C to about 100°C. Described is a method of preparing a homogeneous dispersion containing stabilised crystalline nanoparticles of cerium dioxide with a given lattice, containing a transition metal, Ce1-xMxO2, where M is at least one transition metal and x assumes a value from about 0.3 to about 0.8; (a) preparing an aqueous mixture which contains stabilised cerium dioxide nanoparticles containing a transition metal, Ce1-xMxO2, having a cubic fluorite structure, wherein, wherein said nanoparticles have average hydrodynamic diameter ranging from about 1 nm to about 10 nm and geometric diameter less than about 4 nm; (b) concentrating said aqueous mixture containing said stabilised cerium dioxide nanoparticles containing a transition metal, thereby forming an aqueous concentrate; (c) removing essentially all water from said aqueous concentrate to form an essentially water-free concentrate of stabilised cerium dioxide nanoparticles containing a transition metal; (d) adding an organic diluent to said essentially water-free concentrate to form an organic concentrate of said stabilised cerium dioxide nanoparticles containing a transition metal; and (e) merging said organic concentrate with a surfactant in the presence of a nonpolar medium to form said homogeneous dispersion containing stabilised crystalline nanoparticles of cerium dioxide containing a transition metal, Ce1-xMxO2, where M and x assume values given above. Described is a deposited coating for the catalytic converter of the exhaust system of an internal combustion engine, where said deposited coating is obtained using said homogeneous dispersion. |
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Molybdate-based inorganic pigment / 2492198 Invention can be used in paint-and-varnish industry, in making plastic, ceramics and construction materials. The molybdate-based pigment, which contains cerium and an alkali-earth metal, is a complex molybdate with a scheelite structure of the composition Ca1-3/2XCexMoO4, where 0.10≥x≥0.02. |
FIELD: chemistry.
SUBSTANCE: invention can be applied in microelectronics. To obtaining complex yttrium, barium and copper oxide YBa2Cu3O7-δ, from water solution, which contains yttrium, barium and copper nitrates, combined sorption of yttrium, barium, copper in given molar ratio Y:Ba:Cu = 1:2:3 is carried out at the stage of sorption from the said solution on carboxyl cationite KB-4p-2. After that, obtained material is dried and subjected to successive heating at temperature 110 - for 2 h, at 250°C - for 2 h, at 450°C - for 5 h, at 600°C - for 3 h, at 850°C - for 6 h and after that for 1 hour in oxygen atmosphere.
EFFECT: invention makes it possible to simplify obtaining complex yttrium, barium and copper oxide.
1 ex
The present invention relates to the production of a complex oxide of yttrium, barium and copper composition YBa2Cu3O7-δand can be used in microelectronics.
The known method of obtaining this compound, comprising preparing the initial mixture by mixing the oxides of yttrium, copper, and barium carbonate, followed by extraction and multiple intermediate chafing products annealing (so-called ceramic method of synthesis) (Appl. Series "solid state Chemistry". V.6. - M.: VINITI, 1988, p.36-37). The disadvantages of the method is a multistage process, high temperature synthesis, as well as the difficulty of achieving chemical homogeneity of the product.
Also known chemical method of obtaining YBa2Cu3O7-δby reacting an aqueous solution of nitrates of yttrium, copper, and barium with citric acid followed by evaporation of the solution to the viscous state, dehydration in vacuum and annealed at 900 - 950°C for two hours (EN 2081937 C1, 20.06.1997). Disadvantages of the method: the lack of consensus about the number of the flowing phase transitions, obtaining chemically heterogeneous product.
Also known cryochemical method of obtaining YBa2Cu3O7-δ, based on the dispersion of pre-cooked and mixed aqueous solutions of salts of the corresponding meta is fishing in the refrigerant with the subsequent removal of solvent (ice) by the method of freeze-drying (Sabatin VP, Begun J.V., Gordeev IV and other Cryochemical synthesis of high-temperature superconductors. // Physical chemistry and technology of HTS materials. - M.: Nauka., 1989, pagination 126-127). Disadvantages of the method: quick freezing of fluids in the granules retained a large number of amorphous phases at the stage of thermal decomposition of the salt mixture is partial loss of copper.
The closest to the invention is a method for Y-Ba-Cu-O oxide by deposition of these metals in the form of oxalates from the aqueous solution, containing nitrates and acetates. The deposition is carried out with oxalic acid at a pH of 3.5 to 4.0 at room temperature followed by thermal decomposition of a mixture of oxalates and annealing product of thermolysis in a stream of oxygen at 950°C. the Disadvantage of this method is the difficulty of achieving the stoichiometry of the cations (1:2:3), the composition of the oxides is strongly dependent on pH, the presence of barium carbonate in the products of thermal decomposition (F. Caillaud, J-F. Baumard and A. Smith A model for the preparation of YBa2Cu3O7-δorthorhombic phase by controlled precipitation of oxalates. Mat. Res. Bull., 1988. Vol.23, P.1273-1283).
The purpose of the invention is to simplify the process.
The aim is achieved in that the complex oxide YBa2Cu3O7-δobtained by thermal decomposition of the composite material of the resin - sorbed ions" taken in atomic ratios of 1:2:3.
Distinctive attribute is the kami of the invention is a sorption method, followed by thermal decomposition.
The essence of the invention lies in the fact that during sorption of ions of yttrium, barium, copper from aqueous nitrate solutions of their salts in a carefully calculated concentrations on carboxylic cation exchanger KB-4P-2 results in an even distribution of metal ions and the atomic ratio of 1:2:3.
In the final stages of drying and thermal decomposition occurs burnout of the organic part of the ion exchanger and the interaction of ions with the formation of the complex oxide YBa2Cu3O7-δin the form of microspheres.
Example. A portion of the cation KB-4P-2 in ammonium form, pour a solution containing nitrates of yttrium, barium and copper, and the concentration of yttrium, barium and copper in solution are respectively equal to,
,
. The obtained composite material, the resin - sorbed ions" dried and subjected to successive heat treatment at temperatures of 110°C - 2 hours, at 250°C - 2 hours at 410°C - 5 hours, at 600°C - 3 hours at 850°C for 6 h and then 1 hour in the atmosphere of oxygen. The result is a complex oxide YBa2Cu3O7-δwith an atomic ratio Y:Ba:Cu=1:2:3.
Thus, the proposed method allows us to simplify the achievement of stoichiometry on the cations on stage sorption compared to the prototype. In the conditions of pyrolysis synthesis of essential compounds for implementation through the camping is not on the reactions of the chemical interaction between substances (oxides, salts and so on), and between ions, spaced from each other at atomic distances. Marked facilitates and accelerates the process of formation of the synthesized compounds. The final product in this case is the shape of the grains of the resin granules representing their microstructure of the dense packing of very small crystallites. In the formation of these granules bulk products, the latter retains the primary structure, which provides high mechanical and physico-chemical properties of the finished product.
The way to obtain a complex oxide of yttrium, barium and copper YBa2Cu3O7-δfrom an aqueous solution containing nitrates of yttrium, barium and copper, using a heat treatment, characterized in that together sorption of yttrium, barium, copper in a given molar ratio Y:Ba:Cu=1:2:3 stage sorption from the specified solution of carboxylic cation exchanger KB-4P-2 with further drying and subsequent heating of the cation exchanger at a temperature of 110°C for 2 hours, at 250°C 2 h at 450°C - 5 h at 600°C, 3 h at 850°C - 6 h and then 1 h in oxygen atmosphere.