Method of obtaining basic zinc carbonates
SUBSTANCE: invention can be used in chemical industry. Method of obtaining basic zinc carbonates includes chemical conversion of coarse-dispersed zinc oxide in water solution of carbon dioxide and ammonia, further formation of target product, its filtration, drying, condensation and return of gaseous products to the stage of chemical conversion. Chemical conversion of zinc oxide into basic zinc carbonate is performed in ammonia-carbonate water solution in heterogenic conditions with molar ratio carbon dioxide:ammonia, equal 1:(5-9), temperature 15-50 °C and atmospheric pressure.
EFFECT: invention makes it possible to obtain amorphous sediments of pentazinc hexahydroxodicarbonate Zn5(CO3)2(OH)6 of stoichiometric composition with particle size, which does not exceed 50 nm, to simplify the process, reduce energy consumption and ecological load on the environment.
1 dwg, 3 tbl, 5 ex
The invention relates to a technology for major carbon zinc salts, which can be used as raw materials and intermediate products in the pharmaceutical, microelectronics, chemical, tire, paint and oil industries.
A known method of producing hydroxocobalamin Nickel by dissolving the specified metal in ammonium carbonate solution at elevated temperature and subsequent deposition of the desired product by distillation of the ammonia, and the dissolution of Nickel are in the presence taken separately or in combination with each other nitric acid, ammonium nitrate and Nickel content of nitrate-ion 2-50% with respect to the mass of dissolved metal [description of the invention to as. the USSR №1518307 from 16.10.1987, IPC4C01G 53/06, publ. 30.10.1989]. Because Nickel belongs to the d-metals of the fourth period of the periodic system of chemical elements of Mendeleev, and zinc, the present method can be successfully extended to zinc.
The disadvantages of this method include the variable composition of the finished product, the low productivity of the process, its frequency and low efficiency of each operation, the presence of large amounts of wastewater due to the necessity of washing the obtained precipitation from nitrate ions. In addition, the process which engages stage, flowing at elevated temperatures, resulting hardware complexity of the method and additional energy consumption.
Closest to the proposed method to the technical essence is a method of obtaining a basic carbonate salts, in particular zinc and its oxides, which comprises dissolving (as one of the stages of the process of chemical transformation) metal-containing compounds of zinc ammonium carbonate solution (as a particular case of an aqueous solution of carbon dioxide and ammonia) followed by the formation of the target product, filtering, drying, condensation and return of the gaseous products at the stage of dissolution, and as a metal-containing compound used is inactive (or rather coarse) zinc oxide [description of the invention to the patent of Russian Federation №2043301 from 25.06.1991, MPK C01G 3/00, C01G 3/02, C01G 9/00, C01G 9/02, C01G 51/04, C01G 51/06, C01G 53/04, C01G 53/06, publ. 10. 90.1995]. The result is improved performance of the continuous process stream due to the intensification of the process steps, it is possible to obtain active oxides. In addition, due to trapping gas emissions, the regeneration liquid effluent and re-use them in the process receive waste clean technology.
However, this method has significant drawbacks. P and the temperature increase of the process monohydrate ammonia decomposes and accordingly, changing the concentration of carbonate-ammonium solution, which leads to variability in the composition of the final product (so-called floating, non-stoichiometric composition). In the literature [see NS Nikolaev, V.V. Ivanov, A.A. Shubin. Synthesis of highly dispersed forms of zinc oxide: chemical precipitation and thermolysis. Journal of Siberian Federal University. Chemistry. 2010. series 3, No. 2, p.160-170] noted the existence of several forms of a basic carbonate of zinc, such as Zn5(CO3)2(OH)6(mineral hydrozincite), Zn3CO3(OH)4, hydrates Zn3CO3(OH)4·2H2O, Zn4CO3(OH)6·2H2O. So the finished product is a complex mixture of these substances.
In addition, the method is implemented at temperatures and pressures higher than ambient temperature and normal atmospheric pressure, resulting hardware complexity of the process and additional energy. At the stage of washing the finished product from the impurity cations and anions requires a large amount of water and its subsequent costly cleanup.
It is also known [see NS Nikolaev, V.V. Ivanov, A.A. Shubin. Synthesis of highly dispersed forms of zinc oxide: chemical precipitation and thermolysis. Journal of Siberian Federal University. Chemistry. 2010. series 3, No. 2, p.160 and 170]that the particle size of the primary carbonate C the NCA affects the size of oxide particles, resulting in the process of thermal decomposition. The process of evaporation in this way leads to the formation of coarse particles of carbonate and gidroksicarbonata zinc, and as a result of their thermolysis obtained, as shown by the results of x-ray phase analysis of coarse particles.
The problem solved by the present invention and the technical result achieved are obtaining amorphous precipitation gidroksicarbonata zinc Zn5(CO3)2·(OH)6(hexahydrobenzylcarbonate pentazine) stoichiometric composition with a particle size not exceeding 50 nm, and in simplifying the process, reducing energy consumption for its implementation and reducing the environmental impact on the natural environment.
To solve the problem and achieve the stated technical result in the production method of the main carbon zinc salts, including chemical transformation of metal-containing zinc compounds in an aqueous solution of carbon dioxide and ammonia, followed by the formation of the target product, filtering, drying, condensation and return of the gaseous products through chemical transformation, and as a metal-containing compound used coarse zinc oxide, chemical conversion of zinc oxide in a basic carbonate of the Inca is carried out in ammonium carbonate aqueous solution in a heterogeneous conditions at a molar ratio of carbon dioxide:ammonia equal to 1:(5 to 9) the temperature of 15-50°C and atmospheric pressure.
Thus, the method of obtaining basic carbonate salts of zinc (Zn) includes chemical transformation (dissolution) of the metal-containing zinc compounds in an aqueous solution of carbon dioxide (CO2) and ammonia (NH3(in ammonium carbonate solution), followed by the formation of the target product, filtering, drying, condensation and return of such gaseous substances, such as ammonia and small amounts of carbon dioxide into chemical transformations (dissolution), and as a metal-containing compound used coarse (inactive) zinc oxide (ZnO), chemical conversion of zinc oxide in basic zinc carbonate is carried out in ammonium carbonate aqueous solution in a heterogeneous conditions at a molar ratio of CO2:NH3equal to 1:(5-9), the temperature of 15-50°C and atmospheric pressure.
The results of x-ray phase analysis of the original and the synthesized compounds and the products of their thermolysis of illustrating the invention, are summarized in Tables 1 and 2 and presented in the diffraction pattern (see drawing).
The particle size of the ZnO crystallites was determined from the broadening of the form x-ray diffraction profile (see the diffraction pattern of ZnO powder). Based on the experimentally defined values true physical broadening of the line β (half-width d is fractional reflections from the analyte, grad), you can determine the average crystallite size D (nm), using equation Selyakova-sherrer:
where K - the coefficient of 0.94 for x-ray analysis;
λ is the wavelength of x-ray radiation (nm);
cosθHKLcosine of the scattering angle (dimensionless quantity).
Thus, the product of thermolysis of Zn5(CO3)2(OH)6obtained by dissolving zinc oxide in an aqueous solution of carbon dioxide and ammonia at a molar ratio of CO2:NH3equal to 1:(5 to 9)is zinc oxide with an average particle size equal to 10-50 nm.
Analyze the essential features of the invention.
Chemical conversion of zinc oxide in basic zinc carbonate is carried out in ammonium carbonate aqueous solution in a heterogeneous environment. Unlike the closest analogue where to get the homogeneous saturated solution of Aminatou of zinc and its subsequent evaporation with a selection of basic carbonates of zinc, of variable composition, in the present technical solution of the original solid crystalline zinc oxide is transferred to the solid basic zinc carbonate without getting saturated solution of Aminatou zinc. This greatly simplifies the technology by eliminating stages of evaporation and washing the precipitate. In addition, reduced environmental load of the surrounding nature is th environment. Remain constant with respect to the stoichiometric composition of Zn5(CO3)2(OH)6in crystalline form with a predominance of amorphous phase after thermal decomposition (thermolysis) allows to obtain a final product with a particle size of zinc oxide 10-50 nm. Such small particles have unique features and are used in the manufacture of components of semiconductor devices, electrical contact materials, UV filters, solar cells, sensors, catalysts, sorbents, and so on, in contrast to the properties of coarse particles known method [see RF patent №2043301], which do not possess such properties.
Heterogeneous chemical conversion of zinc oxide in basic zinc carbonate is carried out in an aqueous solution of carbon dioxide and ammonia at a molar ratio of CO2:NH3equal to 1:(5-9).
With decreasing molar relationship CO2:NH3the dissolution of zinc oxide in ammonium carbonate aqueous solution is less than 1:5, for example, 1:4.5 or below leads to the disappearance in precipitation of amorphous phase and enlargement of the particles in the crystalline phase, while increasing the molar ratio of the CO2:NH3more than 1:9, for example, 1:9.5 or above significantly increases the time of conversion of zinc oxide in basic zinc carbonate.
The results of the experiments and the following various molar ratios of CO 3and NH3summarized in Table 3.
Chemical conversion of zinc oxide is carried out at a temperature of 15-50°C. the temperature of the dissolution below 15°C 10°C and below, leads to a significant decrease in the rate of the process of obtaining basic zinc carbonate, and the temperature rises above 50°C 55°C or higher, leads to rapid decomposition of an aqueous solution of ammonia monohydrate and volatilization of gaseous ammonia, which changes the composition of the carbonate-ammonia solution and, as a consequence, the composition of the final product (non-stoichiometric composition of basic carbonate of zinc).
Chemical conversion of zinc oxide is carried out at atmospheric pressure. This pressure provides a stable and secure process that reduces energy consumption and simplifies its implementation in practice.
Implementation of the invention consider the following examples.
Example 1 (comparative). Getting gidroksicarbonata zinc Zn5(CO3)2(OH)6using homogeneous process.
The process is conducted at atmospheric pressure and a temperature of 25°C. In a reaction flask of 200 ml are placed hanging zinc oxide by weight of 1 g and the addition of ammonium bicarbonate by weight of 1.18, Then is added 100 ml of 0.24 M aqueous solution of ammonia. Included magnetic stirrer. Stirring is carried out for 2 hours the solution becomes homogeneous (pH 10,57). Next, the resulting solution was evaporated to 50 ml, and the reaction flask precipitation of basic zinc carbonate, which is separated by filtration and dried at 60°C for six hours.
As shown by the results of x-ray phase analysis, the precipitate is a mixture of coarse ZnCO3and Zn5(CO3)2(OH)6after thermolysis which is obtained ZnO with a particle size greater than 1 μm. The size was determined from the broadening of the form x-ray diffraction profile on the diffractometer DRON-2 (Cu K2- radiation, λ=1,54Å, graphite monochromator on the reflected beam) with a scanning speed of 2 deg/min
Homogeneous method proposed in the prototype, it is not possible to obtain basic zinc carbonate specified composition Zn5(CO3)2(OH)6and particles of zinc oxide with a size of 10-50 nm.
Example 2. Getting Zn5(CO3)2(OH)6in the heterogeneous conditions of the process of transformation with a molar ratio of CO2and NH3- 1:1.
The process is conducted at atmospheric pressure and room temperature. Hanging zinc oxide by weight of 2 g and ammonium hydrogen carbonate and 0.8 g placed in chemical beaker of 500 ml and add 200 ml of distilled water (molar ratio of CO2:NH3- 1:1). Stirring of the reaction mixture is carried out in such a way that th is would be solid ZnO and formed during the reaction the basic zinc carbonate were suspended. Experience time is 24 hours. The precipitate is filtered and dried at 60°C for six hours.
The results of x-ray phase analysis showed that the precipitate is crystalline Zn5(CO3)2(OH)6with a large particle size (see Table 2) from 10 to 100 μm. Particle size was determined using an optical microscope NU-2E.
Examples 3 and 4. Getting Zn5(CO3)2(OH)6in the heterogeneous conditions of the process of transformation with the recommended molar ratio of CO2and NH3.
The process is conducted at atmospheric pressure and room temperature of 20°C. a portion of the zinc oxide by weight of 0.5 g is placed in a chemical beaker (200 ml) and add 75 ml of distilled water. Stirring of the reaction mixture is carried out so that the solid zinc oxide and basic zinc carbonate were suspended. Later in the reaction mixture depending on experience type:
- the first option - 75 milliliters of binary aqueous solution of ammonium bicarbonate (NH4HCO3) and an aqueous solution of ammonia (NH3·H2O) with concentrations of 3,3÷10-2M and 13.2÷10-2M, respectively, the molar ratio of CO2:NH3- 1:5, experience time is 24 hours;
- the second option - 75 milliliters of binary aqueous solution of hydrocarb the Nata ammonia and aqueous ammonia with a concentration of 3.3÷10 -2M and 2.64÷10-1M, respectively, the molar ratio of CO2:NH3- 1:9, experience time is 48 hours.
The obtained precipitation was filtered and dried at 60°C for six hours.
The results of x-ray phase analysis shows that the sediments represent the crystal structure of Zn5(CO3)2(OH)6with small particle size from 20 to 50 nm and a high content of amorphous phase (see Table 3). The size was determined from the broadening of the form x-ray diffraction profile on the diffractometer DRON-2 (Cu K2- radiation, λ=1,54Å, graphite monochromator on the reflected beam) with a scanning speed of 2 deg/min
There is a possibility to use different molar ratio of CO2and NH3in the range between 1:5 and 1:9. The obtained crystal structures and their sizes will meet the stated requirements.
Example 5. Getting Zn5(CO3)2(OH)6in the heterogeneous conditions of the transformation process in pilot conditions.
In a reactor with a volume of 20 liters with anchor stirrer was placed 1 kg of zinc oxide (GOST 10262-73, qualification "H") and 0.4 kg of ammonium bicarbonate was then added to 16 l of an aqueous solution of ammonia with a concentration of 1.84 M (molar ratio of CO2:NH3- 1:7). The synthesis was carried out at a temperature of 20°C for 48 hours. The precipitate, after which Otdelenia from the mother liquor, dried at 50°C for 24 hours. The results of x-ray phase analysis shows that the sediment is crystals of Zn5(CO3)2(OH)6with small particle size and high content of amorphous phase. After thermal decomposition of the obtained crystal grains of zinc oxide with an average size of 20 nm.
Implementation of this technology on an industrial scale, for example, with basic carbon zinc salts in an amount up to 50 kg of above-mentioned conditions flow method proportionally increase.
As a result of implementation of the invention is substantially simplified way to obtain the primary carbon zinc salts of carbonate-ammonia solutions were obtained amorphous precipitation of gidroksicarbonata zinc stoichiometric composition and a particle size not exceeding 50 nm. Decreased energy consumption for the process. Decreased environmental burden on the environment.
|The results of x-ray phase analysis of the source connections|
|The research object||Card number database JCPDS||Hee is practical formula objects of study|
|The ammonium bicarbonate||44-1483||NH4HCO3|
|The results of x-ray phase analysis of the synthesized compounds and the products of their thermolysis|
|The research object||Card number database JCPDS||Chemical formula of research objects||The number cards solid product of thermolysis database JCPDS||The qualitative composition of the products of thermolysis|
|Basic zinc carbonate||72-1100||Zn5(CO3)2(OH)6||79-0205||ZnO|
|The results of heterogeneous chemical ol the rotation of zinc oxide in basic zinc carbonate|
|The molar ratio of CO2:NH3||Qualitative and phase composition of the products of dissolution according to x-ray phase analysis|
|1:10||Zn5(CO3)2(OH)6crystal structure with small particle size and the content of amorphous phase|
|1:9||Zn5(CO3)2(OH)6crystal structure with small particle size and the content of amorphous phase|
|1:7||Zn5(CO3)2(OH)6crystal structure with small particle size and the content of amorphous phase|
|1:5||Zn5(CO3)2(OH)6crystal structure with an average particle size of|
|1:3||Zn5(CO3)2(OH)6crystal structure with a large particle size|
|1:1||Zn5(CO3)2(OH)6crystal structure with a large particle size|
The method of obtaining the main carbon zinc salts, including chemical transformation of metal-containing compounds qi is the AC in an aqueous solution of carbon dioxide and ammonia, followed by the formation of the target product, its filtering, drying, condensation and return of the gaseous products through chemical transformation, and as a metal-containing compound used coarse zinc oxide, characterized in that the chemical conversion of zinc oxide in basic zinc carbonate is carried out in ammonium carbonate aqueous solution in a heterogeneous conditions at a molar ratio of carbon dioxide: ammonia = 1:(5-9), the temperature of 15-50°C and atmospheric pressure.
SUBSTANCE: method of making a planar waveguide of zinc oxide on lithium niobate involves preparing a film-forming solution, holding said solution for 1 day at room temperature, depositing the solution on polished lithium niobate, drying, annealing and gradually cooling in natural cooling conditions of a muffle furnace. The lithium niobate is pre-treated with 96% ethyl alcohol solution. The lithium niobate with the deposited film-forming solution is dried at 60°C for 1 hour, followed by annealing at 400°C in an air atmosphere at heating rate of 14°/min for 1 hour and at 870-1050°C at heating rate of 35°/min for 2-5 hours, with the following ratio of components of the film-forming solution, wt %: zinc nitrate crystalline hydrate 5.2-9.9%; salicylic acid 4.6-4.8%; 96% ethyl alcohol solution - the balance.
EFFECT: invention reduces labour consumption and power consumption of the process of making a planar waveguide which is resistant to radiation in the green spectral region and has maximum refraction index increment values.
1 dwg, 2 tbl, 3 ex
SUBSTANCE: invention relates to opto- and microelectronics and can be used to make opal-like structures. The method of producing photonic-crystal structures based on metal oxide materials involves filling a template consisting of monodispersed micropheres of polystyrene, solutions of metal-containing precursors, followed by annealing the structure on air at temperature of 450-550°C for 8-10 hours. The precursors from which the structure is formed are saturated alcohol solutions of tin dichloride SnCl2·2H2O or zinc nitrate Zn(NO3)2·2H2O.
EFFECT: invention enables to obtain photonic-crystal structures based on SnO2 and ZnO with a photonic stop band in the visible or near infrared spectral range and porosity of not less than 85%.
FIELD: process engineering.
SUBSTANCE: invention relates to making solid solutions with the structure of transitional element zinc ferrite-chromite-based spinel and may be used in organic synthesis for production of butadiene and hydrocarbons from synthesis gas as a catalyst. Proposed method uses blending the initial oxides of zinc, iron (III) and chromium (III), adding sodium chloride in amount of 0.3-1.3 wt % to the mix of mineralising agent oxides, pelletising at 10 MPa and heat treatment of oxides mix at 800-1000°C.
EFFECT: higher efficiency.
1 dwg, 1 tbl, 2 ex
SUBSTANCE: invention relates to the technology of producing salts of carboxylic acids, particularly acetic acid, and a method of producing high-purity anhydrous zinc acetate. High-purity zinc acetate is obtained by reacting a zinc-containing compound with acetic acid, where the zinc-containing compound used is diethylzinc which is pre-diluted with an inert solvent to concentration of not more than 20 wt %. The inert solvent used is preferably undecane. The invention enables to obtain high-purity anhydrous zinc acetate in which content of 18 limited metal impurities, according to chemical spectral analysis, is equal to 5·10-5 - 5·10-6 wt %.
EFFECT: method enables to include the obtained anhydrous zinc acetate into the category of high purity substances ACS 18-4; can be used in electronics, fibre optics, atomic power and other areas of emerging technology.
2 cl, 1 tbl, 1 ex
SUBSTANCE: invention relates to chemical engineering. The method of producing zinc peroxide involves reaction of zinc oxide and hydrogen peroxide, followed by dehydration of the reaction product. Components react in molar ratio zinc oxide/hydrogen peroxide ZnO/H2O2=1.0-0.85, and temperature in the synthesis zone of 15-30°C. When mixing the starting components, zinc oxide is added to hydrogen peroxide which is first stabilised with magnesium sulphate in molar ratio hydrogen peroxide/magnesium sulphate H2O2/MgSO4=700-850. Dehydration of the filtered reaction product is carried out by exposure to microwave radiation.
EFFECT: invention increases content of the basic substance in the obtained product and reduces power consumption.
5 cl, 1 dwg, 1 tbl, 4 ex
SUBSTANCE: invention relates to the technique of producing Zn64 isotope impoverished zinc oxide, purified from tin and silicon impurities, which is currently used as an additive in water coolant of the primary loop of nuclear reactors. Zn64 impoverished zinc oxide powder is obtained from Zn64 impoverished diethylzinc, dissolved in aqueous acetic acid solution with weight ratio of reactants zinc oxide: water: acetic acid equal to 1:(1.6-2.0):(1.8-2.2). The obtained solution is evaporated to oversaturation - formation of a dense crust of zinc acetate, gradually cooled to 25-30°C and then held for 15-20 hours. The zinc acetate crystalline hydrate precipitated from the solution is filtered and undergoes thermal decomposition in air to zinc oxide at 600-800°C for 4-6 hours.
EFFECT: invention reduces content of tin and silicon in the commercial product to less than 10-3 % and cuts the number of process steps.
SUBSTANCE: 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.
EFFECT: invention enables to realise a simple and stable method of producing desired compounds with high output.
4 cl, 46 ex, 2 tbl
SUBSTANCE: invention can be used in chemical industry. The method of producing zinc oxide involves grinding zinc metal powder, treating with a reaction mixture containing ammonia and calcining the obtained mass. The reaction mixture used is ammonium carbonate solution. Treatment with the reaction mixture is carried out in weight ratio of components Zn: ammonium carbonate solution equal to 1:(1-2), and the obtained material is calcined at 240-310°C.
EFFECT: invention increases specific surface area of zinc oxide.
1 tbl, 3 ex
SUBSTANCE: invention relates to chemistry. A neutral calcium-aluminium double salt has the formula Ca2m(Zn2n)Al2(OH)6+2(2m+2n-i)An * oH2O, where m and n assume the following values: m=0.5-3 and 0.5m≥n>0; An=CO3, where that group can be substituted completely or partially with at least one of the following groups selected from OH, ClO4, and o=0-3. This salt is obtained by reaction at step a) CaO or Ca(OH)2, ZnO or Zn(OH)a and Al(OH)3 in an aqueous suspension and adding CO2 or carbonate or bicarbonate of an alkali metal at temperature from 10 to 100°C. Reaction of the product obtained at step (a) with perchloric acid is possible. Double salts on which alkali metal perchlorates are deposited in liquid form are used as adsorbates. The double salts are used as additives for polyolefins as antipyrenes/smoke suppressors or filler material and for immobilising enzymes.
EFFECT: invention enables to obtain novel double salts.
8 cl, 2 tbl, 3 ex
SUBSTANCE: method of producing zinc oxide powder by oxidising zinc with oxygen while heating, where zinc metal first undergoes distillation at temperature lower than boiling point in a stream of an inert gas; the obtained powder is oxidised in a revolving reactor with a controlled atmosphere at temperature lower than the boiling point of zinc.
EFFECT: invention enables to obtain zinc oxide powder containing less impurities than the starting metal using commercial-grade zinc metal and industrial oxygen as starting materials.
SUBSTANCE: invention can be used in electronics, material science, instrument-making, metrology, information technology, chemistry, ecology, biology and medicine. Initial product of electric arc synthesis is separated into light and heavy fractions by distillation in "boiling layer" mode or by floatation. For "boiling layer" mode air is used as carrier-gas and is supplied at rate, which provides mode of laminar flow of light fraction. Sodium nitrate solution with specific weight 1.26-1.37 g/cm3 is used as floatation liquid. Heavy fraction is processed with concentrated hydrochloric acid and ultrasound, washed, dried and successively oxidised with air oxygen at 450 °C and 600 °C with intermediate processing with concentrated hydrochloric acid and ultrasound, washing and drying until constant weight is obtained.
EFFECT: reduction of process duration, improved quality of separated nanotubes due to reduction in them of metal and amorphous carbon.
4 dwg, 3 ex
SUBSTANCE: invention can be used for obtaining carbon nanotubes and nanofibres. Solid disperse catalyst is periodically loaded into reactor, gases are injected and subjected to contact with catalyst particles at the temperature of carbon nanomaterial synthesis. Loading of each following portion of catalyst is performed on the layer of growing nanomaterial. Alternate pressure of gaseous medium is created in reactor by injection of gases when pressure in reactor increases and their discharge, when pressure decreases. Stages of injection of gases into reactor and discharge of gases from reactor are performed by repeated periodical creation of vacuum in lock-chamber.
EFFECT: simplification of hardware process realisation, increased productivity due to uniform catalyst distribution.
2 cl, 2 dwg, 2 ex
SUBSTANCE: method involves mixing phosphates, calcium and silicon compounds, milling and mechanochemical synthesis, wherein the starting components used are disubstituted anhydrous calcium phosphate, annealed calcium oxide and amorphous hydrated silicon oxide with water content of less than 0.5 mol, with specific surface area of 200-450 m2/g in amount of not more than 1.2 mol silicon per elementary cell of hydroxylapatite; mechanochemical solid-phase synthesis is carried out in high-energy planetary mills with drum rotation speed of 1200-1800 rpm for 12-30 minutes. Calcium oxide is annealed preferably at temperature of 900°C for 5 hours.
EFFECT: invention enables to obtain a powdered nanocrystalline single-phase product for 30 minutes of solid-phase mechanical activation.
2 cl, 1 tbl, 6 ex, 7 dwg
SUBSTANCE: invention can be used in chemical industry and metallurgy. The method of producing molybdenum carbide nanoparticles involves dissolving molybdenum pentachloride in ethanol in ratio of 1:(1-3). Urea is added to the obtained solution. Annealing is then carried out in two steps. At the first step, heating is carried out in a vacuum at a rate of not more than 5°C/min to temperature of 430-450°C. At the second step, heating is carried out in a nitrogen atmosphere to temperature of 550-600°C, followed by holding at said temperature for 2.5-3 hours.
EFFECT: invention lowers the process temperature and enables to obtain molybdenum carbide particles with size of 5-10 nm.
2 dwg, 2 ex
SUBSTANCE: invention relates to the field of nanotechnology, and can be used to produce nanotubes and fullerenes. The carbonaceous material is evaporated in the volumetric thermal plasma, and condensed on the outer surface of the anode 2 and the inner surface of the cathode 3. A glow-discharge plasma is used, which is set by electrical voltage supply sufficient to break the inter-electrode gap between the coaxial hollow cathode 3 having a shape of a cup with a permeable bottom 4, and the anode 2 located with the ability to move axially. The carbonaceous material is fed through the permeable bottom 4 of the cathode 3 and is selected from the group consisting of methane, propane, butane for gaseous carbonaceous material or from the group consisting of crude oil, oil fuel, benzene, gas oil for liquid carbonaceous material. The bottom 4 is made in the form of a grid or a membrane.
EFFECT: invention enables to reduce the power consumption of the process, to broaden the types of the used hydrocarbon crude, to simplify the design of the device and to provide the ecological compatibility of the process and its high performance.
4 cl, 1 dwg, 2 ex
FIELD: process engineering.
SUBSTANCE: invention relates to power metallurgy, particularly, to production of metallic nano-sized powders.Initial powder of metal oxide compounds with particle size not exceeding 50 mcm is fed by carrier gas into reactor of gas discharge plasma. Initial material is heated to temperature exceeding that of oxides sublimation to evaporate metal and to reduce metal oxides in hydrogen flow or its mix with nitrogen or by argon. Metallic powder is isolated on cooling metal vapors by pulsating inert gas flow at gas flow rate of 1·10-6-1·10-3 m3/s.
EFFECT: ruled out or minimised agglomeration of condensed nano-sized pareticles.
7 cl, 3 ex
FIELD: process engineering.
SUBSTANCE: invention relates to physical chemistry and can be used for production of photon crystals with preset physical properties. Substrate with pre-applied silica microspheres is placed into reactor. Reactor chamber is evacuated to 10-4 torr. Substrate is heated to 192-230°C to feed precursor vapors at 45-56°C into reaction zone. Vapors are held for at least 1.5 s. Air is fed into reaction chamber to pressure of 10-2 torr. Reaction mix is held for, at least 2 seconds and reactor is evacuated to initial vacuum.
EFFECT: simplified process, expanded process performances due to production of preset size nanoparticles.
3 cl, 3 dwg
FIELD: medicine, pharmaceutics.
SUBSTANCE: group of inventions refers to medicine, particularly toxicology and radiology, to drug preparations based on antioxidant proteins and methods of using them. The pharmaceutical composition for treating toxic conditions wherein the therapeutic effect is ensured by the action of antioxidant, antimicrobial, antitoxic human lacroferrin protein on the human body contains non-replicating nanoparticles of human adenovirus serotype 5 genome with inserted human lactoferrin expressing human lactoferrin in the therapeutically effective amount in the body, and an expression buffer with the particle content not less than 2.33×1011 of physical particles per ml of the expressing buffer. The method of therapy involves administering the composition in the therapeutically effective dose of 7×1011 of physical particles to 7×1013 of physical particles per ml of the expressing buffer per an individual; the composition is administered intravenously.
EFFECT: invention provides the stable therapeutic effect after the single administration of the composition.
17 cl, 14 ex, 4 dwg
SUBSTANCE: ingot manufacturing method involves tempering of an ingot, multiple forging with series change of orientation axis through 90° at the temperature interval of 773-923 K with total true deformation degree of not less than 3 and further annealing at the temperature above isothermic forging temperature by 50 K during 1-5 hours.
EFFECT: obtaining an austenitic steel ingot with nanocrystalline structure and improved strength properties.
2 dwg, 1 ex
SUBSTANCE: invention relates to cold curing epoxide compositions and can be used in making structures, including large-sized structures, from polymer composite materials by vacuum infusion in engineering fields. The epoxide composition includes an epoxide base containing epoxy-diane resin, an active diluent and a curing system based on an amine curing agent and a surfactant, characterised by that the epoxy-diane resin used is a resin or a mixture of resins with molecular weight 340-430, the active diluent used has viscosity of up to 0.1 Pa·s, the amine curing agent is a mixture of a curing agent basedd on an aromatic amine and a cold curing catalyst, and the curing system further includes a heterocyclic imidazole-type compound and a nanomodifier. The technical result is preparation of a high-technology epoxy composition, curable without the need for additional heat and without a large exothermic effect, and characterised by improved physical and mechanical properties.
EFFECT: composition is characterised by high modulus of elasticity of 3,8-4,2 GPa, which allows its use in making deformation-resistant articles from polymer composite materials with higher structural strength.
7 cl, 3 tbl, 12 ex
SUBSTANCE: group of inventions refers to medicine, particularly to magnetic nanoparticles for treating and/or preventing cancer, prepared of ferric oxides or pure iron containing an oxide-containing layer, wherein at least one therapeutically active substance is bound to said particles. Releasing at least one therapeutically active substance is caused or initiated, or accelerated substantially by a variable magnetic field.
EFFECT: group of inventions provides reducing the uncontrolled release of the therapeutically active substances during nanoparticle delivery to cancer cells.
13 cl, 11 ex