Method of producing titanium powder

FIELD: metallurgy.

SUBSTANCE: method involves loading sponge titanium into a retort, vacuuming and heating it in a vacuum, feeding hydrogen to the retort with hydrogenation of the sponge titanium while cooling the retort, extracting the hydrogenated sponge titanium from the retort, grinding it and sieving it into fractions, charging the crushed hydrogenated titanium powder in the retort, dehydrogenating it, cooling the retort and extracting the titanium powder. Hydrogen is fed into the retort at a speed of not more than 360 m3/hour per 1m2 of the retort section with the provision of an excess hydrogen pressure in the retort of not more than 44 kPa. The hydrogenated sponge titanium is ground in an argon atmosphere at an excess pressure of not more than 10-20 kPa, and the dehydrogenation is carried out by sealing the retort, evacuating it to a residual pressure of 0.01 kPa, heating and supplying argon at an overpressure of 10-30 kPa, wherein hydrogen released during dehydrogenation together with argon with a residual pressure of 0.01 kPa and a thermal aging is carried out for 3-5 hours.

EFFECT: production of titanium powder of a given shape, fragmentation, needle type, with a reduced content of gas impurities such as hydrogen, nitrogen, chlorine and oxygen is ensured.

2 cl



Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to a method of processing material which contains a mineral and/or a metal oxide/silicate obtained from a mineral or associated with a mineral. The method includes processing raw material by reacting a mineral and/or metal oxide/silicate obtained from the mineral or associated with the mineral with ammonium bifluoride of general formula NH4F·xHF, wherein 1<x≤5. The reaction product is an ammonium fluorometal compound, which is subjected to thermal treatment for thermal decomposition thereof to obtain an anhydrous fluoride.

EFFECT: rapid, cheap anhydrous process of producing anhydrous fluorides from natural minerals.

23 cl, 5 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: disclosed is a method of producing titanium via reduction thereof from a tetrachloride using a liquid tetrachloride and dispersed aluminium as a reducing agent. The process is carried out in the temperature range of -23°C to +137°C and weight ratio of the initial titanium tetrachloride to aluminium of not less than 5.27 to 1.00 with intense mixing. The system is kept in a pseudo-Newtonian liquid state by using highly dispersed initial aluminium and dispersed products - titanium and aluminium tetrachloride with relative excess of the liquid phase. An apparatus for implementing the method is a flat-bottom conical reactor mounted on a magnetic mixer and fitted with batchers for feeding tetrachloride and dispersed aluminium, as well as a device for separating suspensions of titanium, aluminium trichloride and titanium tetrachloride. The latter is returned to the reactor and solid phases are separated by sublimation and subsequent condensation of aluminium trichloride. Powdered titanium is fed for further processing.

EFFECT: simple technique owing to lowering of temperature.

2 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to layered fire-resistant furnace lining, used in the process of titanium ore dressing with formation of enriched with titanium oxide and iron oxide liquid slag, to degradation-resistant substance in presence of enriched with titanium oxide and iron oxide liquid slag, to method of obtaining thereof, and to preliminarily formed layered fire-resistant lining. Layered fire-resistant lining contains first layer, which contains alumina and zirconium dioxide, including approximately 90-99 wt % of alumina and approximately 1-10 wt % of zirconium dioxide of the total weight of the first layer, and the second layer, containing degradation-resistant substance in presence of enriched with titanium oxide and iron oxide liquid slag. The second layer is located between slag and the first layer, and the total content of calcium oxide, magnesium oxide, yttrium oxide and cerium oxide constitutes less than 1 wt % of the total weight of the fire-resistant mass.

EFFECT: improvement of lining properties.

11 cl, 6 dwg, 4 ex

FIELD: chemistry.

SUBSTANCE: installation includes tank for storing of titanium tetrachloride, group of placed in a line reactors connected to each other with inclined overflow pipes, thickener, tank for purified titanium tetrachloride and expansion bucket for solid residue. Each reactor is made with hermetic lid, with branch pipes for input and branch pipes for output of titanium tetrachloride. Mixer of propeller type, which consists of engine, drive and blades, is fastened on lid of each reactor. In first reactor heater is placed and second and the following reactors are equipped with diffusers. Diffuser is made in form of hollow cylindrical ring, placed coaxially with drives of mixers and rigidly fastened to lid of reactor and to mixer drive with holders. On external side of cylindrical ring ribs are rigidly fastened opposite each other in pairs. Branch pipe for supply of copper reagent is made in lid of second reactor.

EFFECT: increase of titanium tetrachloride purification quality.

8 cl, 3 dwg

FIELD: metallurgy.

SUBSTANCE: invention relates to production of metal titanium. This method comprises formation of initial stock composed of water suspension containing titanium compounds produced by introduction of titanium particles into preset water volume. Said initial stock is displaced through serial processing zones. Then said initial stock is transferred via consecutive processing zones wherein metal is reduced with the help of carbon contained in offgas fed to said working zones and by alternating spinning magnetic fields generated in said zones. Note here that obtained metal particles are precipitated with their accumulation and subsequent discharge of finished metal. Note here that this process is conducted at continuous processing of said stock. Process exploits water suspension wherein dispersity of particle as ore containing copper compounds makes 0.001-1.0 mm. Note here that magnetic fields are used, their intensity making 1·104-1·106 A/m, while frequency makes 40-70 Hz, quantity of fields makes 2 to 6. Finished metal is produced as titanium granules. Invention covers the device for process implementation.

EFFECT: lower costs, higher quality.

6 cl, 2 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: claimed is titanium-enriched residue after leaching of ilmenite with hydrochloric acid as raw material for obtaining titanium-containing pigment by means of sulfuric acid method. Titanium enriched residue consists of friable and porous residue, obtained after removal of iron from crystal lattice of ilmenite (FeTiO3) by leaching with hydrochloric acid, and metatitanic acid aggregates. Residue contains small amounts of retile and titanium augite, with larger part of constituting it TiO2 being amorphous. Solid substance, obtained after leaching, is dried with formation of titanium-enriched residue. Residue is soluble in sulfuric acid, with water content in it constituting not more than 20%, with residue representing white, light-yellow or light-gray particles or powder, in which content of amorphous TiO2 constitutes 65-97%, the total content of iron constitutes not more than 8%, and specific weight of residue constitutes 2.9-3.6.

EFFECT: obtaining titanium-containing pigment by means of titanium-enriched residue, which makes it possible to efficiently recycle finely disperse ilmenite of the region, obtain solution of titanium sulfate with super low ratio of iron to titanium dioxide (Fe/TiO2) and double productivity of recycling equipment.

7 cl, 6 dwg, 12 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: invention relates to method of titanium obtaining. Method includes presence of titanium oxide with the level of admixtures of at least 1.0 wt %, taken in form of ore or ore concentrate. After that performed is reaction of titanium oxide with formation of titanium oxycarbide. After that, electrolysis of titanium oxycarbide in electrolyte is carried out, with titanium oxycarbide being made as anode. Then, extraction of refined metal titanium from cathode in electrolyte, with the level of admixtures being 0.5 wt %, is carried out.

EFFECT: realisation of method of refining titanium from ore.

FIELD: metallurgy.

SUBSTANCE: proposed method comprises mixing of initial titanium-bearing slag with soda ash, mix sintering and leaching of produced cake, first, in water for production of iron-titanium-bearing precipitate and, then, in muriate for production of titanium-bearing precipitate. Then, pulp is filtered to separate the precipitate to get titanium dioxide concentrate. note here that initial slag sintering with soda ash occurs at 900°C and Na2CO3:slag ratio equal to (0.98-1.15):1. Cake sintering in water is conducted to transfer sodium silicate to solution while titanium dioxide concentrate is made by calcination of precipitate resulted from hydrochloride-acid treatment. Note here that said initial titanium slag represents that of reducing fusion of ilmenite.

EFFECT: simplified process, higher pulp filtration rate.

2 cl, 1 tbl

FIELD: metallurgy.

SUBSTANCE: treatment method of a mixture of niobium and/or tantalum and titanium oxides for separation of niobium and/or tantalum from titanium involves dilution of the mixture at heating in the hydrofluoric acid solution so that a fluoride solution is obtained. A tetramethylammonium hydroxide solution or its salt is added at mixing to the obtained fluoride solution and evaporated to dryness. Formed complex fluorides of niobium and/or tantalum and tantalum with a tetramethylammonium cation are treated by low-molecular aliphatic ketone for extraction of complex niobium and/or tantalum fluorides in the form of tetramethylammonium hexafluoroniobate and/or hexafluorotantalate to the solution. Tetramethylammonium hexafluorotitanate is obtained in the deposit.

EFFECT: increasing separation degree of niobium or tantalum from titanium; simplifying the method owing to reducing the number of stages and the time required for the separation process; reducing volumes of processed solutions.

8 cl, 9 ex

FIELD: metallurgy.

SUBSTANCE: method involves carbothermal vacuum treatment. Prior to carbothermal treatment, a charge is prepared, which consists of perovskite concentrate and carbon-containing material in the ratio suitable for formation of calcium carbide, and titanium carbides and oxycarbides. Opening is performed in one unit in two stages. At the first stage, carbothermal treatment is performed at the temperature of 1100-1300°C and residual pressure of 10-100 Pa so that solid mixture of calcium carbides and titanium carbides and oxycarbides is obtained. The second stage is performed at the temperature of 1400-1500°C and pressure of 5-10 Pa for dissociation of calcium carbide and its stripping so that elementary calcium and carbon is obtained and with concentration in the residue of precious components of titanium, tantalum, niobium and rare-earth metals, which are contained in perovskite concentrate and are subject to chlorination.

EFFECT: improving specific productivity, reducing technological operations and use of a cheap reducing agent - carbon-containing materials.

1 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: fine silver powder is produced by electrolysis of silver nitrate solution with concentration of silver of 15-60 g/dm3 and free nitric acid of 5-20 g/dm3 at constant current density of 1.5-2.0 A/dm2. Titanium rods are used as cathodes while silver plates make anodes.

EFFECT: particles of silver powder sized to 1-20 mcm.

1 tbl, 3 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to powder metallurgy. Proposed method comprises electrolysis of metal salts solution with cathodic reduction of metal ions under conditions of plasma. Electrolysis is conducted with the use of anode as the plate and cathode as metal wire placed in glass tube at the voltage not over 40 V. Plasma originates in the electrolyte volume nearby cathode working surface.

EFFECT: higher quality of metal powder.

4 ex

FIELD: process engineering.

SUBSTANCE: invention relates to production of ultra-dispersed zinc powder. This process comprises zinc wire feed to continuous laminar gas flow and heating it in HF field of counter-current inductor to fusion point. Fused drops are formed at wire end suspended in inductor field. Saud fuse drop is evaporated by said laminar gas flow with vapour condensation to metal zinc particles. Said particles are discharged, cooled and caught by filter. Said laminar gas flow represents a downstream reducing agent gas flow. Said reducing agent consists of hydrogen or its mix with inert gas to allow reduction of refractory zinc oxide to metal on drop surface.

EFFECT: continuous production of said powder in free bulky state.

6 dwg, 5 ex

FIELD: metallurgy.

SUBSTANCE: powder synthesis is performed in a sealed vessel in argon environment under temperature of 850 K. Reaction mixture is molten salts containing the following, wt %: neodymium 24-26, nickel 23, eutectic of lithium chloride and potassium chloride - the rest. Neodymium is introduced in reaction mixture resulting from corrosion of massive metal in molten salts. Reaction mixture is exposed under 850 K for 2 hours, and then temperature is increased to 1170 K, and it is exposed for 3 hours. Alloy is subjected to hydrotreating under salts dissolution in water, and powder NdNi5 is dried under temperature below 320 K in vacuo.

EFFECT: intermetallic compound powder is characterised by high pureness, high sorption properties, capability of reversible absorption of hydrogen great quantities.

1 dwg

FIELD: metallurgy.

SUBSTANCE: invention relates to hydrometallurgy of lanthanides, particularly, to crystalline nanopowders of lanthanide oxides. Proposed method comprises deposition of lanthanide salts from nitric solutions of solid oxalic acid at continuous introduction of polyacrylamide, its separation, flushing, drying, heat treatment of produced sediment and subsequent treatment in weak alternating magnetic field at 20-50 Hz and with amplitude of 0.05-0.1 tesla.

EFFECT: nanosized particles with uniform grain sizes, higher water resistance.

1 dwg, 1 tbl, 1 ex

FIELD: process engineering.

SUBSTANCE: invention relates to powder metallurgy, particularly, to materials intended for production of electrolytic metal powders. It can be used in production of catalysts, electroplating and electronics. Cathodic reduction of metal ions from metal salt solution is carried out in electrolytic cell with rotary cathode and anode or insoluble anode. Cathode is composed of a rod with partially (90-99%) isolated surface. Cathodic reduction is executed at current density from 100 A/dm2 to origination of electrolyte plasma and metal salt concentration over 100 g/l to saturation.

EFFECT: higher process efficiency at high yield and quality of powder.

3 ex

FIELD: metallurgy.

SUBSTANCE: set of invention relates to powder metallurgy. Proposed method comprises feed of aluminium powder and primary active gas to prechamber. These are mixed and ignited in said prechamber to change aluminium over in gas phase by self-sustaining exothermal reaction. Formed mix is fed into primary combustion chamber for afterburning of metal in gas phase at feed of secondary active gas, the air, and production of condensed combustion products. Prechamber walls are cooled down to rule out sticking of condensed phase thereto by feeding of gas chemically neutral to aluminium. Distilled water is fed into primary combustion chamber for cooling purposes. Produced condensed combustion products along with distilled water are fed into pickup device to cool formed suspension of said condensed products so that nanodispersed aluminium oxide powder can be isolated therefrom. A portion of said suspension is retuned to said pickup device after extra cooling. Invention proposes also the device to this end.

EFFECT: efficient and stable process.

5 cl, 1 dwg

FIELD: metallurgy.

SUBSTANCE: proposed method comprises heating of metal uranium in evacuated reaction vessel at residual pressure of 10-1-10-2 mmHg and 250-300°C with subsequent feed of hydrogen to 750-800 mmHg. Uranium hydration is performed for time interval defined by preset formula. Reaction vessel with produced uranium hydride powder is subjected to evacuation another time at 220°C to residual pressure in reaction vessel of 10-1-10-2 mmHg. Nitration of produced uranium hydride is made in nitrogen flow at 250-300°C Pressure in reaction vessel is adjusted from 1 to 800 mmHg depending upon the change in area of powder reaction surface.

EFFECT: increased dispersion of uranium nitride powder, accelerated powder production.

2 cl, 1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to production of gallium nitride and can be used in electronic, aerospace, hard alloy, chemical branches of industry to obtain highly pure nitride, applied for manufacturing products, which possess high luminescent properties, chemical and radiation stability, thermal stability, stability in aggressive media, stability of physical properties in wide ranges of temperature. Method of obtaining gallium nitride powder includes: preparation of exothermal mixture, consisting of element to be nitrided, gallium, inorganic azide - sodium azide and galloid salt - ammonium fluoride or ammonium chloride, and ignition of mixture in nitrogen environment under pressure, with obtained powder being used for preparation of exothermal mixture with sodium azide and galloid salt, carrying out four-fold synthesis and each time exothermal mixture is prepared from powder, obtained at the previous stage, with sodium oxide and galloid mixture.

EFFECT: invention provides final product output about 100%.

1 tbl, 2 ex

FIELD: process engineering.

SUBSTANCE: invention relates to production of powders for microwave hardware and micro optics. Proposed method comprises preparation of water solutions of yttrium (III) and iron (III) salts. First, precipitator agent, a highly-basic gel anionites hydroxide AB-17-8 is brought in contact with the solution of yttrium (II) salt at the room temperature for 60 minutes. Then, the solution of iron (III) salts id added. Precursor product is settled from obtained solution and separated therefrom, dried and annealed at, at least 700°C.

EFFECT: nano-sized iron-yttrium garnet powder produced without use of aggressive media, high temperature and pressure.

4 dwg, 3 ex

FIELD: powder metallurgy, namely production of finely dispersed titanium powder.

SUBSTANCE: method comprises steps of hydrogenating initial titanium; disintegrating titanium hydride; heat decomposition of titanium hydride in vacuum and disintegration of formed cake. Heat decomposition is performed by several stages while realizing additional disintegration of cake between said stages. Before hydrogenating initial titanium, subjecting it to thermal activation at temperature 400 - 650°C. Hydrogenation is realized till providing content of hydrogen 440 - 468 cm3 per 1 g of titanium. Titanium hydride is disintegrated till achieving specific surface at least by 2 times exceeding that of produced titanium powder. Heat decomposition of titanium hydride is realized at least by two stages. Additional disintegration of cake is realized at residual content of hydrogen in range 100 - 380 cm3 per 1 g of titanium. According to invention residual content of hydrogen in powder is no more than 4 cm3 per 1 g of titanium. Yield of ready product consists at least of 94% of initial titanium mass; size fraction of titanium powder particles is less than 40 micrometers; specific surface measured according to standard method is in range 0.8 - 1.5 m2/g.

EFFECT: improved quality parameters of fine titanium powder.

2 cl, 1 ex