Method for opening perovskite concentrate. RU patent 2507278.
 Phosphosemihydrate processing method / 2507276Invention refers to processing of freshly obtained phosphosemihydrate and can be used to obtain concentrate of rare-earth elements (REE) and gypsum product for construction materials. Phosphosemihydrate is processed with water solution containing fluorine-ion. Sulphuric acid leaching is performed with displacement and separation of the water solution containing fluorine-ion, as well as with conversion of REE and impurity components to a leaching solution and production of a phosphosemihydrate layer saturated with a sulphuric-acid solution. Then, water displacement of the remaining amount of sulphuric acid solution is performed so that washed phosphosemihydrate and a leaching solution is obtained Phosphosemihydrate is neutralised with a calcium-containing reagent so that a gypsum product is obtained. Rare-earth elements and impurity components are extracted from the leaching solution by sorption using sulphoxy cationite so that a lean sulphuric-acid solution is formed; REE and impurity components are desorbed from saturated cationite by its processing with an ammonium sulphate solution so that a strippant is obtained; REE and impurity components are deposited from the strippant with an ammonium-containing precipitator in two stages and REE deposit is separated. |
 Method for opening loparite concentrates / 2506333Invention refers to metallurgy of rare metals. A method for opening loparite concentrates involves preliminary machining of loparite concentrates and further treatment of activated loparite concentrates with 30% of HNO3 solution at the temperature of 99 °C. To further treatment there subject are activated loparite concentrates with double amount of energy of variation of loparite crystal lattice parameters of at least 73 kJ/mole and with stored total amount of energy, which corresponds to surface of areas of coherent dissipation and microdeformations with at least 9.5 kJ/mole of loparite. |
 Method of processing phosphogypsum / 2504593Method of processing phosphogypsum involves step-by-step agitation sulphuric-acid leaching of rare-earth metals and phosphorus while feeding sulphuric acid to the head step, using the obtained leaching solution of the head step at subsequent leaching steps, separating the undissolved residue from pulp of a tail step and washing with water, treating the leaching solution of the tail step to obtain a mother solution, using the mother solution and the washing solution for leaching. Leaching of the rare-earth metals and phosphorus at the second and subsequent steps is carried out from a mixture of phosphogypsum and the leached pulp from the previous step. Sulphuric acid is fed to the head leaching step in an amount which enables to extract rare-earth metals and phosphorus into the solution at the head step and subsequent steps at pH values at the tail leaching step not higher than pH at the onset of precipitation of rare-earth metal phosphates. The tail step for leaching rare-earth metals and phosphorus is carried out while simultaneously treating the leaching solution by extracting rare-earth metals by sorption with a cationite. The rare-earth metal-saturated cationite is separated from the mother pulp and taken for producing a rare-earth metal concentrate. A portion of the mother solution is pre-purified from phosphorus by precipitation thereof with a basic calcium compound. The obtained phosphorus-containing precipitate is fed for recycling. |
 Plasma-carbon production method of rare-earth metals, and device for its implementation / 2499848Method involves carbon thermal reduction of oxide compound of rare-earth metal in vacuum so that powder of rare-earth metal carbide, which is free from residues of oxygen impurity, is obtained. Then, it is cooled down and mixed with high-melting metal powder in the ratio that is sufficient for performance of exchange reactions between rare-earth metal carbide and high-melting metal, and mixture is heated with hot volumetric plasma discharge to the temperature of ≥1800°C. With that, evaporating rare-earth metal is collected on condensers and hard-alloy carbide of high-melting metal is obtained. The device includes a vacuum system, cathode and anode assemblies arranged concentrically in the chamber, and a steam line and a condenser-cooler, which are coaxial to them. With that, an internal electrode represents an anode of high-current vacuum plasma discharge burning in an annular discharge cavity formed with coaxial cylindrical electrodes. The anode is made from high-melting electrically conducting material in the form of a crucible having a capacity, and a thin-wall cathode enveloping it, outside which there located is a starting resistance heater, is also made from high-melting electrically conducting material, for example tungsten, tantalum or graphite. |
 Cerium extraction method / 2495147Cerium extraction is performed after preliminary preparation of a catalyser. Crushing of the used catalyser is performed. Crushed catalyser is subject to annealing at the temperature of 650-800°C during 3-6 hours. After annealing the catalyser is cooled down to room temperature and cerium compound is extracted by dilution of ignited catalyser in concentrated hydrochloric acid. Obtained solution with suspended particles of cerium dioxide is heated to boiling, exposed at boiling temperature of 100-110°C during 30-120 minutes and during 3-12 hours at temperature of 0-20°C so that a deposition is obtained. The obtained deposition is separated from mother solution by means of filtration by draining the solution from the deposition surface to a filter with the size of filtering material pores of not more than 2 mcm. Deposition on the filter is washed from iron compound and dried till constant weight of cerium dioxide. |
 Method of extraction of rich components from production solutions for processing of black-shale ores / 2493279Method includes sorption of rich components from production solutions by ion-exchange material counterflow under controlled pH of environment and oxidation-reduction potential Eh. Sorption is performed by ion-exchange materials in stages from production solutions containing uranium, molybdenum, vanadium and rare earth elements. At the first stage uranium and molybdenum are extracted by anion-exchange material sorption. At the second stage vanadium is extracted by anion-exchange material sorption with hydrogen dioxide available at Eh of 750-800 mV, pH of 1.8-2.0 and temperature of 60°C, at that vanadium sorption is performed till complete destruction of hydrogen dioxide and till Eh is below 400 mV. Then barren solutions are transferred to cationite at pH of 2.0-2.5 and Eh of 300-350 mV for extraction of rare earth elements. |
 Processing method of black-shale ores / 2493273Processing method of black-shale ores includes crushing, counterflow two-stage leaching by sulfuric acid solution upon heating, separation of pulps formed after leaching at both stages by filtration. Then valuable soluble materials are washed from deposit at the second stage with strengthened and washing solutions being produced, marketable filtrate is clarified at the first stage for its further processing. Ore is crushed till the size of 0.2 mm, leaching at the first stage is performed by cycling acid solution with vanadium under atmospheric pressure, temperature of 65-95°C during 2-3 hours, till residual content of free sulphuric acid is equal to 5-15 g/l. Leaching at the second stage is performed at sulphuric acid rate of 9-12% from the quantity of initial hard material under pressure of 10-15 atm and temperature of 140-160°C during 2-3 hours. Cake filtered after the first stage is unpulped by part of strengthened solution which content is specified within 35-45% of total quantity. |
 Processing method of black-shale ores with rare metals extracting / 2493272Processing method of black-shale ores with rare metals extracting includes leaching of ore by sulphuric acid solution with dilution of rare metals. Leaching is performed in autoclave by sulphuric acid solution consisting of free and combined sulphuric acid with ratio of H2SO4(free):H2SO4(comb)=2:1, and containing 25-45 g/l of iron sulphate, 70-90 g/l of aluminium sulphate and 0.5 g/l of nitric acid. At that the process is performed under pressure in autoclave equal to 10-15 atm with mixing at temperature of 140-160°C in concentration range of general H2SO4(gen) equal to 350-450 g/l under pulp density S: L=1:0.7-0.9, preferably 1:0.8, under constant oxidation-reduction potential Eh in the system equal to 350-450 mV during 2-3 hours till residual concentration of free H2SO4(free) is within 45-75 g/l. |
 Method of extracting rare-earth metals (rem) from phosphogypsum / 2492255Proposed method comprises REM and phosphorus leeching by sulfuric acid solution to obtain leaching solution and insoluble residue. Said insoluble solution is processed by calcium compound to pH over 5. PEM concentrate is extracted from said solution by crystallisation and fed to REM and phosphorus leaching stage. Prior to leaching phosphogypsum is subjected to flushing with water to obtain flushing solution containing REM and phosphorus. Said insoluble residue is flushed before processing by calcium compound. Obtained flushing solution is processed by calcium compound to produce pulp with pH not over that of REM phosphate precipitation beginning and combied with said flushing solution. REM is sorbed by cation exchangers and separated to desorb REM therefrom to produce desorbent and recovered cation exchanger. Said recovered cation exchanger is sent to REM sorption while desorbent is sent to REM concentrate production stage. Phosphorus and associated impurities are deposited from sorption mother pulp. Obtained pulp is separated in residue to be recovered and water phase to be used as circulating water. |
 Method of extracting rare-earth metals from phosphogypsum / 2491362Method includes leaching of rare-earth metals (REM) from phosphogypsum with 1-5% solution of sulphuric acid, REM sorption from leaching solution with cationite, REM desorption, precipitation of REM concentrate from desorbate, obtaining REM concentrate and mother liquor, which is used for REM desorption. Cationite after desorption is returned at sorption stage. Phosphor and fluorine are precipitated from mother liquor, phosphor -and fluorine-containing sediment are filtered and filtrate is used as return water in leaching. REM leaching and sorption are carried out simultaneously. Obtained pulp is filtered through mesh filter with separation of saturated REM cationite. After that, pulp is filtered with obtaining non-dissoluble residue and mother liquor of sorption. Before desorption cationite is treated with part of desorbate. |
| Combined carbothermic production of calcium from carbonate / 2501871 Proposed method comprises making the charge from calcium carbonate, primarily, from chemically deposited chalk or high-quality sifting in production of limestone and carbon, primarily from reused graphite, obtained at final stage of carbothermic process. Note here that starting charge is pelletised, placed in furnace and heated in vacuum in one unit at three steps. At first step, calcium carbonate is dissociated in the presence of carbon at 600-700°C for 2-4 hours and residual pressure of 40-50 Pa to remove carbon monoxide. At second step, calcium carbide (CaC2) is synthesized at 1400-1500°C and 100-150 Pa to remove carbon monoxide. At third step, calcium carbine is dissociated to produce elementary calcium and graphite at 1300-1400°C and < 10 Pa. |
 Calcium carbide / 2501733Method includes thermal processing of crushed limestone and coal with discharge of gaseous products, which are applied for production of carbonic acid. Thermal processing is carried out in one reactor. At the first stage in the process of introduction of raw material into reactor it is subjected to heating to 1000°-1200°C by transmission of heat from constructive elements of loading canal and by exposure of raw material to plasma beam in zone of free movement of raw material particles. Thermal processing of raw material is realised in atmosphere of carbon dioxide. Further synthesis of calcium carbide is realised at temperature, at least, 1700-1800°C by induction heating of reaction mass. Obtained calcium carbide liquid is discharged. Gaseous products, from which carbon oxide and carbon dioxide are separated, are discharged from upper part of reactor, and at least, part of discharged carbon dioxide is applied for filling loading canal. For production of carbonic acid volume of carbon dioxide, remaining after filling loading canal and entire volume of carbon oxide are applied. |
| Plasma-carbon production method of rare-earth metals, and device for its implementation / 2499848 Method involves carbon thermal reduction of oxide compound of rare-earth metal in vacuum so that powder of rare-earth metal carbide, which is free from residues of oxygen impurity, is obtained. Then, it is cooled down and mixed with high-melting metal powder in the ratio that is sufficient for performance of exchange reactions between rare-earth metal carbide and high-melting metal, and mixture is heated with hot volumetric plasma discharge to the temperature of ≥1800°C. With that, evaporating rare-earth metal is collected on condensers and hard-alloy carbide of high-melting metal is obtained. The device includes a vacuum system, cathode and anode assemblies arranged concentrically in the chamber, and a steam line and a condenser-cooler, which are coaxial to them. With that, an internal electrode represents an anode of high-current vacuum plasma discharge burning in an annular discharge cavity formed with coaxial cylindrical electrodes. The anode is made from high-melting electrically conducting material in the form of a crucible having a capacity, and a thin-wall cathode enveloping it, outside which there located is a starting resistance heater, is also made from high-melting electrically conducting material, for example tungsten, tantalum or graphite. |
| Method of processing kyanite concentrate / 2489503 Method involves mixing a concentrate, a carbonaceous reducing agent and a pore-forming additive in form of ammonium sulphate, pelletising the obtained mixture, firing and holding at maximum temperature with reduction of silicon dioxide to a gaseous monoxide, crushing the obtained sinter, treatment thereof with ammonium bifluoride and calcining the reaction mass to obtain an aluminium-containing product, wherein ammonium sulphate is taken in an amount of 10-20% of the mass of the concentrate; before pelletising, the mixture is milled to obtain particles with size of 50-75 mcm in amount of at least 80%; the mixture is fired at temperature of 1690-1750°C; ammonium bifluoride is taken in amount of 0.4-14% of the mass of the sinter; and the reaction mass is calcined at 700-900°C. Before treatment with ammonium bifluoride, the sinter can be treated with 10-20% hydrochloric acid. The degree of extraction of aluminium oxide from the concentrate is increased by 1.3-9.9%. Content of aluminium oxide in the end product reaches 97.7% with content of silicon oxide impurities of 0.13-1.0%. |
 Method of processing solid or melted substances / 2484152Solid or melted substances are loaded on graphite body heated, at least, partially, inductively. Reducing agents are introduced therein, other than graphite carbon to collect flowing reduced and/or gasified melt. Note here that reducing agents are introduced along with solid or melted loaded particles. Said reducing agents represent natural gas, coal dust, brown coal dust, hydrocarbons, hydrogen, carbon oxide and/or ammonia to be introduced together with steam, oxygen, carbon dioxide and/or halogens or halogen hydrides. |
 Reducing method of metals from oxides / 2476035Reducing method of metals from oxides refers to reducing technologies of metals from non-organic oxides, at which preparation of homogeneous mixture is performed from ultradisperse powders of metal oxide and carbon, supply of prepared mixture under pressure to high-temperature zone in the well, which is formed with plasmatron jet, decomposition of metal oxide with formation of carbon dioxide that is removed through upper tuyeres of the well, and finished product is removed in the form of ultradisperse metal powder through tap holes in lower part of the well. |
| Procedure for depletion of solid copper-zinc slag / 2398031 Invention refers to procedure for depletion of solid copper-zinc slag. The procedure consists in supply of charge containing solid copper-zinc slag and carbonic reducer at weight ratio of slag to solid carbonic reducer 1: (0.06-0.1) into heated furnace. Also charge in the heated furnace is blasted with oxygen containing oxidant by means of upper not-immersed blast; consumption of oxygen-containing oxidant is determined by contents of oxygen in it from condition of 60-110 kg per ton of slag. Further there is produced a rich with copper phase and zinc is transferred into a gas phase. |
 Method of processing of iron-titanium concentrate / 2385962Method includes formation of charge consisting of concentrate and sodium carbonate by means of intergrinding of components and reduction of charge components at presence of taken with excess carbonaceous reducing material at temperature 850-1300°C. Additionally batch material reduction is implemented up to providing of content of metallic iron in the range of particles dimensions 10-300 mcm not less than 80%. Received partly reduced conservative mass, consisting of metalise phase containing main part of iron and vanadium and oxide phase, containing main part of titanium and vanadium, it is grinned up to size not more than 300 mcm. Then it is implemented leaching of vanadium from reaction mass and leaching residue is separated from vanadate solution. After separation residue of leaching is subject to gravitational separation in water flow with separation of metalised and oxide phases. Metalised and oxide phases are separately subject to wet magnetic separation for receiving of metallic iron and titanium oxide concentrate. Additionally wet magnetic separation is implemented in the range of field intensity 20-300 E. |
 Reduction method of metal and oxygen compositions / 2360982At reduction of metal and oxygen composition effect as reducer, herewith at first stage gaseous CO is passed into reaction chamber, containing specified composition of metal and oxygen. In conditions, providing conversion of CO into solid carbon and carbon dioxide, formed solid carbon is introduced into metal and oxygen composition. At the second stage solid carbon, which is introduced into metal and oxygen composition at the first stage, reduces metal and oxygen composition. Additionally at the second stage it is, at least, the first material- promoter, conducive reduction of specified metal and oxygen composition. Additionally the first material- promoter contains the first metal- promoter and/or composition of the first metal- promoter. |
| Method of tin manufacturing from cassiterite concentrate / 2333268 Invention concerns tin metallurgy field and can be used for tin manufacturing while treatment of cassiterite concentrates. Method of tin manufacturing from cassiterite concentrate with content of 35-50% SnO2 includes batch preparation by blending of tin concentrate with coal and flux additive. In the capacity of flux additive it is used sodium carbonate and sodium nitrate. Melting is implemented at temperature 850-1000°C during 2 hours. For mentioned concentrate it is kept up following mass ratio: concentrate : coal : sodium carbonate : sodium nitrate, equal to 1 : (0.2-0.25) : (0.12-0.15) : (0.06-0.08). It allows without concentrate pretreatment to provide tin manufacturing of 98% purity at less in comparison with tradition approach, temperature. |
 Tantalum-base alloy refining method / 2499065Tantalum-base alloy refining method involves vacuum electronic beam remelting in a horizontal crystalliser of the charge placed into it so that fumes of its metallic impurities are released on the surface that condenses them, and fumes of gas-containing impurities and production of a tantalum ingot by movement of an electronic beam from the beginning to the end of the crystalliser throughout the charge surface with its further switch-off. The charge contains metallic impurities of high-melting metals with the melting temperature close to that of tantalum. Vacuum electronic beam remelting is performed in two stages. The tantalum ingot produced at the first stage and containing impurities of high-melting metals is subject to electrochemical processing with release of tantalum-containing cathode residue that is subject to the second remelting stage so that an ingot of conditioned tantalum and fumes containing tantalum, which are returned to electrochemical processing, are obtained. From the first stage of the remelting process to the second one the specific power of an electronic beam is increased from 0.024-0.035 to 0.040-0.045 kW/mm2, and beam travel speed is decreased from 40-60 to 4-6 mm/min. |
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
The invention relates to metallurgy and relates to a method of opening concentrate in a vacuum. Invention can be used for opening of titanium concentrates, in particular , but primarily it is intended for opening concentrate when using co opening-up method in a vacuum.
The method involves blending materials ( concentrate and carbon) with the expectation of receiving restoration of a mixture of calcium carbide and titanium.
The method consists of two stages: the first stage is the formation of calcium carbide and titanium, with the subsequent decomposition of calcium carbide in the second stage of the metal calcium and carbon, both stages are held in one cycle in a single device.
There is a method of opening concentrate (Reznichenko V.A. Shabalin L.I. , deposits, metallurgy, chemical technology. - M: Nauka, 1986 270). The disadvantage of this method is the lack of comprehensiveness in smelting concentrate on pig-iron and slag: a significant part of niobium goes in cast iron, which requires additional operations to highlight it.
The disadvantage of this method is also dilution of the resulting slag at the expense of transition in it of all the calcium where its content is more than 25%. This requires the additional consumption of reagents (chlorine - 1,88/ton of slag, 100% nitric acid - 1,0 t/t slag) to highlight the further processing of slags on materials.
The disadvantage of this method is the low extraction showdown concentrate: titanium - 76%, niobium and tantalum - 42%.
The disadvantage of this method is also passing receiving a large number of little demand calcium nitrate CA(NO 3 ) 2 .
In the basis of the invention is to provide a method of processing concentrate at complex use of all valuable components of the original material, reducing reagent consumption, increase efficiency, reduce the number of process operations, reduce energy costs.
The problem is solved so that the method of combined processing concentrate in a vacuum original mixture prepared from concentrate and coal-bearing materials.
The problem is solved also. that the original mixture is prepared at once in such proportions, to the initial stage, at a temperature of 1100-1300 OC and residual pressure 50-100 PA obtain a mixture of solid products consisting of calcium carbide and carbide () titanium.
The problem is solved that at the second stage, in vacuum at a temperature of 1400-1500 OC and residual pressure of 5-10 PA calcium carbide dissociates in gaseous calcium with its subsequent condensation, and receive solid carbide () titanium, tantalum, niobium, rare earth metals and carbon.
The well-known technology of oxide materials ( concentrate or titanium slag) adding to the mixture of carbon-bearing materials at temperatures of 850-900 Celsius or pre oxide materials at temperatures to 400 deg C. The oxide () materials obtaining Plava chlorides of rare-earth metals and gaseous - titanium, tantalum and niobium.
The problem is solved that remained after the high-temperature processing and distillation product contains calcium carbides () titanium and other valuable components concentrate (REM. tantalum, niobium) and carbon. Such charge without prior preparation (add carbon containing materials suitable for the chlorination of the existing technology of obtaining the gaseous chlorides Piana, tantalum and niobium and Plava chlorides of rare earth elements contained within the original concentrate and concentrate in the solid residues at the second stage of the process after the distillation of calcium, and can be disposed of in the existing chlorine technology.
Table 1 shows concrete examples of the method.
Table 1Examples of the implementation of the combined method
No.Composition of charge
StageTemperature, C
Pressure, PA
Time, hour
Removing calcium, %
1і 3 +6S
1 1200 50-100 2-4 2 1400 5-10 4-6 95,2 2і 3 +6C, g.
1 1300 50-100 2-4 - 10%) 2 1500 5-10 4-6 96,3Method of tapping concentrate, including processing in a vacuum, characterized in that before the processing prepare a mixture consisting of concentrate and carbon-containing material in a ratio suitable for the formation of calcium carbide, carbide and titanium, the autopsy carried out in a single device in two stages, with the first stage processing is done at a temperature of 1100-1300 OC and residual pressure 10-100 PA with the formation of solid mixture of carbide calcium carbide and titanium and the second stage is carried out at a temperature of 1400-1500 OC and a pressure of 5-10 PA for the dissociation of calcium carbide and its distillation of obtaining elementary calcium and carbon and with the concentration of the residue contained in concentrate valuable components titanium, tantalum, niobium and rare earth metals, which subject to chlorination.