Method of allocating concentrate of valuable metals contained in heavy oils and products of their processing
SUBSTANCE: presented method includes processing heavy crude oil with a low-temperature plasma generated by microwave (MW) electromagnetic radiation. The method is implemented as follows. Heavy crude oil is loaded to the heated reactor equipped with an electrode with a through-hole for supplying inert gas-argon. An inert gas is fed through the electrode, after which the power is turned on and the plasma is generated. At the tip of the electrode, a breakdown is initiated with further formation of gas bubbles, the temperature inside of which reaches 1500 K. The processing of crude oil is carried out for 2 minutes. Heavy crude oil is used as a processed sample with the density of 900 to 1100 kg/m3. A copper rod is used as a material for the electrode. The method allows to obtain a concentrate of valuable metals such as Ni, V, Mo, Co, Cu, Zn, and others contained in crude oil.
EFFECT: production of a solid product from heavy crude oil and liquid hydrocarbons with a reduced metal content.
2 cl, 3 tbl, 3 ex, 1 dwg
SUBSTANCE: method includes water processing, leaching of phosphate with sulphuric acid solution with concentration 3-6 wt % with conversion of REE, calcium and thorium into leaching solution and with obtaining gypsum product, extraction of REE, calcium and thorium from leaching solution by sorption with sulphoxide cationite. Leaching is carried out with sulphuric acid solution and L:S not less than 1.4:1. Sorption of REE, calcium and thorium is realised in stages. At first stage leaching solution is passed through cationite before beginning of REE breakthrough into forming primary depleted sulphuric acid solution. After that, desorption of calcium and thorium from saturated cationite with primary depleted sulphuric acid solution is carried out with obtaining primary calcium-thorium-containing strippant. At second stage remaining leaching solution is passed through cationite before REE breakthrough into secondary depleted sulphuric acid solution, which is applied for calcium and thorium desorption with obtaining secondary calcium-thorium-containing strippant. Then desorption of REE with solution of ammonium nitrate and precipitation of REE from strippant at pH 7.35-7.5 are realised.
EFFECT: obtaining non-radioactive rare earth concentrate with extraction of REE from phosphogypsum into non-radioactive concentrate and with reduction of applied sorbent consumption.
6 cl, 5 ex
SUBSTANCE: ferrous ore is subjected to intensive machining to destruct mineral aggregates and for deep opening of the phosphate minerals of rare-earth minerals, yttrium and thorium, then ore is leached by solutions of the nitric acid at 180-240°C. Under such conditions the phosphate minerals of the listed elements completely decompose and go into solution, and escaping phosphoric acid is adsorbed on iron oxides (3+) with generation of the insoluble compounds, thus ensuring creation of the dephosphorized nitrate solutions suitable for extraction processing. Increased temperature ensures hydrolysis of the ferrous nitrates even in strongly acidic (nitric) solutions.
EFFECT: simplified method of difficult chamoisite processing using hydrometallurgy method ensuring separation to solution per single operation of the rare-earth metals, yttrium and thorium, and to separate them from phosphorus and iron, and decreasing of chemicals consumption due to exclusion of the alkali treatment.
2 cl, 1 tbl, 7 ex
SUBSTANCE: invention relates to rare and radioactive element technologies and can be used to obtain concentrates of rare and rare-earth elements from monazite. The method of processing monazite concentrate includes treating the feed stock with a mixture of sulphuric acid and ammonium fluoride at 200-230°C for 30-40 min, purifying the obtained product from phosphate and fluoride products by sublimation, water leaching sulphates of rare-earth elements, neutralising the solution with barium chloride, selectively separating the thorium, uranium, iron and rare-earth product, wherein separation of the rare-earth product is carried out through a step of precipitating double salts of rare-earth elements with ammonium sulphate, followed by conversion into nitrates of rare-earth elements through a calcination step, dissolving in nitric acid and solvent refining from thorium impurities.
EFFECT: invention provides high degree of extraction and purity of the rare-earth product.
3 cl, 2 dwg, 3 ex
SUBSTANCE: in the process of flotation-extraction of samarium (III) as the organic phase applied is isooctyl alcohol, and as a collector - SAS of an anion type sodium dodecylsulphate in the concentration, corresponding to the reaction stoichiometry: Sm+3+3NaDS=Sm(DS)3+3Na+, where Sm+3 is the samarium (III) cation, DS- is dodecylsulphate-ion. Flotation-extraction is realised at pH=7.5-8.5 and a ratio of organic and water phase being 1/20-1/40.
EFFECT: increased degree of samarium extraction due to the formation of strong complexes of samarium cations with sodium dodecylsulphate, transferred into the organic phase.
1 dwg, 1 ex
SUBSTANCE: invention relates to a method of extracting europium (III) cations from a weak or technogenic raw material by liquid extraction. The method of extracting the europium (III) cations includes liquid extraction from water-salt solutions with the application of isooctyl alcohol as an extragent. Before extraction into the water-salt solution added is SAS of an anion type, which is represented by sodium dodecylsulphate, with the formation of europium dodecylsulphate solvate for its transportation through a water and organic phase. Sodium dodecylsulphate is added into the solution in a concentration, corresponding to stoichiometry of a reaction: Eu+3+3C12H25OSO3Na=Eu[C12H25OSO3]3+3Na+, where Eu+3 is the europium cation, C12H25OSO3Na is sodium dodecylsulphate, Eu[C12H25OSO3]3 is the solvate. Liquid extraction is realised at pH=3.0-6.0.
EFFECT: increase of the europium extraction degree due to the formation of strong solvates of europium and extraction of the europium cations from water solutions of its salts.
SUBSTANCE: invention relates to a processing method of Domanic formations. The method involves agitation neutralisation - decarbonation by treatment with pulp of crushed ore or by a neutraliser of a hardened solution cleaned from aluminium so that a productive solution and decarbonated cake is obtained. Then, a clay product is leached from decarbonated cake in the form of nepheline with the hardened solution so that pulp sulphate is obtained. After that, autoclave oxidation leaching of uranium, vanadium, molybdenum and rare-earth metals is performed from a solid phase of pulp sulphate in presence of substances that oxidise vanadium selectively so that a hardened solution, which contains aluminium, vanadium, uranium, molybdenum and rare-earth metals, and insoluble residue is obtained. Gold and platinum is extracted from the insoluble residue. Potassium aluminium sulphate alum is extracted from the hardened solution. Uranium and molybdenum and vanadium and rare-earth metals are extracted from the productive solution.
EFFECT: extraction of aluminium, uranium, vanadium more than 90%, reduction of emissions to atmosphere due to complex use of residues of Domanic formations.
16 cl, 1 dwg, 1 ex
SUBSTANCE: invention relates to a method of extracting rare earth elements (REE) from extraction phosphoric acid (EFA). The method includes the application of an anionite of a phosphate-mixed form in a cyclic process of sorption-desorption. Desorption at all, except the last, stages-cycles is carried out until a ratio of initial (C0) and final (C) concentrations of the acid corresponds to the condition 0.25≤C/C0≤0.75, and at the last one until the concentration of desorbed phosphoric acid is not more than 0.15 mol/l. Passing of EFA through a column with an anionite is carried out at each stage of the cycle from bottom to top to a breakthrough, corresponding to a relative concentration, corresponding to the condition 0.25≤C/C0≤0.75. An obtained enriched in REE solution is directed to the extraction of a solid REE concentrate. Desorption at each stage of the cycle is carried out with diluted phosphoric acid with obtaining at all, except the last one, stages-cycles of a purified phosphoric acid desorbate and a last stage-cycle desorbate - with a relative concentration of phosphoric acid, corresponding to the condition 0.25≤C/C0≤0.75, and with the concentration lower than 0.25 mol/l. The latter is returned to the desorption stage.
EFFECT: increased extraction of the REE concentrate.
7 cl, 8 dwg, 4 tbl, 6 ex
SUBSTANCE: method includes leaching using water-soluble fatty carboxylic acids with less than 3 carbon atoms per molecule as the leaching agent. The desired products to be extracted are then separated from the obtained solution. Leaching is carried out with addition of red mud in portions while controlling pH and ceasing addition of the red mud upon achieving pH 2.3-3.8. After leaching, the solution is held at a given leaching temperature for at least one hour.
EFFECT: high degree of extracting valuable components and high efficiency of the process by preventing precipitation of finely dispersed aluminium hydroxide.
SUBSTANCE: invention relates to method of obtaining compounds of rare earth metals (REM) in complex processing of phosphate raw material, in particular apatites. Claimed is method of sulphuric acid decomposition of REM-containing phosphate raw material with concentration of REM in phosphogypsum. Method includes addition of sodium salt, potassium salt or their mixture. Sodium salts are added in amount 0.25-5.0 kg in terms of Na2O, potassium salts - in amount 0.25-5.0 kg in terms of K2O, and their mixture - in amount 0.25-5.0 kg in terms of Na2O and K2O per 1 kg of REM in terms of REM oxides in composition of phosphate raw material.
EFFECT: increased degree of REM concentration in phosphogypsum due to increase of REM transition into phosphogypsum to 98%.
2 cl, 6 ex
SUBSTANCE: invention refers to liquid extraction processes, in particular to obtainment of rear-earth metals concentrates, in non-ferrous and ferrous metallurgy, during utilisation of chemical and metallurgical production waste and for purification of shaft, mine and industrial waste water. The method of rear-earth metals removal from diluted water acid solutions involves consecutive steps of liquid-phase extraction of rear-earth metals to organic phase and re-extraction of rear-earth metals from organic phase by settlement of rear-earth metals to solid phase in the form of slightly soluble salt of strong acid.
EFFECT: providing efficient removal of rear-earth metals without neutralising of acid containing in organic phase and use of cheap commercially available reagents.
7 cl, 6 ex
SUBSTANCE: invention relates to metallurgy and can be used for out-of-furnace production of metals and alloys in the oxidic metallothermic processes proceeding due to heat emission in chemical reactions of reduction of metals from oxides or concentrates. In the method the exothermic furnace charge is loaded on the gas-permeable compacted fire-resistant backfill on the bottom of the fore-hearth and into the thin-walled cylinder which is pre-installed in the shaft of melting furnace coaxially to its punched walls. The space between the thin-walled cylinder, walls of the fore-hearth and the furnace shaft is filled up with granular gas-permeable fire-resistant material, then the thin-walled cylinder separating the metallothermic furnace charge and granular fire-resistant material is removed, furnace charge is filled up from above with also granular gas-permeable fire-resistant material, the beginning of exothermic reaction is initiated during which the drainage removal of gases through gas-permeable fire-resistant material and the punched horn walls is performed. The melting furnace is fitted with a vacuumiser and the gas-tight fire-resistant gasket separating gas-permeable fire-resistant material of furnace shaft and the fore-hearth the internal diameter of which is equal to that of the named thin-walled cylinder, and external diameter is equal to that of the bearing flange of the furnace shaft, while the walls of the fore-hearth are made with holes, and on its internal surface the metal grid is fixed, and the fore-hearth is interfaced with the vacuumiser and tightly connected to the furnace shaft housing along the perimeter through the named gas-tight gasket to provide the conditions of pumping out of metal directly into the fore-hearth volume.
EFFECT: invention allows to increase density of metal structure and to reduce in it the concentration of residual gases by vacuumising of metal at the final stage of melting.
2 cl, 5 dwg, 1 tbl
SUBSTANCE: method includes formation of the melted zone 12 between polycrystalline billet 5 and side surface of the horizontally located cylindrical seed crystal 6, holding of the melted zone for time period necessary to stabilise the thermal conditions of growth of monocrystal disk, melt directing to side surface of the seed crystal during movement of the seed crystal in vertical direction of monocrystal growth and seed crystal rotation in direction of crystallization front attack, at that during growth the current diameter of the monocrystal disk is automatically measured, based on the measurement results the speed of the billet 5 and seed crystal 6 movement and rotation is set, the seed crystal movement during growth is performed continuously for the entire process of growth of the monocrystal disk. The method is implemented in the device including growth chamber 1 with top 3 and bottom 2 stocks for movement of the respectively polycrystalline billet 5 and seed crystal 6, additional drive 4 for liquid metal directing from the melting zone to the side surface of the seed crystal 6, installed on shaft 7 of the additional drive 4. The device additionally has system of automatic control of polycrystalline billet and seed crystal rotation and movement connected with bottom 2 and top 3 stocks, and with additional drive 4. The bottom stock 2 is mechanically connected with the additional drive 4 converting rotation axis of the bottom stock 2 from vertical position to the horizontal.
EFFECT: assurance of stability growth of monocrystal disk with large diameter, and increased output of suitable products by means of state stabilization of the melted zone during growth.
5 cl, 3 dwg
SUBSTANCE: proposed method comprises grinding of concentrate and pyrometallurgical break-down of concentrate in two steps. At first step, sodium is subjected to carbothermic reduction from concentrate by sodium evaporation at the pressure p=10-50 Pa, temperature T=1000 K and carbon content with respect to concentrate mC=2.9 wt %. Sodium vapours are withdrawn from reaction volume and condensed at T=300 K. At second step, further carbothermic reduction of produced enriched concentrate is performed at p=10-50 Pa, temperature T=2000 K and carbon content relative to enriched concentrate mC=28 wt % with reduction of refractory metal oxides to carbides in condensed phase and transition of rare earth element oxides to gas phase. Said phase is withdrawn from reaction volume and condensed at T=300 K.
EFFECT: higher yield of sodium, rare earth elements and refractory metals without application of harmful reagents.
SUBSTANCE: invention 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.
EFFECT: providing effective opening of loparite concentrates with extraction of 99% of rare-earth metals to the solution.
SUBSTANCE: method of electron-beam melting of products from high-melting metals and alloys and device for the method's implementation are proposed. The above method involves arrangement of molten material inside replaceable shape-generating melting pot and installation inside cooled vacuum chamber of cathode assembly, anode and melting pot. The latter is fixed inside anode made in the form of a metal pipe and arranged axisymmetrically inside cathode assembly with system of annular focusing electrodes and thready annular cathode. Melting of material in melting pot or first of the bottom part, and then of the whole material is performed by moving anode or cathode assembly relative to each other along their vertical axis with formation of crystallisation zone of molten product at the pot bottom and by movement of zone of molten material upwards with velocity providing the formation of shrinkage hole in upper part of the product.
EFFECT: obtaining complex products of high strength; increasing the surface area of its carrying section.
7 cl, 2 dwg, 8 ex
SUBSTANCE: set of elongated rods is produced by fabrication of multitude of rods. Each rod is made by preparing at least one non-metallic preceding compound, by chemical reduction of preceding compounds for production of metallic material and by making compound of metallic material for fabrication of rod. The rod has length equal to length of the set. The set of rods can be used as consumable source material in melting and casting operations.
EFFECT: equal regulated length and similar controlled configuration of cross section of set of rods.
10 cl, 4 dwg
SUBSTANCE: invention relates to production of zirconium (hafnium) by magnesia-thermal reduction of its tetrachloride in reduction reactor. Proposed method comprises feeding solid tetrachloride into service bin for subsequent continuous feed into evaporator. Note here that feed of solid zirconium (hafnium) tetrachloride into said service bin is carried out by pneumatic transport means using dried inert gas fed from tight feeder so that constant solid residue of tetrachloride is left in service bin: H≥0.5D, where H is height of residue of loaded zirconium (hafnium) tetrachloride layer, D is service bin diametre. Inert gas used after pneumatic transport is forced back via pipeline into feeder.
EFFECT: better quality of produced zirconium/hafnium, higher efficiency.
SUBSTANCE: proposed method comprises placing mix material into autoclave, heating it, initiating reduction reaction by firing mix material, its melting to produce refractory metal ingot, and unloading finished product. Reaction mix material placed in autoclave, said material is heated directly in autoclave. Autoclave is placed in tightly closed pit representing a straight flow tube with running water to cool down autoclave housing before firing reaction mix material. Mix material is heated by autoclave housing heat. Note here that heating time interval is calculated allowing for time of heating autoclave, its transportation, cooling, and firing reaction mix with due allowance for recovery of the housing mechanical strength provided by cooling the housing and increasing gas pressure. Proposed device incorporates tightly closed vertical pit representing a straight flow tube with running water to cool down autoclave housing before firing reaction mix material. Metal tight tank is arranged in aforesaid pit, while its bottom part represent a cone with cover to remove reaction products.
EFFECT: reduced costs.
5 cl, 1 dwg
SUBSTANCE: device consists of retort-reactor and retort-condenser mounted above retort-reactor with it bottom up; retort-condenser is coupled with working cavity of retort-reactor and is equipped with water-cooled caisson. The retort-reactor has a false bottom on top covered with a sheet of a refractory metal inert to interaction with zirconium at temperature up to 1000°C. Also the device is equipped with a heat shield installed between connecting flanges of the retort-reactor and retort-condenser; the shield is furnished with a steam line and a branch for coupling with systems of vacuumising and inert gas filling. Additionally, the steam-line of the heat shield is made in form of a conic orifice with its point upward and with ratio of diametre at the point to diametre at the base within ranges from 0.2 to 0.7. Before input to the steam line on the side of the retort-reactor there is installed a tray forming a gap where steam flows through from the retort-reactor to the retort-condenser. A circular stop is secured in the working cavity of the retort-reactor adjoining the heat shield; the internal cavity of the circular stop is made in a shape of a conic orifice with its point upward to the bottom of the retort-condenser.
EFFECT: raised efficiency of device and upgraded quality of sponge zirconium.
SUBSTANCE: procedure consists in degreasing chips with water solution of detergent implementing ultra-sonic bath, in washing chips in hot water, in their drying and crumbling. Also before degreasing chips are crumbled and simultaneously sprinkled with water solution of detergent; degreasing is performed in the ultra-sonic bath where concentration of detergent is 10-40 g/l at temperature 50-65°C during 5-10 minutes. Upon sizing and/or magnet separation chips can be introduced into composition of alloys as addition to charge materials.
EFFECT: increased quality of metal produced out of metal chips, and its reduced prime cost.
4 cl, 1 tbl, 2 ex
SUBSTANCE: method of heap leaching of silicate nickel ores includes ore crushing, ore mix preparation with fluoride adding from the group: sodium silicofluoride, fluoric calcium, ammonium fluoride and/or ammonium hydrofluoride amounting 1.3-1.7 wt % (in terms of fluorine). Then the mix is balled by pelletizing using the concentrated sulphuric acid in the ratio S : L = (88.0-94.0): (6.0-12.0) as a binder. After pelletizing the pellets are laid in a heap and leached by sulphuric acid solution.
EFFECT: shortening time of leaching at high level of extraction of nickel, cobalt and magnesium, decrease of power and material inputs.
4 cl, 1 tbl, 2 ex