Method of chlorinating polymetallic niobium-tantalum containing raw material and device for implementing method

FIELD: chemistry.

SUBSTANCE: group of inventions pertains to the metallurgy of rare metals, in particular to the method of chloric decomposition of polymetallic niobium-tantalum containing raw material with obtaining of chlorides of niobium and/or tantalum and a device (chlorinator) for carrying out the chlorination process. The method involves chlorinating polymetallic niobium and/or tantalum containing materials in molten chlorides using chlorine, condensation and separation of the obtained pentachlorides of niobium and/or tantalum and chlorides of admixtures and tapping of the melt. Chlorination is done in the layer of melt with height of 500-1000 mm, containing iron chloride (up to 25% iron) and/or copper (up to 40% copper), as well as sodium chloride in quantity of not less than 1.2 kg for 1 kg of iron and not less than 2.2 kg for 1 kg of aluminium in the initial materials. The process is carried out at 550-850°C with consumption of chlorine of 1.7-2.2 kg for 1 kg of the initial materials. Tapping of the melt is done from the upper level through a tapping line. The chlorinator is water cooled, lined with graphite and equipped with a separation chamber, located in the upper part of the chlorinator. The ratio of the diameter of the chlorinator to the diameter of the separation chamber is equal to (2÷2.5):3, and the ratio of their heights is (1÷2):1. There is a removable graphite pipe for supplying chlorine, which runs through a water cooled connection pipe, tightly joined to the cover of the chlorinator, to the bottom of the chlorinator. Tapping of the melt is done from the upper level through a heated tapping line, lined with graphite.

EFFECT: design of a efficient method of chloric decomposition of polymetallic niobium-tantalum containing raw materials with obtaining of chlorides of niobium and/or tantalum.

2 cl, 1 dwg, 3 ex

 

The invention relates to the metallurgy of rare metals, in particular to method the chlorine decay niobium-tantalum raw materials and production of chlorides of niobium and/or tantalum and devices for the implementation of the chlorination process.

Chlorine is widely used in the industry are rare and non-ferrous metals due to its high reactivity and high efficiency separation and purification of chlorides with obtaining pure metals or their compounds.

However, successful chlorination of complex rare-metal mineral raw materials with gaseous chlorine is possible under certain conditions:

by maintaining chloretone temperatures of the order of 1000°C;

- the presence of some excess chlorine;

- introduction into the reaction zone of reductants such as coke;

- the use of complex and expensive devices - chlorinators.

Known chlorine method of processing of loparite concentrate. Chlorination is subjected briketirovannogo the charge in the mine chloretone or powder charge in molten chlorides. Chlorination in the melt has decisive advantages over chlorination in mine chloretone: continuity of the process, the possibility of automation, high velocity, and specific performance of the device, the lack of redistribution of briquetting and coking.

The total process chlorin is of loparite can be expressed by the schema:

[Ca(Na,Ln)][Ti(Nb,Ta)]O3+nC+mCl2→TiCl4+NbCl5+TaCl5+NbOCl3+LnCl3+CaCl2+NaCl+nCO2/CO (1).

A distinctive feature of the chlorination process loparite in the molten salt is that salt bath consists of chlorides of rare earth elements, sodium and calcium, formed during the interaction of the concentrate with chlorine according to the reaction (1). Thus, the chlorination can be performed without introducing additional fusible components.

The process is as follows.

Powdered concentrate and pitch coke load on the mirror of the melt by means of a screw feeder located in the upper part of charator. In the lower zone of charator through tuyeres serves chlorine, which barbthroat through the layer of chlorides. Passing through a layer of molten chlorides, chlorine is heated and reacts with dispersed in the melt concentrate and a reducing agent. Chlorination concentrate spend 100% of chlorine at a temperature of melt 950-1000°, the contents of loparite in the melt up to 1.5%carbon, about 2-3%, the layer height of the melt 2.8 to 3.5 meters

Gaseous products of chlorination, presents the advantage of chlorides of elements 4-6 groups of the Periodic system, form a gas-vapor mixture (ASG) and removed through a set of charator for cleaning and condensation. Low volatile products chlorine is the formation - chlorides 1-3 groups of the Periodic system are accumulated in rasplavnoj tub and periodically removed through the drain opening of the melt below the melt level, and are directed through the discharge chute into the receiving containers for collecting melt (see Korovin S. and other Rare and trace elements. Chemistry and technology. Moscow, MISIS, 1999, Vol.2, s-332).

Rasplavnye XLERATOR is a shaft made of high strength refractory and resistant to aggressive melts ceramic materials. The most complex devices charator are tuyere, which provide pressurized chlorine input through the wall of charator in the melt in a significant drop of temperature, vibration and abrasive action of the melt and of products of incomplete chlorination on the details of the tuyeres and the wall adjacent to the contact zone of the melt and chlorine. Therefore, it is tuyere node determines the lifetime of charator.

The disadvantages of the described method of chlorination niobium, tantalum-, titanium containing mineral raw materials - loparite concentrate are:

- high temperature chlorination;

to use a reductant;

- localization of the chlorination reaction interphase bubble chlorine to melt.

High temperature chlorate lead to rapid wear of the parts x the speaker, increase the ash components melt and make the necessary extra equipment for cleaning the calibration gas containing chlorides of niobium, tantalum and titanium, from the chlorides of iron and aluminum. This complicates the condensing system and increases the costs of carrying out the process. At the same time, reducing the temperature of 250-300°can increase the service life of charator several times.

The use of carbon-containing reducing agents leads to the dilution of the calibration gas non-condensable gases, which complicates its condensation.

When the chlorination loparite concentrate oxide as raw materials most of the chlorides of niobium and tantalum is formed in the shape of oxochloride. This requires additional chlorination of oxychlorides Nb and TA performed in special devices.

The melt level to ensure the necessary degree of absorption of chlorine is about 3 M. This leads to an increased cost of manufacture of charator.

Melt the chlorinators are used primarily for chlorination of shredded materials. Chlorination is difficult comminuted scrap and other metal materials in existing chlorinators leads to a low degree of chlorination. Existing chlorinators are sensitive to changes in performance associated with change in heat flux. This is especially true when x is aerovane metallic materials, flowing with great heat.

The known method of chlorination of these materials in molten chlorides NaCl+NaFeCl4[see Zelikman A.N. and other Niobium and tantalum, Moscow, metallurgy, 1990, p.100-102].

Crushed material or powder poured on the nozzle of the pieces of graphite immersed in the melt. The chlorination is carried out at 700-750°C. with Intensive stirring reach by bubbling chlorine supplied through tuyeres located in the lower part of charator.

The chlorides of iron contained in the feedstock is dissolved in the melt and remain in it as CHLOROFORMATES NaFeCl4and NaFeCl3. The chlorides of the elements of 4-6 groups, in particular niobium and tantalum form of higher chlorides in the form of vapor removed from charator in the condensation system.

This option is the implementation of the chlorination process allows you to:

- recycle metal waste (scrap radio engineering products, mechanical waste processing, waste parts of niobium and/or tantalum), metal powders, ferroniobium or other metal materials;

- get pentachloride niobium and/or tantalum as a technical product;

- fully absorb the chlorine in the limited volume of the melt;

to reduce the temperature of the chlorination up to 750-800°and to ensure absorption by the melt charator iron and other impurities.

XLERATOR dlyaprorabotki of this material is mine, lined with fireclay bricks. In the lower part of charator are tube for feeding chlorine (lance) years and for draining of the melt in the collection. On the cover of charator is the boot device and the duct for removal of the calibration gas to the condenser with a scraper connected to the collector chloride [see Zelikman A.N. and other Niobium and tantalum, Moscow, metallurgy, 1990, p.100-102].

The disadvantages of this device are:

- the location of the tuyeres in the lower part of chlarotera, which complicates maintenance and reduces the service life of the apparatus for the above reasons;

- low thermal conductivity of the material used in the lining of clay. Fireclay is satisfactory abrasion resistance, but does not have the necessary conductivity for thermal management flows;

- no special heat-removing elements in the design of charator is not possible to improve its performance on metal concentrates.

These method and apparatus are closest to the declared.

Object of the invention is a method and device designed to receive pentachloride niobium and/or tantalum from different types of polymetallic raw materials, providing the following technical indicators: increase in the rate of chlorine up to 99% or more when the melt level to 1 m; to increase the specific productivity is eljnosti of charator (mass absorbed chlorine to the volume of charator) and increasing the share of pentachloride in the total mass of the resulting chlorides of niobium and tantalum.

The method of achieving these results is the chlorination of complex niobium and/or tantalum materials in the melt containing the chlorides of iron (up to 25% of iron and/or copper (up to 40% copper), in the layer of melt thickness of 500-1000 mm, at temperatures 550-850°and at a flow rate of chlorine 1.7 to 2.2 kg per kg of raw materials. To keep the resulting aluminum chloride and iron (III) in the form of low volatile complexes NaAlCl4and NaFeCl4in the melt is injected sodium chloride in an amount of not less than 1.2 kg per 1 kg of iron and not less than 2.2 kg per 1 kg of aluminium in the original concentrate.

The presence in the melt of iron ions (II) and/or copper (I) as vectors of chlorine to ensure complete absorption of chlorine in the process, its high performance and almost the very possibility of the implementation process in small chloretone. If the feedstock is no iron and/or copper, they are specially based achievements in the melt content of 5-25% for iron and/or 10-40% of copper. Usually use a cheaper iron. The higher the concentration in the melt iron ions and/or copper - vectors of chlorine, the greater the load on chlorine able to take XLERATOR, higher performance and lower layer of the melt sufficient to fully absorb the chlorine. Maintaining a constant concentration of absorbing chlorine ions iron (II) and/or the copper (I) is achieved by the presence in the melt of the excess metal material, the reducing ions of iron (III) and/or copper (II).

If the depth of bubbling the melt is less than 500 mm, the degree of absorption of chlorine can be reduced, especially when the concentration in the melt of iron less than 5-10% and/or copper is less than 10-15%. This reduces the degree of chlorine. Increasing the depth of the melt above 1000 mm is not advisable, because deteriorates heat and mass transfer in the layer height of the melt in a narrow shaft charator and increases its hydraulic resistance.

The reduction of the melt temperature in the chlorination below 550°not desirable, because the chlorination process at this temperature is unstable and leads to the accumulation of the lower chlorides in the melt. Increasing its more than 850°delete from PACS number of low volatile impurities, which complicates the condensation and cleaning.

To solve the problem chlorination complex niobium and/or tantalum materials is carried out in the device, consisting of charator and condenser (see drawing). XLERATOR is a vertical apparatus equipped with a charging device (1), a pipe for supplying chlorine (2) and socket for output ASG (5)located on the lid of charator. Socket for output calibration gas is connected to the capacitor with scrapers (6). XLERATOR made of steel pipes with bottom lined with graphite glass and equipped with an external water-cooled R the head. The camera separation (4) located in the upper part of charator directly above the shaft charator (3). The ratio of the diameter of the shaft charator (3) to the diameter of the camera separation (4) is (2÷2,5):3 and the ratio of their heights - (1÷2):1; these relationships sizes allow you to fully separate the melt from the CBC, which increases the performance of the device. Settled in the condenser (6) chlorides from ASG going in the cube-the collection (7). The melt is removed from charator accumulating through a heated line drain (8) in the collection (9), which is periodically replaced.

Thus, XLERATOR is divided into 4 functional parts (counting from below):

1) the area of the input and distribution of chlorine, heat reactions of chlorination;

2) the cooling zone and intensive mass-, heat transfer in the upper part of the melt;

3) the zone of separation ASG and melt;

4) the upper part is for loading, exhaust fumes, temperature control and other

Note some of the design features described charator and its nodes.

In the design of charator used the lining of graphite with high thermal conductivity and sufficient mechanical, thermal and chemical durability in the conditions of the chlorination of metallic materials. The combination of design charator a two layer cooled housing, stainless steel pipe, with a tight PR is Gnanou lining of graphite allows you to effectively remove heat from the melt and lead the process of chlorination of metallic materials with high specific capacity in continuous mode.

Chlorine is available on a removable tube for feeding chlorine, the main part of which is graphite tube (2)passing through the gas zone, the melt layer and chloronema of bulk material to the bottom of charator. To secure the tube to supply chlorine to cover charator graphite tube is inserted into the water-cooled node stainless steel, coupled with nitric and perchloric lines by means of flange connections. The implementation of feed of chlorine by means of a removable tube for feeding chlorine installed to provide a flow of chlorine through the layer of melt and neprolongirovannogo material to the bottom of chlarotera, without compromising the integrity of the shell and lining allows replacement tube for feeding chlorine as wear without major repairs other parts of charator; change the angle and design of the inlet node of chlorine to change the circulation of the melt in chloretone; to use the tube for feeding chlorine as an internal electrode in a pair with graphite lining for heating the melt during periods of start and stops of the chlorination process.

The invention consists in the following.

The source material is crushed and powder of less than 3 mm or pieces the size of 3-50 mm using the boot device (1), respectively screw or sector of the feeder through a nozzle in the lid of charator load in W the hut of charator (3) on the surface of the melt. The melt level is 500-1000 mm

The chlorination process is carried out at a temperature of 550-850°C. chlorine Consumption average of 1.7 to 2.2 kg per 1 kg of raw materials, adjust the readings of the differential pressure gauge installed on the chlorine line. Formed during the chlorination of calibration gas passes through the camera separation (4), where it is separated from dust and drops of the melt, and exits through the outlet nozzle CBC (5)located on the lid of charator.

ASG enters the water-cooled condenser (6) with scrapers where it settles in the bulk of pentachloride niobium and/or tantalum (PHL) and chlorides of some other elements (tin, titanium, etc.), passing in gaseous state at the temperature of chlorination. PHL powder enters the cube-the collection (7). Nscontainerframe gases and vapors are sent to dolabellane in the dust chamber and the gases in the bubble scrubber (not shown).

When the chlorination in the melt, the accumulation of high-boiling chlorides of impurity elements (iron (II), copper, manganese, and others). The accumulation of the melt through a heated and lined graphite drain line (8) into the removable collection of the melt (9), where it is unloaded and sent for recycling.

Additional introduction into the melt of sodium chloride in the specified quantity, conducting the chlorination at a temperature of 550-850°who, the camera separation in the design of charator allow separation of the resulting chlorides, part of which goes to the ASG (NbCl5, TaCl5, TiCl4, SiCl4, SnCl4etc), and some remains in the melt (AlCl3, FeCl3, FeCl2, MnCl2, CuCl2, CuCl and others).

The implementation process at relatively low temperatures with retention in molten chlorides of iron and aluminum eliminates the use of saline irrigation filter for CBC, as is the case in technology chlorination loparite.

The proposed device allows you to adjust the performance of the device in a wide range of boot for improved heat and mass transfer and timing that allows the treatment of various forms of scrap: powders, lumpy material, fragments of the products, the size of which allows you to place them in the zone of chlorination, which cannot be done in the existing types of melt chlorinators.

How practically tested during the processing of the following types of complex niobium and/or tantalum materials: ferroniobium copper-niobium scrap, metal waste superalloys and powders of niobium and/or tantalum.

The invention is illustrated by the following examples.

Example 1

Ferroniobium in the amount of 100 kg of crushed and videoscom 10-50 mm in size using a pie feeder (1) is loaded into the mine charator (3) on the surface of the melt through the nozzle in the lid of charator. The initial level of the melt in chloretone is 800 mm

Chlorine is fed through a graphite tube for feeding chlorine (2), immersed in the melt. Sienna tube for feeding chlorine attached to the lid of the water-cooled pipe of stainless steel. The chlorination process is carried out at a temperature of 750°C. chlorine Consumption is 2.2 kg per 1 kg of the original ferroniobium. Formed during the chlorination of calibration gas exits through the outlet (5)located on the lid of charator passes through the camera separation (4), where it is separated from the melt droplets.

The ratio of the diameter of the upper part of charator (3) to the diameter of the zone of chlorination (4) is 2:3 and the ratio of their heights 2:1. ASG enters the water-cooled condenser (6) with scrapers where it condenses the bulk formed in the chlorination process of the low-boiling PHL, with the chlorides of some other elements (tin, titanium and so on). The amount of PHL in the form of a powder enters the cube-the collection (7), which replaces the accumulation. Nscontainerframe gases and vapors are sent to dolabellane and gas purification. The melt is removed from charator accumulating through the drain line (8) and freezes in the collection of the mold (9), which is periodically replaced. After cooling, the melt is discharged from the mold and sent for further processing.

The iron content in the source ferroniobium conc is the is 28 kg, and aluminum 6 kg To the melt additionally add to 47.1 kg of sodium chloride that is 2.2 kg per 1 kg of aluminum and 1,21 kg per 1 kg of iron in the original concentrate.

The resulting mixture PHL sent on receipt of individual compounds of niobium and tantalum. The degree of chlorination of raw materials exceeds 98%. The CBC analysis indicates that the average concentration of chlorine is not more than 0.3%, i.e. the degree of its use exceeds 99,3%.

Example 2

Copper-niobium scrap in the amount of 100 kg in the form of pieces with a size of 10-30 mm hairout same way as described in example 1 with the following differences.

The initial level of the melt in chloretone is 500 mm, the chlorination Process is carried out at a temperature of 550°C. chlorine Consumption is 1.7 kg per kg of the original scrap. The ratio of the diameter of the upper part of charator (3) to the diameter of the zone of chlorination (4) equal to 2.5:3 and the ratio of their heights 1:1. Pentachloride niobium sent for cleaning.

The degree of chlorination of raw materials exceeds 98%. The CBC analysis indicates that the average concentration of chlorine is not more than 0.28 per cent, i.e. the degree of its use exceeds 99,2%.

Example 3

The metal powder tantalum in the amount of 100 kg hairout same way as described in example 1 with the following differences.

The initial level of the melt in chloretone is 1000 mm Process harir the training is carried out at a temperature of 850° C. the Flow rate of chlorine is 1.0 kg per kg of the original powder. The ratio of the diameter of the upper part of charator (3) to the diameter of the zone of chlorination (4) is 2:3 and the ratio of their heights of 1.5:1. Pentachloride tantalum sent for cleaning.

The degree of chlorination of raw materials exceeds 99%. The CBC analysis indicates that the average concentration of chlorine is not more than 0.3%, i.e. the degree of its use exceeds 99,3%.

The main results of the implementation of the invention consist in the following:

the degree of chlorine increased to 99% or more when the melt level to 1 m;

- specific performance charator (kg absorbed chlorine to the volume of charator) increased from 150 to 520-1100 kg/(m3·h);

- weight of pentachloride to the total mass of the resulting chlorides of niobium and tantalum was 90% or more.

This has led to a drastic decrease in the height and area of the reaction zone charator (with comparable performance, increase productivity and improve its environmental performance, increased total extraction of niobium and/or tantalum 6-7% due to the exclusion of the operation of defloriani, reduced losses low volatile lower chlorides of niobium and/or tantalum with the output of the process melt.

1. The method of producing pentachloride niobium and/or tantalum, including chlorination chlorine polymetallic n is Obi and/or tantalum materials in molten chlorides, condensation and separation of the resulting pentachloride niobium and/or tantalum and chloride impurities and draining of the melt, characterized in that the chlorination is carried out in the layer of melt height of 500-1000 mm, containing chlorides of iron (up to 25% of iron and/or copper (up to 40% copper), and sodium chloride in an amount of not less than 1.2 kg per 1 kg of iron and not less than 2.2 kg per 1 kg of aluminium in the original materials, and the process is conducted at a temperature of 550-850°at a flow rate of chlorine 1.7 to 2.2 kg per 1 kg source materials, and the discharge of the melt is carried out with the top level of the melt through the drain line.

2. Device for receiving pentachloride niobium and/or tantalum chlorination complex niobium and/or tantalum materials in molten chlorides containing vertical XLERATOR, equipped with a tube for feeding chlorine, boot device and socket for output vapor-gas mixture located on the lid of chlarotera, and the collection of the melt, characterized in that XLERATOR made water cooled, lined with graphite and equipped with a camera separation, located in the upper part, and the ratio of the diameter of the shaft charator to the diameter of the camera separation is (2÷2,5):3, and the ratio of their heights is (1÷2):1, tube for feeding chlorine is made of graphite and are removable and passing through tightly coupled with cover charator vodoohda the intake pipe to the bottom of chlarotera, and the drain line is made to be heated and lined with graphite.



 

Same patents:

FIELD: non-ferrous metallurgy, possibly production of highly purified powders of tantalum and niobium with large specific surface by metal thermal reduction.

SUBSTANCE: method is realized at using as corrosion protection means layer of halide of alkali metal formed on inner surface of vessel before creating in reaction vessel atmosphere of inert gas. Charge contains valve metal compound and halide of alkali metal. It is loaded into reaction vessel and restricted by protection layer of halide of alkali metal having melting temperature higher than that of charge by 50 - 400°C. Before loading charge, valve metal compound and alkali metal halide may be mixed one with other. Mass of protection layer of alkali metal halide Ml and charge mass Mc are selected in such a way that that to satisfy relation Ml = k Mc where k - empiric coefficient equal to 0.05 - 0.5. Gas atmosphere of reaction vessel contains argon, helium or their mixture. Fluorotantalate and(or) oxyfluorotantalate or fluoroniobate and(or) oxyfluoroniobate of potassium is used as valve metal compound. Sodium, potassium or their mixture is used as alkali metal. Chloride and(or) fluoride is used as alkali metal halide. Valve metal compound and alkali metal halide may contain alloying additives of phosphorus, sulfur, nitrogen at content of each additive in range 0.005 - 0.1% and 0.005 - 0.2% of mass valve metal compound respectively. Invention lowers by 1.3 - 2 times contamination of powder with metallic impurities penetrating from vessel material. Value of specific surface of powder is increased by 1.2 - 1.8 times, its charge is increased by 10 - 30 %, leakage current are reduced by 1.2 - 1.5 times.

EFFECT: improved quality of valve metal powder, enhanced efficiency of process due to using heat separated at process of reducing valve metal for melting protection layer.

9 cl, 1 tbl, 4 ex

FIELD: hydrometallurgy; ore concentrates processing.

SUBSTANCE: the invention is pertaining to the field of hydrometallurgy, in particular, to processing of the loparite concentrate. The method includes a decomposing of the loparite concentrate at the temperatures of 103-105°C and the concentration of hydrofluoric acid of 38-42 mass % with production of the pulp containing fluorides of titanium, rare earth elements (REE), niobium, tantalum and sodium. The pulp is filtered at the temperature of 90-95°C with extraction into the fluorotitanium solution of fluorides of niobium and tantalum and no less than 58 % of sodium in terms ofNa2O and separation of the sediment containing fluorides of rare earth elements (REE) and a residual sodium. The produced solution is cooled down to 18-24°C with separation of the second sediment of sodium fluorotitanate. After that they extract niobium and a tantalum from the solution by octanol-1 extraction at a ratio of the organic and water phases as 1.1 : 1. The sediment of REE fluorides is washed from fluorotitanate by sodium water in a single phase at the temperature of 90-95°C and at the solid :liquid ratio = 1:2-2.5. The cleansing solution is separated and evaporated with extraction of the additional sediment of sodium fluorotitanate. After extraction of niobium and tantalum the fluorotitanium solution is evaporated and filtered with separation of the first sediment of sodium fluorotitanate from the concentrated solution of fluorotitanium acid, which is directed to extraction of titanium. The gained first, second and additional sediments of sodium fluorotitanate are combined and subjected to conversion with production of sodium fluorosilicate and the conversional fluorotitanium acid added to fluorotitanium solution before its evaporation. The technical result of the invention is a decrease in 2.0-2.5 times of the volume of the cleansing solutions at provision of a high degree of extraction of compounds of titanium and other target products. The produced sodium fluorotitanate contains the decreased amount of the impurity ingredients of calcium and strontium.

EFFECT: the invention ensures a decrease in two-two and a half times of the volume of the used cleansing solutions at provision of a high degree of extraction of compounds of titanium and other target products and a decreased amount of impurities of calcium and strontium in the sodium fluorotitanate.

7 cl, 1 dwg, 1 tbl, 3 ex

FIELD: metallurgy of rare and dispersed metals, chemical technology.

SUBSTANCE: invention relates to a method for extraction separation of tantalum and niobium. Method involves extraction separation of tantalum from niobium with organic solvent. As an organic solvent method involves using a mixture of methyl isobutyl ketone taken in the amount 40-80 vol.% with aliphatic (C7-C9)-alcohol taken in the amount 20-60 vol.%. At the extraction process tantalum transfers into organic phase and niobium - into aqueous phase. Then organic and aqueous phases are separated. Invention provides enhancing the extraction degree of tantalum into organic phase and to enhance the separation degree of tantalum and niobium in extraction.

EFFECT: improved separating method.

5 tbl, 5 ex

FIELD: metallurgy; methods of preparation of charges for production of niobium-bearing material.

SUBSTANCE: the invention is dealt with production of niobium-bearing materials used for production of special steels. The technical result is an increased degree of transition of niobium into an alloy, decreased share of impurities in the alloy, decreased production costs. For this purpose the charge for production of a niobium-bearing material contains the raw material containing niobium pentaoxide, a nickel-bearing material, aluminum, calcium oxide, calcium fluoride and an exothermic oxidative additive. At that in the capacity of the exothermic oxidative additive it contains potassium chlorate with moisture of 2-12% at the following ratio in shares in respect to the total weight of the charge: niobium pentaoxide - 0.470-0.520, nickel - 0.190-0.270, aluminum - 0.180-0.200, calcium oxide - 0.030-0.040, calcium fluoride - 0.003-0.004, potassium chlorate with moisture of 2-12% - 0.043-0.049. At preparation of the charge after mixing of components it is exposed to compaction in the crucible up to the value of the plastic strength of 0.4-10.0 MPa.

EFFECT: the invention ensures an increased degree of niobium transition into an alloy, decreased share of impurities in the alloy, decreased production costs.

2 cl, 1 tbl, 3ex

FIELD: electrometallurgy, namely processes for producing high-purity niobium ingots used in power generation plants operating with use of low-temperature superconductivity effect.

SUBSTANCE: method comprises steps of electron-beam refining of consumable niobium blank; using blank of niobium of given kind containing niobium uniformly distributed along its length and produced by iodide refining as consumable blank in order to produce niobium ingots with predetermined (in range 200 - 500) relation of specific resistances at temperature values 193K and 9.2K; determining mass relation of niobium of given kind and niobium produced by iodide refining according to relation of specific resistances at temperature values 193 K and 9.2 K with use of expression mn/mu = (500 - ρ2939.2)/(800 + 2 x ρ2939.2) where mn - mass of niobium of given kind, g; mu - mass of niobium produced by iodide refining, g; ρ293 - specific resistance of niobium at temperature 193K, ohm x m2/m ; ρ9.2 - specific resistance of niobium at temperature 9.2K, ohm x m2/m.

EFFECT: enhanced efficiency of process, lowered cost price of high-purity niobium ingots.

2 tbl, 2 ex

FIELD: production of pure niobium.

SUBSTANCE: method includes reducing fusion of niobium pentoxide with aluminum and calcium to provide crude ingots followed by heat treatment and multiple electron beam refining. As an additional raw material in step of reducing fusion sublimates (preferably in non-oxidized form) from second and subsequent electron beam refining are used. Such sublimates are obtained by subsequent cooling of furnace smelting chamber under residual pressure of 10-2-10-4 mmHg for 1.0-3.0 h, letting-to-helium under 1-3 mmHg for 1.0-3.0 h, and letting-to-air for 20-40 min. Sublimates are added in amount of 4.5 % based to feeding niobium pentoxide. Claimed method affords the ability to increase niobium pentoxide consumption by 73 kg in respect to 1000 kg of pure niobium in crude ingots.

EFFECT: production of pure niobium with increased effectiveness without deterioration of refined niobium quality.

2 cl, 1 tbl

The invention relates to pyrometallurgy, in particular the production of niobium from its oxide, and can be used for the production of ferroniobium

The invention relates to the field of hydrometallurgical processing of tantalum raw materials and are aimed at achieving its complex use

The invention relates to ferrous metallurgy and can be used to obtain alloy powders of tantalum or niobium

The invention relates to metals, in particular tantalum, and products made from tantalum, as well as to methods of obtaining and processing of tantalum

FIELD: rare metal metallurgy, possibly extraction of rhenium out of technogenic raw material containing metallic rhenium or its alloys.

SUBSTANCE: method comprises steps of chlorinating with chlorine gas at 20°C in liquid medium dimethylformamide and water at mass relation of technogenic raw material: dimethylformamide : water such as 1 : (20 - 25) : (8 - 10) and at relation of technogenic raw material : chlorine such as 1 : (35 - 45). Method is simply realized for one stage without heat supply; it does not need deficient equipment and high-cost reagents. Method allows for one operation provide rhenium extraction degree 25.7% at initial temperature of process 20°C and initial content of rhenium in alloy 42.5%.

EFFECT: significantly simplified process of rhenium extraction from waste alloys of special technology branches, lowered energy consumption.

1 tbl, 4 ex

FIELD: metallurgy of rare metals; methods of rare metals raw materials chlorination.

SUBSTANCE: the invention is pertaining to metallurgy of rare metals, in particular, to the methods of rare metals raw materials chlorination. The technical result of the invention is an increased speed of the rare metals raw materials chlorination and decreased consumption of reactants due improved wetting of the carbon-containing deoxidizing agent with a saline melt. The method includes a grinding of rare metals raw materials, its batching with the carbon-containing deoxidizing agent, treatment of the charge with 0.5-2.0 % water solution of soluble potassium silicate or sodium silicate or their mixture, a graining, drying of granules and a chlorination of the granular raw at the temperature of 750-1000°C in a melt containing an alkali metal chloride or a mixture of chlorides of alkali and alkali-earth metals.

EFFECT: the invention ensures an increased speed of chlorination of the rare metals raw materials and decreased consumption of reactants.

8 ex

The invention relates to the field of metallurgy of rare metals and is intended to obtain rare metal by chlorination of the oxide materials in molten salts and can be used for the production of chlorides hafnium, titanium, niobium, tantalum and other metals
The invention relates to the field of non-ferrous metallurgy, in particular to the metallurgy of titanium, namely the composition of such mixture to the chlorination process in molten chloride salts
The invention relates to a method for integrated processing of anthropogenic vanadium raw materials, including chlorination in molten chlorides of the metals with the formation of the vapor-gas mixture and the spent molten salt chlorinators, condensation of chlorides of vanadium, titanium and silicon, distillation and chemical separation and purification, recycling of titanium tetrachloride and silicon, hydrolysis of oxytrichloride vanadium emitting precipitation of metavanadate ammonium and/or vanadium pentoxide, niobium, Department of precipitation from the mother solution, washing, drying and/or calcining to produce commodity of vanadium compounds
The invention relates to ferrous metallurgy, in particular to a method of processing a variety of vanadium products

The invention relates to the field of metallurgy manganese and can be used to produce manganese metal, ferromanganese and compounds of manganese for the production of high-grade ferromanganese, for the biomedical industry and the production of catalysts of the poor mn containing ores

The invention relates to ferrous metallurgy, in particular to methods and devices for obtaining refractory metal chlorides by chlorination of molten chloride salts
The invention relates to ferrous metallurgy, in particular to the preparation of raw materials for chlorination

FIELD: metallurgy of rare metals; methods of rare metals raw materials chlorination.

SUBSTANCE: the invention is pertaining to metallurgy of rare metals, in particular, to the methods of rare metals raw materials chlorination. The technical result of the invention is an increased speed of the rare metals raw materials chlorination and decreased consumption of reactants due improved wetting of the carbon-containing deoxidizing agent with a saline melt. The method includes a grinding of rare metals raw materials, its batching with the carbon-containing deoxidizing agent, treatment of the charge with 0.5-2.0 % water solution of soluble potassium silicate or sodium silicate or their mixture, a graining, drying of granules and a chlorination of the granular raw at the temperature of 750-1000°C in a melt containing an alkali metal chloride or a mixture of chlorides of alkali and alkali-earth metals.

EFFECT: the invention ensures an increased speed of chlorination of the rare metals raw materials and decreased consumption of reactants.

8 ex

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