Method of tantalum receiving

FIELD: metallurgy.

SUBSTANCE: invention concerns rare-metal industry. Particularly it concerns receiving of metallic tantalum by metallothermic reduction of its salts. For receiving of metallic tantalum charge, containing mixture of double complex chloride salt of tantalum - KTaCl6 and potassium chloride - KCl in ratio 1:(0.2÷0.5) by mass are fed by portions or uninterruptedly in the form of powder or melt on melt mirror of metallic sodium, taken in excess 60-80% of stoichiometrically necessary amount. Reduction is implemented at temperature 550-650°C, with speed of charge feeding 15-20 g/cm2·hour of area melt mirror of metallic sodium melt. Received reduced reactionary mass is subject to vacuum- thermal processing at temperature 500-540°C and residual pressure, not exceeding equilibrium pressure of sodium steams at temperature of vacuum- thermal processing of unreacted sodium. After vacuum- thermal processing it is implemented hydro metallurgical treatment of reactionary mass.

EFFECT: exclusion of ecological pollution of environment.

4 cl, 2 tbl, 2 ex

 

The invention relates to rare-metal industry, in particular to a technology for metallic tantalum metallothermic restoration of its salts.

The resulting tantalum is used in the form of powders in the production of the volume-porous electrodes of the capacitors and as a source of metal for the production of ingots of high purity, which produce structural products, spray targets for electronics.

A known method of producing tantalum, including the production of chloride double salt of tantalum from pentachloride tantalum, Incoterms recovery blend containing double chloride complex salt of tantalum KTaCl6and potassium chloride, at a temperature 370-720°Spoluchennya reaction mass contains up to 4% tantalum chlorides lower valences (TaCl3and TaCl4). Dopostavleno them to the metal and the salt distillation products of the process (ZnCl2and KCl) are vacuum heat treatment at a temperature of 1000-1010°C and a pressure of about 1·10-3mm Hg(see RF patent №2219269, SW 34/24, publ. 2003).

The disadvantage of this method is the necessity of using high-temperature vacuum thermal processing (1000-1010° (C) to dovolenkovania chloride tantalum lower valences. Such processing requires expensive equipment (contrasenya p the Chi and high vacuum equipment vacuum 1· 10-3mm Hg).

A known method of producing tantalum from a mixture containing tortontilt potassium and potassium chloride, nitratereductor restoration at a temperature of 500-700°C. the Method involves dosing in the reactor during the recovery process of fortuntate potassium, molten sodium and potassium chloride. By adjusting the feed rate of the components of the reaction and slag-forming additives (KCl), their ratio and the reaction temperature, to produce a powder with different specific surface (see RF patent №2242329, B22F 9/18, publ. 20.12.2004,).

One of the major drawbacks of this method is the need to create a special redistribution of complex fluoride, tantalum (K2TaF7from pentachloride tantalum, which is the product of processing TotalStorage raw materials. In addition, the hydrometallurgical processing of the recovered tantalum for separating slag from the production of environmentally harmful fluorine-containing effluent contributes to environmental pollution.

In Russia, the main raw material source for the production of tantalum are loparite concentrates, which are processed using chlorine technology with getting pentachloride niobium and tantalum.

The technical purpose of this invention is the creation of production of metallic tantalum from pentachloro the s tantalum using existing domestic raw materials. This production has a significant economic benefits in comparison with traditionally used abroad obtaining of tantalum fluoride salts.

A method of obtaining a valve metal, such as niobium and tantalum, including the introduction into the reactor from a Nickel salt of a valve metal composition R2MX7where R is alkali metal, M is tantalum or niobium, X is a halogen from the group of F, Cl, Br, as well as sodium chloride or potassium, melting salts and restoration of the valve metal of the alkali metal in the presence of active additives in the helium atmosphere at a temperature 800-840°With continuous stirring of the melt. The effect of the active additive is advanced relative to the melt interaction with residual moisture and oxygen present in the atmosphere of the reactor. The active additive is introduced in the form of a powder of a valve metal in the amount of 0.3 to 3.0% by weight of the salt of a valve metal. As a source of salt tantalum use only K2TaF7. The process is conducted when the flow of molten sodium in the melt containing fluoride salt tantalum, potassium chloride or sodium and metal powder tantalum.

The resulting reaction mass is washed successively with water, 10%hydrochloric acid, 1%solution of hydrofluoric acid and distilled water and vysushila is so

Enter the metal tantalum forms on the wall of the reactor protective intermetallic film Ni3Ta and Ni2The one that prevents the contamination of impurities from the material of the reactor (see RF patent №2164194, B22F 9/18, publ. 20.03.2001,). The method adopted for the prototype.

The disadvantages of this method is the need for fluoride salts of tantalum and pollution fluoride wastes.

The technical result of the claimed invention is to provide a technology of producing metal powder tantalum from its chloride compounds and elimination of environmental pollution.

The technical result is achieved in that in the method of producing metal tantalum, including nitratereductor recovery blend containing salt tantalum halide and potassium chloride, by heating and stirring, the hydrometallurgical processing of the recovered reaction mixture, according to the invention as a salt of halide tantalum use double chloride complex salt and potassium tantalum composition KTaCl6the restoration is subjected to a mixture of double chloride complex salts of tantalum KTaCl6and potassium chloride KCl at a ratio of 1:(0,2÷0,5) by weight, the mixture was fed to the surface of the molten sodium taken in excess of 60-80% of the stoichiometrically necessary quantity, t is mperature 550-650° With, before the hydrometallurgical processing of the received recovered reaction mass is subjected to vacuum thermal processing at a temperature of 500-540°and a residual pressure not exceeding the equilibrium vapor pressure of sodium at a temperature of vacuum thermal processing of unreacted sodium; the charge to restore served on the mirror of molten metallic sodium in the form of a powder or melt speeds of 15-20 g/cm2·h surface area of the molten metallic sodium, and the mixture onto the surface of the melt is served in portions or continuously.

The method consists in a new set of distinctive features and parameters of the process metallotrejderskogo recovery of tantalum.

The first significant difference is the composition of the original mixture for recovery. In contrast to the use of complex fluoride, tantalum, which is obtained from pentachloride tantalum transfer it to the oxide of tantalum and only then in the tantalum fluoride, the use of double chloride complex salt does not require such a complex redistribution. Dual integrated tantalum chloride can be obtained in the process of distillation separation of niobium and tantalum in primary production, existing in Russia - processing of loparite concentrate on chlorine technology.

The second is the significant difference is quantitative characteristics of the components of the process nitratereductor recovery the ratio of the double chloride complex salts of tantalum and potassium chloride 1:((0,2÷0.5) and 60-80%of the excess reductant is sodium.

The third significant difference is the set of operations - recovery distillation of the excess of reducing agent restore options and distillation.

The above differences provide metal tantalum, meets the requirements of the production of capacitors, a high yield of the recovered tantalum (close to 100%), elimination of environmentally harmful fluoride effluent and the lack of need for fluoride compounds of tantalum from pentachloride tantalum.

The filing of the charge, consisting of a complex of tantalum chloride and potassium chloride on the surface of such a strong reducing agent like sodium metal, leads to the total recovery of tantalum to metal without the formation of an intermediate of lower chlorides of tantalum or decomposition of the complex of chloride on pentachloride tantalum and potassium chloride. The latter is especially important as feeding on the surface reducing pentachloride tantalum instead of its dual complex of chloride or thermal decomposition of the latter into its component parts in the submission process leads to the preferential evaporation of pentachloride tantalum and putting it into the cold zone of the apparatus. Under the stated conditions, the degree is vosstanovleniya tantalum double complex chloride at a temperature of 550-650° With close to 100%, whereas tantalum from his pentachloride under these same conditions are restored only by 3-5%, and the bulk of it evaporates, not reacting, and is taken out from the reaction zone.

Substantiation of the parameters.

Excess potassium chloride in the amount of 0.2-0.5 by weight of the double complex of tantalum chloride provides a shift in the equilibrium of the reaction of thermal decomposition of the complex of tantalum chloride:

KTaCl6↔TaCl5+KCl to the left, i.e. decomposition of the double complex salts of chloride tantalum and provides a more complete recovery of tantalum.

On the other hand, an excess of potassium chloride stabilizes the temperature of the recovery process. High esotericist recovery process dual complex of tantalum chloride sodium leads to local overheating of the supplied mixture and, consequently, to increase the degree of thermal decomposition of the double complex of tantalum chloride. The presence of inert in the process of excess potassium chloride reduces the degree of overheating of the charge and thereby stabilizes the recovery process. The minimum process temperature (550° (C) and the minimum excess of potassium chloride (20%) virtually eliminate thermal decomposition of the complex of tantalum chloride, thereby ensuring the completeness of recovery t is ntala.

Completeness of recovery of tantalum can also be achieved by raising the temperature of the recovery up to 650°but if the increase in the number of excess potassium chloride to 50% by weight of the double complex of tantalum chloride.

The feed rate of charge on the surface of the reductant is also linked to local overheating of the supplied charge. The stated interval feeding speed of the charge (15-20 g/cm2·h) consistent with the stated interval of an excess of potassium chloride.

High speed feeding of the charge (up to 20 g/cm2·h) require a larger excess of potassium chloride within the stated interval of its content in the charge.

Low feed speed (from 15 g/cm2·h) do not cause local overheating of the charge with minimal claimed the excess of potassium chloride in the charge.

High excess reductant is sodium, which constitutes 60-80% of the stoichiometrically necessary quantity, related to the intake of the filing of the charge on the surface of the molten sodium, and stir by mechanical means. In this case, to achieve full recovery fed to the reactor charge shall be under a layer of reducing agent, or perhaps a thermal decomposition of the dual complex of tantalum chloride and, accordingly, the loss of tantalum due to evaporation and removal of pentachloride tantalum. The amount of the excess will restore the La provides full coverage (dip) served as charge, and solid products of the recovery process (KCl, NaCl, TA) layer of liquid sodium to the end of the feed mixture. With a maximum excess of potassium chloride in the mixture (50%) required maximum excess reductant (80%), with a minimum number of potassium chloride (20%) - 60% of the excess of metallic sodium.

To remove excess reducing agent spend his distillation under conditions of low vacuum. The efficiency of the distillation define the claimed range of temperature of distillation and the residual pressure, providing a minimum equilibrium vapor pressure of the sodium in this temperature range.

The claimed invention is illustrated in the examples.

Example 1. In the retort stainless steel with a diameter of 130 mm and a height of 350 mm establish welded niobium glass with a diameter of 100 mm and a height of 250 mm, which is poured from the refiner 1100 g of metallic sodium. The retort, closed the lid, heated to 570°in argon atmosphere and begin filing of the charge consisting of a mixture of a double complex of tantalum chloride (KTaCl6) and potassium chloride in the amount 2586 g 646 g, respectively. The estimated excess reductant was 60%and the excess KCl - 25%. The feed mixture is conducted at an average speed of 1,216 kg/h, which corresponds to the specific feed rate to 15.5 g/cm2·am In the process of filing the charge contents of the glass continuously stirred IU onicescu stirrer, providing a finding of initial components, and solid reaction products under the layer of reducing agent. After the filing of the charge and dismantling of the stirrers on the cover of the retort install the condenser. Reduce the temperature of the reaction mass up to 525°and vaccum the retort through the condenser, the residual pressure in the retort support is 5.0 mm Hg, which is less than the equilibrium vapour pressure of sodium vapor at a given temperature. After 25 minutes, the evacuation and heating of the retort stop. The cooled reaction mass knock out of the Cup and subjected to hydrometallurgical processing aqueous solution of hydrochloric acid. The obtained tantalum powder is washed and dried.

The mass of the obtained powder of tantalum was 1051, the output of tantalum powder 97,34%.

Example 2. In the retort stainless steel with a diameter of 130 mm and a height of 350 mm establish welded niobium glass with a diameter of 100 mm and a height of 250 mm, which is poured from the refiner 1000 g of metallic sodium. The retort, closed the lid, heated to 640°in argon atmosphere and begin filing of the charge consisting of a mixture of a double complex of tantalum chloride (KTaCl6) and potassium chloride in the amount of 2300 g and 1100 g, respectively. The estimated excess reductant was 78%, and the excess KCl - 48%. The feed mixture is conducted at an average speed of 1,570 kg/h, which is suitable for the t specific speed of 20 g/cm 2·am In the process of filing the charge contents of the glass continuously stirred with a mechanical stirrer, providing a finding of initial components, and solid reaction products under the layer of reducing agent. After the filing of the charge and dismantling of the stirrers on the cover of the retort install the condenser. Reduce the temperature of the reaction mass up to 525°and vaccum the retort through the condenser. The residual pressure in the retort support is 5.0 mm Hg(pressure less than the equilibrium vapor pressure of sodium at a given temperature). After 25 minutes, the evacuation and heating of the retort stop the Cooled reaction mass knock out of the Cup and subjected to hydrometallurgical processing aqueous solution of hydrochloric acid. The obtained tantalum powder is washed and dried.

The mass of the obtained powder of tantalum was 940,16 g, and the output of the tantalum powder is 97.9%.

In tables 1 and 2 shows the fractional and chemical composition of the tantalum powders obtained in examples 1 and 2.

Table 1.
Fractional composition of the tantalum powder obtained in examples 1 and 2.
№ p/pFraction, mmOutput fraction, %
Example 1 Example 2
10.51,30,8
20.5 to+3,019,820,6
3-3+1035,7of 40.3
4-10+3026,027,3
5-30+7011,36.8
6-70+1005.94,2
Only100,0100,0

Table 2.
The content of admixtures in powdered tantalum obtained in examples 1 and 2.
# exampleThe content of impurities, ppm
ONAlFeCaNbSiNaMgToW
1160010103652035205369
215001010485 2040205388

Data presented in table indicate that you have received this invention tantalum powder meets THE 95205-82 on tantalum materials for the production of ingots of the highest grade.

The chemical composition of the obtained powder meets the requirements of a capacitor tantalum powders. Easy grindability conglomerates, which consist of the obtained powders, allows to obtain fine-grained capacitor powders.

Thus, the claimed invention allows to:

1) to create the technology of production of metal tantalum directly from domestic sources of raw materials;

2) get the metal tantalum high quality that complies with the requirements of the major consumers of tantalum producing volume-porous electrodes of the capacitors, sputtering targets, and structural materials.

1. Method of producing metal tantalum, including nitratereductor recovery blend containing salt tantalum halide and potassium chloride, by heating and stirring, the hydrometallurgical processing of the recovered reaction mixture, characterized in that as the halide salts of tantalum used in the t of the double chloride complex salt and potassium tantalum composition KTaCl 6the restoration is subjected to a charge of a mixture of double chloride complex salts of tantalum - KTaCl6and potassium chloride - KS1 in the ratio 1:(0,2÷0,5) by weight, by filing a charge on the surface of the molten sodium taken in excess of 60-80% of the stoichiometrically necessary quantity, at a temperature of 550-650°With, before the hydrometallurgical processing of the received recovered reaction mass is subjected to vacuum thermal processing at a temperature of 500-540°and a residual pressure not exceeding the equilibrium vapor pressure of sodium at a temperature of vacuum thermal processing of unreacted sodium.

2. The method according to claim 1, characterized in that the charge to restore serves on the surface of the molten metallic sodium in the form of a powder or melt.

3. The method according to claim 1, characterized in that the charge on the surface of the mirror area of the molten metallic sodium is served with a speed of 15-20 g/cm2·h

4. The method according to claim 1, characterized in that the charge on the surface of the molten sodium is served in portions or continuously.



 

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1 dwg, 1 ex

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

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

FIELD: metallurgy.

SUBSTANCE: method includes reduction of fluorine tantalite of potassium with liquid sodium in medium of melted saline bath of halogenides of alkali metals by means of alternate portioned dozing of sodium, and further - of fluorine tantalite of potassium. Fluorine tantalite of potassium is introduced into mixtures with part of the charge of halogenides of alkali metals, used for making of a saline bath. Amount of halogenides of alkali metals in the mixture introduced into melt with fluorine tantalite of potassium constitutes from 60 to 125% (wt) from weight of fluorine tantalite of potassium.

EFFECT: dimension in size of powder particles, reduction of duration of reduction process, decreasing of power consumption for melting of saline charge and forced cooling of reaction vessel.

1 tbl, 1 ex

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