Procedure for extraction of niobium from water solution containing fluorine
SUBSTANCE: procedure for extraction of niobium from water solution containing fluorine consists in sorption by contacting solution and anionite. Anionite is subjected to acidic or water treatment before sorption. Sorption is carried out with anionite of grade ANP containing exchange groups at pH=2-4.
EFFECT: optimal conditions for fast and efficient procedure for niobium extraction out of water solution containing fluorine.
4 dwg, 2 tbl, 3 ex
The method of extraction of niobium fluoride aqueous solution relates to the field of extraction of substances with the use of sorbents and can be used in ferrous and nonferrous metallurgy, as well as for the treatment of industrial and domestic wastewater.
It is known the use of ion exchange resins for processing solutions integrated (HF) anions niobium [R. Ripen and I. Kitano. Inorganic chemistry. Volume 2. Chemistry of metals. M.: Mir. 1972. .183]. To this end, apply a strongly basic anion exchange resin followed by elution of the niobium solution of NH4Cl and Hcl.
The disadvantage is that no sorption of fluoride-niobates from aqueous solutions by ion-exchange resin brand AMP.
The closest technical solution is the method of extraction of niobium fluoride aqueous solution, including sorption by contacting the solution and the anion brand AMP [Lebedev K.B. Ion exchangers in nonferrous metallurgy, M., metallurgy, 1975, s].
The disadvantage of this method is that it is not given optimal conditions sorption of niobium fluoride aqueous solutions by ion-exchange resin brand AMP.
Task to be solved by the claimed invention is directed, is to find the optimum conditions for rapid and effective method of extraction of niobium in the form of anion NbF72-of the fluorine-containing aqueous solution.
Technical R is the result, which can be achieved by implementation of the invention is the efficiency of the process of adsorption of anion NbF72-of the fluorine-containing aqueous solution.
This technical result is achieved by the known method of extraction of niobium fluoride aqueous solution, including sorption by contacting the solution and the anion brand AMP, before sorption conduct preliminary acid or water processing anion-exchange and sorption of lead at pH=2-4 anion exchange resin containing exchange group
The essence of the method is illustrated in the data of table 1 and table 2 and figures 1 - 4, where there are dependencies residual concentration of niobium, mg/DM3and sorptive exchange capacity (SOY) sorbent, mg, Nb on 1 g of sorbent, from the time of sorption, h, pH and method of pre-treatment sorbent.
Examples of specific implementation method
Sorption Nb was obtained from 100 cm3the original solution of K2NbF7the mass of sorbent 1, the Sorbent previously in the day was kept at 0.1 N. solutions of NaOH, HCl or distilled water.
Gel strong basic anion exchanger AMP with a spherical granules obtained by aminating HMS styrene and 3.5 to 4.0% DVB pyridine. The particle size of the granules 0,63-1,60 mm; specific volume of the swollen resin of 2.7-2.9 cm3/g, the mechanical strength of 98-99%; OYe 3,3-3,7 mg-ekvg. Exchange group:
The concentration of ions of niobium was determined on the photocolorimeter brand KFK-3, and acid-base characteristics of the solution was controlled by a pH-meter pH-121.
In the absorption process of mixing and maintaining the set value of pH was carried out until a constant value SOY sorbent, testified to the occurrence of sorption equilibrium.
Sorption was carried out at room temperature.
Using the values of the concentrations of niobium ions in aqueous solution source and after sorption, the expected SOYBEAN, mg/g
Example 1 (1)
Figure 1 from a solution with an initial concentration of 500-900 mg/DM3Nb given according SOY, mg/g of sorbent from the pH and pre-treatment sorbent (graphics processing sorbent: 1 acid, 2 - water, 3 - alkaline to pH interval=1-6.
Research has shown that the best results were obtained at pH=2-4 at acidic or aqueous processing of the sorbent. Through the day, sorption, there is a slight precipitate. In the case of the alkali treatment of the sorbent, as well as at pH=5-6 with aqueous or acidic treatment of the sorbent solution became turbid immediately, as soon as there was contact of the sorbent and solution, and in the process of sorption soon fell sediment. The appearance of turbidity in the solution reduces the results of sorption.
Example 2 (table 1, figure 2).
the Sorbent previously in the day was kept at 0.1 N. the solution is Hcl.
In table 1 and figure 2 are given the results of sorption Nb ions at pH=4 within 24 hours of adsorption and the initial concentration 979-2994 mg/DM3. It is seen that at pH=4 and acidic treatment of the sorbent best results sorption obtained at the time of sorption of no more than 3 hours. It is established that SOY sorbent increases with increasing concentration of the original solution, when the concentration of the initial solution 2555 mg/DM3Nb SOY=160 mg/g
Example 3 (table 2 and figure 3).
Sorbent previously in the day was kept in distilled water.
In table 2 and figure 3 are given the results of sorption Nb ions at pH=3 within 24 hours of adsorption and the initial concentration 979-2994 mg/DM3. It is seen that at pH=3 and water handling sorbent best results sorption obtained at the time of sorption of less than 4 hours when there is no clouding of the solution. It is established that SOY sorbent increases with increasing concentration of the original solution, when the concentration of the initial solution 2555 mg/DM3Nb SOY=149 mg/g
Figure 4 according to table 1 and table 2 and figure 2 and 3 shows the isotherms of sorption - dependence SOY, mg/g of sorbent from the equilibrium solution concentration, mg/DM3Nb, at acidic (figure 1) and water (graph 2) treatment of the sorbent for the sorption time 4 hours
From the data table. 1 and 2 and figure 1-4 shows that at room temperature the results of the sorption depend on before kiteley processing sorbent, the initial solution concentration, pH of the solution in the process of sorption and sorption time.
Compared with the prototype sorption on ion-exchange resin brand AMP under optimal conditions is a quick and effective method of extraction of niobium ions of the fluorine-containing water solutions.
|The dependence of the residual ion concentration Nb from the time of adsorption and the initial concentration of the solution at acidic treatment of the sorbent, pH=4|
|Time, h||Residual concentration, mg/DM3Nb|
|The dependence of the residual ion concentration Nb from the time of adsorption and the initial concentration of solution in water handling sorbent, pH=3|
|Time, h||Residual concentration, mg/DM3Nb|
Method for the recovery of niobium from a fluorine-containing aqueous solution, comprising the sorption by contacting the solution and the anion brand AMP, characterized in that before sorption conduct of acid or water processing anion-exchange and sorption of lead at pH 2-4 anion exchange resin containing exchange group
SUBSTANCE: procedure consists in heating chemically active gas containing gaseous hydrogen. Further, the procedure consists in bringing oxide of refractory metal to contact with said heated gas in form of particles of pentaoxide of tantalum for reduction of tantalum pentaoxide in form of particles. Also, weight ratio of gaseous atomic hydrogen and tantalum pentaoxide in form of particles is over 1.5:1 at temperature from 1900 °K to 2900 °K with formation of primary metal of tantalum. Another version of the procedure consists in heating chemically active gas containing gaseous hydrogen. Oxide of refractory metal is brought into contact with said heated gas in form of particles of niobium oxide chosen from a group containing of niobium dioxide, niobium pentaoxide and their combination for reduction of said niobium oxide in form of particles. Weight ratio of gaseous hydrogen and niobium oxide in from of particles is at least 9:1 at temperature from 2100°K to 2700°K with formation of primary metal of niobium.
EFFECT: raised efficiency of production of primary metal of tantalum or niobium due to performing process in one stage.
24 cl, 4 tbl, 14 dwg
FIELD: process engineering.
SUBSTANCE: invention relates to production of barrier metal powder to be used as anode material for electrolytic capacitors. Proposed method comprises feeding first barrier metal powder and reducing component into reactor with hot zone, making said powder and said reducing component interact in nonstatic conditions sufficient for simultaneous agglomeration of first barrier metal powder and reduction in oxygen content in said powder. Said interaction produces component consisting of second barrier metal powder containing barrier metal particles with reduced oxygen content. Note here that nonstatic conditions include agitating, dropping, rotating and combination thereof. Note also that reducing component is selected from the group comprising magnesium, calcium, aluminium, lithium, barium and strontium reducing components and combination thereof.
EFFECT: powder with greater surface area, bulk density and plasticity.
FIELD: process engineering.
SUBSTANCE: invention relates to production of high-quality powders of heat-resistant metals. In compliance with proposed method, powder containing magnesium tantalate and/or niobate is produced. Said powder is heated in inert atmosphere in the presence of magnesium, calcium and/or aluminium to temperature sufficient for removal of magnesium tantalate and/or magnesium niobate from the powder, and/or it is heated in vacuum to temperature sufficient for removal of magnesium tantalate and/or magnesium niobate from the powder. Note that heating is carried out in whatever sequence.
EFFECT: production, minimisation or elimination of magnesium tantalite/niobate presence.
22 cl, 3 tbl, 2 ex
FIELD: technological processes.
SUBSTANCE: present invention relates to a method of reducing primary powder of valve metals and tantalum powder, suitable for use as anode material for electrolytic capacitors. The powder of valve metals is reduced by reducing metals such as aluminium, magnesium, calcium, barium and/or lanthanum and/or their hydrides, in an atmosphere of an inert carrier gas. Reduction is carried out without contact between the reduced powder of valve metals and the liquid reducing metal/metal hydride. The powdered metal and reducing metal/metal hydride are put into a reactor in different places so that the reducing metal/metal hydride can reach the powdered metal only in vapour form. Tantalum with specific surface area of 4-8 m2/g is pressed to density of 5 g/cm3 and sintered at 1210°C for 10 minutes. The obtained anode is formed at formation anode of up to 10 V has specific capacitance of 220000-350000 mcFV/g. Tantalum powder with specific surface area of 3.5-6 m2/g is pressed to density of 5 g/cm3 and sintered at 1210°C for 10 minutes. The obtained anode which is formed at formation voltage of up to 10 V has specific capacitance of 180000-250000 mcFV/g.
EFFECT: reduced aggregation of primary structures, high specific capacitance of capacitors made from the prepared powder.
21 cl, 5 dwg, 4 tbl, 12 ex
FIELD: process engineering.
SUBSTANCE: invention relates to reclamation of barrier metal powders, namely those of niobium, tantalum or alloys thereof. For this, metal is heated to temperature that exceeds melting point of reclaiming material. The latter is most frequently represented by lanthanum, yttrium or cerium. In using lanthanum, reclamation is performed at 940-1150°C. Besides reclamation is carried out in two stage. Note that barrier metal powder is reclaimed that has been produced in reclaiming barrier metal oxide by gaseous lanthanum, yttrium or cerium.
EFFECT: powder with low content of sodium, potassium and magnesium, production of capacitors with high specific capacitance.
6 cl, 5 ex
FIELD: process engineering.
SUBSTANCE: invention relates to powder metallurgy. Component of oxide particles is mixed with reducing agent to form homogeneous mix. Obtained mix is fed into furnace for it to be ignited to initiate the exothermal reaction and produce high-temperature flashout. Note here that said mix is fed by disperser other than rotor/stator disperser to distribute it uniformly over the furnace cross section area, while mix furnace reaction zone location time TR varies from 0.1 s to 30 s. Oxide particles are selected from the group including refractory metal oxides, particles of refractory metal oxide alloys, powders of refractory metal sub oxides, powders of refractory metal sub oxides alloys and mixes thereof. Reducing agent is selected from the group including magnesium, aluminium, potassium and mixes thereof. In compliance with one of the versions, exothermal reaction is initiated at constant rate, while reaction zone temperature equal to flashout temperature is set to be constant. Besides exothermal reaction is initiated by heating the mix to ignition temperature or adding another reagent or catalyst.
EFFECT: uniform mix distribution, higher degree of reduction.
42 cl, 5 tbl, 7 dwg, 2 ex
SUBSTANCE: invention refers to production of powders of valve metals, particularly to niobium and tantalum powders. Powders of oxides of corresponding valve metals are reduced by means of vaporous reducing metals and/or their hydrides, preferably at presence of inert gas-carrier. Reduction is carried out at partial pressure of reducing metal/metal hydride from 5 to 110 gPa and general pressure less 1000 gPa. Tantalum powder with specific surface 0.9-6 m2/g w reveals stability of agglomerates determined as ratio D50-value according to ASTM B 822 and value D50uv less, than 2, is more preferable; less, than 1.7, the most preferable, less, than 1.5 measured after ultrasonic treatment.
EFFECT: production of powder possessing high stability of agglomerates.
14 cl, 2 tbl, 4 dwg, 16 ex
SUBSTANCE: method involves treatment of fine-grained concentrate by extracting agent - aliphatic alcohol saturated with hydrogen fluoride acid so that pulp is used. It is exposed and mixed with conversion of the main part of niobium and tantalum fluorides to organic phase, and titanium, calcium, lanthanides and the rest part of niobium and tantalum fluorides are concentrated in solid phase. Then pulp is clarified and extract is removed from solid phase. As extracting agent there used is pentanol or its mixture with octanol-1 or decanol at pentanol content in mixture of not less than 20% and at saturation of extracting agent with hydrogen fluoride acid till concentration is 119-184 g/l. Treatment of the concentrate with extracting agent is performed at the ratio S:L=1:7.5-10.
EFFECT: increasing the concentrate opening degree and degree of conversion of niobium to organic phase at providing high tantalum extraction degree.
2 cl, 8 ex
SUBSTANCE: method includes heating of charge, containing oxygenous or oxygenous and oxygen-free composition of tantalum or niobium and halogenide of alkali metal with formation of melt. Into melt it is introduced alkali metal at blending and it is implemented reduction of tantalum or niobium at temperature 550-850°C. Additionally amount of oxygen in melt is regulated by means of changing of ratio of components of harge according to relation where n(O) - amount of oxygen, mol, k - empirically determined coefficient, k=60-350 mol, m1 and M1 - mass and molar mass of oxycompound of tantalum or niobium correspondingly in kg and kg/mol, m2 and M2 - mass and molar mass of oxygen-free composition of tantalum or niobium correspondingly in kg and kg/mol, m3 and M3 - mass and molar mass of alkali metal halogenide correspondingly in kg and kg/mol.
EFFECT: increased purity of powder, increasing of its specific surface area.
5 cl, 1 tbl, 7 ex
SUBSTANCE: invention elates to metallurgical field, particularly to device for receiving of tantalum powder of condensing grade by magnesium-thermal recovery. Device contains heated rotating tubular reactor with rotating drive and magnesium evaporator. Reactor allows on inner surface of rib. Additionally evaporator and reactor are implemented in the form of sections of united horizontally located block, divided to each other by partition with central opening and are placed into waterproof vessel. Additionally vessel is outfitted by thermal shield, located from the side of input of rotating drive and is heated by furnace with zonal heating.
EFFECT: there is provided consistent regeneration and increasing of evaporating surface of magnesium and prevention of formation in it of oxide, evaporation rate enhancing of magnesium, more efficient usage of evaporator volume.
SUBSTANCE: procedure consists in leaching at atmospheric or raised pressure, in production of effluent and in utilisation of ion-exchanging resins for absorption and extraction of nickel and cobalt. Before extraction of nickel and cobalt effluent in form of solution or pulp is treated with cation or chelate resin possessing selectivity relative to extraction of iron, aluminium and copper for their removal; it also increases pH of solution.
EFFECT: elimination of neutralisation stage of solution, efficient purification of effluent, prevention of nickel losses and avoiding division of solid and fluid phase of formed pulp at laterite ore leaching.
6 cl, 2 dwg
SUBSTANCE: procedure for extraction of scandium consists in extracting scandium out of producing sulphuric acid solution whereto alkali agent is added before extraction to bring its acidity to pH equal to 2.5-3.0 on solid extractant (SOLEX) with raised selectivity to scandium. Further, scandium is re-extracted from the SOLEX after complete extraction by processing it with solution of fluorine-hydrogen acid at ratio 1:3 of water and organic phases. Successively, scandium fluoride is settled and the SOLEX is washed. Before re-extraction the SOLEX is after-saturated with a part of concentrated solution of scandium produced from preceding re-extraction. Extraction and re-extraction are performed in the same sorption unit; spent sulphuric acid solution and the SOLEX washed with water are returned for extraction of scandium. The procedure for production of the SOLEX consists in synthesis of styrene-di-vinyl-benzene with di-2-ethyl-hexyl ether of phosphoric acid at presence of initiator of copolymerisation. As initiator there is used di-nitrile of azo-di-izobutyric acid to increase strength properties of granules of extractant at the following ratio, wt %: di-2-ethyl-hexyl ether of phosphoric acid - 40-60, di-nitrile of azo-di-izobutyric acid - 3-5, ammine-methyl-phosphonic acid - 3-5, styrene-di-vinyl-benzene - the rest. Produced mixture is poured with distilled water and heated at equal ratio of water and organic phases, overflowed through a sieve and rapidly cooled at continuous mixing with formation of porous granules of the SOLEX which are cut and dried.
EFFECT: efficient process for extraction of scandium.
4 cl, 1 tbl, 4 ex
SUBSTANCE: production of Mo-99 consists in filling solution reactor with fuel solution of uranyl-sulphate, in starting reactor up to specified power, in forming Mo-99 in fuel solution, in reactor shut-down, in conditioning fuel solution for decay of short-lived radionuclide and in sorption of Mo-99 from solution. Also, after reactor shut-down fuel solution is poured out of the reactor into at least one nuclear-safe reservoir; fuel solution is conditioned in this nuclear-safe reservoir. An empty reactor is repeatedly filled with fuel solution, is started up to specified power and Mo-99 is repeatedly generated in fuel solution. For the period of Mo-99 generation in the fuel reactor poured fuel solution in the nuclear-safe reservoir is conditioned. Mo-99 is sorbed from conditioned fuel solution by pumping it through at least one sorption column wherefrom Mo-99 is sorbed into at least one nuclear-safe reservoir for fuel solution conditioning. Fuel solution is conditioned, if necessary. Repeatedly emptied reactor is filled with fuel solution from the nuclear-safe reservoir for fuel solution conditioning.
EFFECT: raised efficiency of solution reactor producing Mo-99 under discrete mode due to reduced idle time.
9 cl, 1 dwg, 1 ex
SUBSTANCE: procedure consists in saturating pulp prepared from ore with oxygen and in introducing leaching reagents and sorbents. Further, there are performed sorption leaching with saturation of sorbent with metal impurities and partially with valuable metals, in counter-flow sorption of base part of valuable metals and in withdrawing sorbents saturated with valuable metals. Also, before introduction of leaching reagents activating solution, treated with light radiation in ultraviolet region of spectre or photo-electro-chemically treated, is introduced into pulp prepared out of ore containing valuable metals in dispersed form. Sorption leaching is carried out in electric field for electro-sorption extraction of primarily leached metals with periodic withdrawal of sorbent from zone of electro-sorbtion.
EFFECT: reduced losses of industrially valuable metals.
SUBSTANCE: procedure consists in production of sample containing uranium and silicon dioxide, in treatment of sample containing uranium and silicon dioxide and in production of material containing dissolved uranium and silicon dioxide. Also, material contains SiO2 over or equal to 100 mg/l. Further, dissolved uranium is extracted from material using at least one strong base anion-exchanging resin of macro-reticular structure. There is obtained uranium containing product in combination with strong-base anion-exchanging resin of macro-reticular structure. Further, uranium containing product is eluted and extracted from combination with strong-base anion-exchanging resin of macro-reticular structure.
EFFECT: increased efficiency of uranium extraction from mediums with high contents of silicon dioxide.
9 cl, 3 tbl, 1 ex
SUBSTANCE: procedure consists in acid extraction of compounds of rare earth elements from phospho-gypsum by mixing extract suspension, in separation of insoluble sedimentation of crystal gypsum from extraction solution and in extracting compounds of rare earth elements from extraction solution. Also, acid extraction is performed with solution of mixture of sulphuric and nitric acids at ratio from 3.2 to 1.2 and concentration from 1 to 3 wt % at ratio L:S (liquid : solid) from 4 to 5 during 8-12 min with simultaneous hydro-acoustic effect onto mixed extraction suspension. Rare earth elements are extracted from extraction solution by means of cation-exchanging sorption with infiltration of extraction solution through cation-exchanging filter.
EFFECT: increased degree of extraction of rare earth elements and 2 times reduced time for process at lower concentrations and volumes of acid reagents.
3 cl, 2 tbl, 4 ex
SUBSTANCE: procedure consists in underground leaching nickel with solution of sulphuric acid and in pumping product solution out. Further, acidity of product solution is reduced, and nickel is sorbed on ionite resin with its following desorption. Upon desorption raffinate of nickel sorption is made-up with sulphuric acid and directed to leaching as leaching solution. Also, excessive sulphuric acid is sorbed on separate ionite with following desorption for reduction of product solution acidity. Upon nickel sorption raffinate is made-up with sulphuric acid and with sulphuric acid after operation of its desorption.
EFFECT: simplification of process, increased ecological safety and reduced consumption of sulphuric acid.
1 dwg, 1 tbl
SUBSTANCE: invention relates to method of extracting stibium from sulphate solutions. Proposed method comprises sorption on anionite and desorption of stibium from anionite by desorption solution. Sorption is carried out using Lewatit K 5517 anionite, while desorption is made via feeding desorption solution through stationary anionite layer at the rate of 0.35-0.46 m/h at 45-50°C. Desorption solution represents disulphide alkaline solution with molar ratio S/NaOH=0.5 and/or alkaline solution of sodium sulphide with sodium concentration of at least 26 g/l.
EFFECT: stibium extraction and increased stibium concentration in solution intended for electrolysis.
3 dwg, 3 tbl
SUBSTANCE: invention relates to method of extracting stibium and arsenium from solution of gold-containing concentrate bioleach solutions. Proposed method comprises sorption of stibium and arsenium on anionite. Note here that sorption is performed on Lewatit K 5517 anionite, and stibium and arsenium are desorbed there from. Prior to desorption, anionite is subjected to sulphuric-acid washing out of iron deposit. Washing-out comprises rinsing by 1.2-1.3%-sulphuric acid with S:L ratio equal to 1:4 at 45-50°C, flow rate of rinsing solution in anionite of 1.0-1.3 m/h, and dissolution of iron (III). Then, remaining iron (III) is washed out by 3%-solution of sodium sulphite at pH=1.5 and S:L=2.
EFFECT: higher yield of stibium and arsenium due to selective wags-out of iron for further desorption of them.
3 dwg, 1 tbl
SUBSTANCE: invention relates to the method of processing sulphide gold-containing concentrates. Proposed method comprises bioleach of concentrate involving stibium dissolution and extraction from solution by sorption. Note here that stibium sorption from bioleach solution is carried out on anionite Lewatit K 5517 at 45-50°C, anionite flow rate making 50-100 g/l of solution for 8-10 hours. After sorption, desorption is carried out.
EFFECT: expanded process performances, increased extraction of stibium of gold-containing ores.
2 dwg, 1 tbl, 1 ex
SUBSTANCE: invention relates to sorption-mediated recovery of molybdenum from solutions containing heavy metal cations. Method of invention comprises providing solution to be treated, sorption of molybdenum(VI) on anionite at pH < 7. Sorption is conducted from solutions with anionites AM-2b and AMP at solution pH below pH of hydrolytic precipitation of heavy metal cations but higher than pH of formation of molybdenum cations (pH ~ 1).
EFFECT: increased process selectivity and reduced number of stages in preparation of pure molybdenum.
9 dwg, 3 tbl, 4 ex