Method of extracting scandium

FIELD: chemistry.

SUBSTANCE: invention relates to hydrometallurgical processing of mineral material, particularly scandium-containing "tailings" obtained during beneficiation of titanium-magnetite ore by wet magnetic separation. The method of extracting scandium is three-step sulphuric acid leaching of scandium, wherein at the first step, leaching is carried out with recycled solution after extraction of scandium at temperature of 30-50°C and solid to liquid ratio of 1:6-7 for 3-4 hours; the pulp is then divided into a solid phase and a liquid phase; at the second step, a portion of the solution obtained from the first step is returned to the solid phase and sulphuric acid is added to concentration of 340-360 g/l and sodium fluoride is added in amount of 20-25 kg fluorine/t solid; leaching is carried out at temperature of 95-98°C and solid to liquid ratio of 1:2.5-3 for 3-4 hours; further, at the third step, the pulp is diluted in solid to liquid ratio of 1:6.5-7.5; treatment is carried out at temperature of 95-98°C for 3-4 hours.

EFFECT: invention increases extraction of scandium, cuts the overall duration of the leaching process and consumption of sulphuric acid and sodium fluoride.

3 ex, 1 tbl

 

The invention relates to the hydrometallurgical processing of mineral raw materials, in particular, to the scandium-containing "tails", obtained during the concentration of magnetite ores by the method of wet magnetic separation.

The known method of two-stage acid leaching with the use of fluoride supplements [RF patent №2034074, SW 59/00], namely, that at the first stage is supplied the raw materials and the solution after extraction of scandium. The leaching is conducted at a temperature of 95°C for 3 h, when the residual acidity 35 g/l In the second stage, the solid residue after filtration leached with sulfuric acid in the presence of potassium fluoride at a temperature of 95°C for 12 h with residual acidity 198 g/l Consumption of sulfuric acid was 1.2 t/t and potassium fluoride in terms of fluorine 30 kg/so the Extraction of scandium 71,9%.

However, this method is associated with high consumption of sulfuric acid. The authors proposed a three-stage process for the recovery of scandium from the tailings of magnetic separation, comprising leaching with sulfuric acid in the presence of sodium fluoride, and recycling the obtained solutions. The first stage is served raw materials and working capital solution after extraction of scandium, sulfuric acid. Then the slurry is separated by filtration. In the second stage uses a portion of the obtained filtrate, sulfur is added to the slot and sodium fluoride. In the third stage, the liquid phase is diluted twice, sulfuric acid is not added.

The technical result of the invention is to reduce the total time leaching up to 12 hours, the consumption of sulfuric acid up to 860 kg/t of sodium fluoride in terms of fluorine up to 23 kg/t and increasing recovery of scandium to 78%.

The technical result is achieved by the fact that scandium is extracted from the tailings of magnetic separation. Leaching of lead in three stages, with the first stage leaching lead working solution after extraction of scandium at a temperature of 30-50°C, and the ratio of T:W=1:6-7 for 3-4 h, and then the slurry is separated into solid and liquid phases, in the second phase to the solid phase of the return of the obtained solution from the first stage and add sulfuric acid to a concentration of 340-360 g/l and sodium fluoride 20-25 kg of fluorine/t solid, leaching is carried out at a temperature of 95-98°C and a ratio of T:W=1:2.5 to 3 for 3-4 h, then in the third stage, the pulp is diluted in the ratio T:W=1:6,5-7,5 processing is carried out at a temperature of 95-98°C for 3-4 hours

The essence of the proposed method can be explained as follows.

Example 1. The proposed method was tested on the "tails" enrichment of titanium-magnetite ores by the method of wet magnetic separation, containing 0,012% scandium. The first stage is served raw materials and working solution after extracts and scandium, containing 106 g/l of sulfuric acid and 100 kg/t of free sulfuric acid. The leaching is conducted at a temperature of 30°C and a ratio of T:W=1:6 for 3 h, the residual acidity of 55 g/L. Then the pulp is separated by filtering.

Second stage is to use 50% of the volume of the obtained filtrate is added sulfuric acid in the amount of 750 kg/t to the concentration of 340 g/l Consumption of sodium fluoride in terms of fluorine 20 kg/so the Leaching is carried out at a ratio of solid to liquid T:W=1:2.5 V for 3 h at 95°C. the residual acidity of 175 g/L.

In the third stage, the pulp is diluted to the ratio of T:W=1:6,5. Sulfuric acid is not added. Processing time 3 h at 95°C. the residual acidity of 106 g/l

Using this technology, the total leaching time 9 h, the consumption of sulfuric acid 850 kg/t of sodium fluoride in terms of fluorine 20 kg/t, the degree of extraction of scandium in a solution of 70%, the content of scandium in the cake 0,0036%.

Example 2. On a similar sample from example 1 were carried out researches. The first stage is served raw materials and working capital solution after extraction of scandium containing 100 g/l of sulfuric acid and 100 kg/t of free sulfuric acid. The leaching is conducted at a temperature of 40°C and a ratio of T:W=1:7 for 4 hours residual acidity 45 g/L. the resulting slurry, after the first stage is separated by filtering.

The second with the adiya's used 50% of the volume of the obtained filtrate, added sulfuric acid in the amount of 760 kg/t to the concentration of 356 g/l Consumption of sodium fluoride in terms of fluorine 23 kg/so the Leaching is carried out at a ratio of solid to liquid T:W=1:3 for 4 h at 95°C. the residual acidity of 170 g/l

In the third stage, the pulp is diluted to the ratio of T:W=1:7. Sulfuric acid is not added. The processing time of 4 h at 95°C. the residual acidity of 100 g/l

Using this technology, the total leaching time of 12 h, the consumption of sulfuric acid 860 kg/t of sodium fluoride in terms of fluorine 23 kg/t, the degree of extraction of scandium in the solution to 78.3%, the content of scandium in the cake 0,0026%.

Example 3. Research conducted on material from example 1 containing scandium 0,012%. The first stage is served raw materials and working capital solution after extraction of scandium containing 93 g/l of sulfuric acid and 105 kg/t of free sulfuric acid. Leaching was carried out at 50°C and a ratio of T:W=1:7 for 4 hours residual acidity 41 g/L. Then the pulp is separated by filtering.

Second stage is to use 50% of the volume of the obtained filtrate is added sulfuric acid in the amount of 770 kg/t to the concentration of 360 g/l Consumption of sodium fluoride in terms of fluorine 25 kg/so the Leaching is carried out at a ratio of solid to liquid T:W=1:3 for 4 hours at a temperature of 98°C. the residual acidity 170 is/L.

In the third stage, the pulp is diluted to the ratio of T:W=1:7,5. Sulfuric acid is not added. The processing time of 4 h at a temperature of 98°C. the residual acidity of 93 g/l

Using this technology, the total leaching time of 12 h, the consumption of sulfuric acid 875 kg/t of sodium fluoride in terms of fluorine 25 kg/t, the degree of extraction of scandium in a solution of 80%, the content of scandium in the cake 0,0024%.

Data examples are summarized in table 1.

When the ratio of T:W=1:6 there is extraction of scandium in a solution of 54%, the content of scandium in the KEK - 00,55%.

When the ratio of T:W=1:8 extraction of scandium in the solution does not change, but increases the consumption of reagents and equipment volume.

The method of extraction of scandium, including multi-stage leaching with sulfuric acid using fluoride additives, characterized in that the extraction of scandium lead from the tailings of magnetic separation by three-stage acid leaching, with the first stage leaching lead working solution after extraction of scandium at a temperature of 30-50°C, and the ratio of T:W=1:6-7 for 3-4 h, and then the slurry is separated into solid and liquid phases, in the second phase to the solid phase of the return of the obtained solution from the first stage and add sulfuric acid to a concentration of 340-360 g/l and sodium fluoride 20-25 kg of fluorine/t solid, videla is ivanie carried out at a temperature of 95-98°C and a ratio of T:W=1:2.5 to 3 for 3-4 h, next, in the third stage, the pulp is diluted in the ratio T:W=1:6,5-7,5, processing is carried out at a temperature of 95-98°C for 3-4 hours



 

Same patents:

FIELD: metallurgy.

SUBSTANCE: proposed method comprises sulfuric acid leaching of scandium from red mud, pulp filtration, scandium sorption from sulfuric acid solutions, desorption from organic phase by carbonate solution to obtain column effluent. Then, scandium poorly soluble compounds are precipitated from column effluent, precipitate is filtered out, flushed, dried and annealed to get scandium-bearing concentrate. Note here that said leaching is performed by 10.0-13.5%-sulfuric acid at pulp initial vibration cavitation at rotary velocity of 35-60 m/s for 15-35 min. Scandium is precipitated from column effluent by potassium caprinate in amount of 75-100 g/t of scandium at pH 3.5-4.5 and exposure for 15-25 min.

EFFECT: increased yield.

3 cl, 2 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises extraction of rare-earth metal cations by organic phase including extragent solution in inert diluter. Naphthenic acid is used as said extragent. Kerosene is used as inert diluter. Extraction is conducted in three stages at relationship between organic and aqueous phases O:A=1·(9-11) at every stage. Note here that, at first stage, europium cations (III) are extracted at content of naphthenic acid in kerosene of 10-13 vol. % and aqueous solution pH 5.0-5.1. At second stage, samarium cations (III) are extracted at content of naphthenic acid in kerosene of 13-16 vol. % and aqueous solution pH 4.6-4.7. At third stage cerium and lanthanum cations (III) are extracted at the same content of extragent and pH 5.0-5.1.

EFFECT: higher yield.

4 dwg, 1 ex

FIELD: metallurgy.

SUBSTANCE: method of extracting rare-earth metals from solutions containing iron (III) and aluminium comprises sorption of rare-earth metals on sorbent. Ampholyte with iminodiacetic functional groups is used as said sorbent. Sorption is carried out after preliminary neutralisation or acidification of solution to pH 4-5 by whatever alkaline or acid agent to add ampholyte in obtained pulp with separation of solid fraction. Sorption is conducted at ampholyte:pulp ratio of 1:50-1:150, phase contact time of 3-6 h and in the presence of reducing agent.

EFFECT: higher selectivity.

5 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of separating deactivated rare-earth elements during nitric acid treatment of apatite concentrate from nitrate-phosphate solutions. The method of treating a rare-earth phosphate concentrate isolated from apatite involves decomposition of the rare-earth phosphate concentrate with nitric acid, treating the obtained solution with oxalic acid with precipitation of rare-earth oxalates in two steps, at the first step of precipitation of oxalates of thorium and rare-earth elements, 5-10% oxalic acid in stoichiometric amount is added to rare-earth elements present in the solution, and at the second step of precipitation of rare-earth oxalates, 110-115% oxalic acid in stoichiometric amount is added to rare-earth elements present in the initial solution, and the rare-earth oxalates are then calcined to rare-earth oxides.

EFFECT: invention provides high economic efficiency of the process, which is achieved by avoiding the need to process and bury the precipitate containing thorium.

3 cl, 2 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises multistep leaching of red slag by the mix of sodium carbonate and bicarbonate on forcing annealing furnace flue gases containing carbon dioxide there through to obtained solution. Then, three-step holding of said solution at increased temperatures is performed along with selective separation of precipitates after every said step. At first step, said solution is heated to temperature not exceeding 80°C for, at least, 1 hour. Thereafter, it is settled for, at least, two hours at natural cooling. At second step, said solution is boiled and mixed for, at least, two hours. At third step, said solution is evaporated to 50% of initial volume to add 46%-solution of sodium hydroxide to concentration of Na2Ocaustic of 1.5-2.0 kg/m3. Now, it is boiled for, at least, 2 hours and precipitate containing scandium oxide is settled for 10-16 hours at natural cooling.

EFFECT: simplified process, higher yield of scandium oxide.

1 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to hydrometallurgy, in particular, to the method for extraction of europium (III) from salt solutions by floating extraction. In process of floating extraction of europium (III) cations the organic phase is represented by isooctyl alcohol, and the collector of surfactants of anion type is sodium sodium dodecyl sulfate in the concentration corresponding reaction stoichiometry: Eu+3+3NaDS=Eu(DS)3+Na+, where Eu+3 - cation of europium (III), DS- - dodecyl sulfate-ion. At the same time the floating extraction is carried out at pH=7.5-8.5, and at the ratio of organic and water phases 1/20-1/40.

EFFECT: increased extent of europium (III) extraction.

2 dwg

FIELD: metallurgy.

SUBSTANCE: invention refers to non-ferrous metallurgy, and namely to complex processing of red muds of alumina industry. Processing method of red muds of alumina industry involves obtaining of red mud pulp, extraction and concentration of rich components by combination of classification and magnetic separation methods. After the pulp classification, fine-grain fraction pulp is extracted and subject to vibrocavitation treatment and further magnetic separation with extraction of magnetic and non-magnetic products. At that, magnetic product is subject to additional classification so that iron-bearing and scandium-bearing concentrates are obtained.

EFFECT: increasing the complexity degree of processing of red muds owing to increasing the extraction degree of rich components to target products - scandium-bearing concentrate and iron oxide concentrate.

4 cl, 3 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises dissolving scandium-bearing concentrate in sulfuric acid, removing acid-insoluble residue, and precipitating scandium in the presence of ammonium compounds. Then, precipitate is filtered, flushed, dried and calcined to obtain scandium oxide precipitate. With acid-insoluble residue removed, sulfuric acid concentration in filtrate is increased to 540-600 g/dm3, ammonium chloride is added to solution in amount of 26.7-53.5 g/dm3 at 50-70°C and held for one hour at mixing. Produced precipitate is flushed by ethanol at volume ratio of 1-10-11.

EFFECT: simplified process, higher purity scandium oxide.

3 ex

FIELD: chemistry.

SUBSTANCE: method of extracting yttrium (III) from salt solutions involves floatation extraction using an organic phase and a collector. The organic phase used is isooctyl alcohol. The collector used is an anionic surfactant - sodiium dodecyl suphate in a concentration which corresponds to the stoichiometry: Y+3+SDS-=Y[DS]3, where Y+3 is a yttrium cation, DS- is a dodecyl sulphate ion. Floatation extraction is carried out at pH=7.0-7.8 and ratio of the organic phase to the aqueous phase of 1/20-1/40.

EFFECT: high degree of extraction of yttrium.

2 dwg, 1 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to complex processing method of carbon-silicic black-shale ores, which contain vanadium, uranium, molybdenum and rare-earth elements. The above method involves ore crushing to the particle size of not more than 0.2 mm and two leaching stages. Oxidation sulphuric-acid leaching is performed at atmospheric pressure. Autoclave oxidation sulphuric-acid leaching is performed at the temperature of 130-150°C in presence of oxygen-containing gas and addition of a substance forming nitrogen oxide, as a catalyst of oxygen oxidation. Ion-exchange sorption of uranium, molybdenum, vanadium and rare-earth elements is performed from the obtained product solution.

EFFECT: increasing extraction degree of vanadium, uranium, molybdenum; improving the complexity of ore use owing to associated extraction of rare-earth elements.

18 cl, 1 dwg

FIELD: process engineering.

SUBSTANCE: invention relates to nonferrous metallurgy and may be used for metallothermic production of nanocrystalline niobium powders, mainly, for electrolytic capacitors. Niobium oxide compound, magnesium or calcium niobate, is reduced by vapors of magnesium or calcium. Reduction by magnesium vapors is carried at 600-950°C and by calcium vapors at 950-1050°C for 2-9 hours. Said reduction is performed in either vacuum at residual pressure of 1.3-13.3 Pa or atmosphere of argon or helium at 1-50 kPa. Reduction products are processed by solution of mineral acid to remove formed magnesium or calcium oxides. Obtained powder is flushed with deionised water to neutral state and dried.

EFFECT: niobium powder specific surface increased to 73 m2/g that corresponds to niobium particle size of 9,6 nm, content of magnesium and calcium impurities makes (8-31)·10-4 and (7-15)·10-4 wt %, respectively, oxygen content does not exceed 0,27 wt % per m2.

4 cl, 10 ex, 1 tbl

FIELD: metallurgy.

SUBSTANCE: proposed method comprises sulfuric acid leaching of scandium from red mud, pulp filtration, scandium sorption from sulfuric acid solutions, desorption from organic phase by carbonate solution to obtain column effluent. Then, scandium poorly soluble compounds are precipitated from column effluent, precipitate is filtered out, flushed, dried and annealed to get scandium-bearing concentrate. Note here that said leaching is performed by 10.0-13.5%-sulfuric acid at pulp initial vibration cavitation at rotary velocity of 35-60 m/s for 15-35 min. Scandium is precipitated from column effluent by potassium caprinate in amount of 75-100 g/t of scandium at pH 3.5-4.5 and exposure for 15-25 min.

EFFECT: increased yield.

3 cl, 2 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises sulfuric acid leaching of scandium from red mud, pulp filtration, scandium sorption from sulfuric acid solutions, desorption from organic phase by carbonate solution to obtain column effluent. Then, scandium poorly soluble compounds are precipitated from column effluent, precipitate is filtered out, flushed, dried and annealed to get scandium-bearing concentrate. Note here that said leaching is performed by 10.0-13.5%-sulfuric acid at pulp initial vibration cavitation at rotary velocity of 35-60 m/s for 15-35 min. Scandium is precipitated from column effluent by potassium caprinate in amount of 75-100 g/t of scandium at pH 3.5-4.5 and exposure for 15-25 min.

EFFECT: increased yield.

3 cl, 2 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises extraction of rare-earth metal cations by organic phase including extragent solution in inert diluter. Naphthenic acid is used as said extragent. Kerosene is used as inert diluter. Extraction is conducted in three stages at relationship between organic and aqueous phases O:A=1·(9-11) at every stage. Note here that, at first stage, europium cations (III) are extracted at content of naphthenic acid in kerosene of 10-13 vol. % and aqueous solution pH 5.0-5.1. At second stage, samarium cations (III) are extracted at content of naphthenic acid in kerosene of 13-16 vol. % and aqueous solution pH 4.6-4.7. At third stage cerium and lanthanum cations (III) are extracted at the same content of extragent and pH 5.0-5.1.

EFFECT: higher yield.

4 dwg, 1 ex

FIELD: metallurgy.

SUBSTANCE: method of extracting rare-earth metals from solutions containing iron (III) and aluminium comprises sorption of rare-earth metals on sorbent. Ampholyte with iminodiacetic functional groups is used as said sorbent. Sorption is carried out after preliminary neutralisation or acidification of solution to pH 4-5 by whatever alkaline or acid agent to add ampholyte in obtained pulp with separation of solid fraction. Sorption is conducted at ampholyte:pulp ratio of 1:50-1:150, phase contact time of 3-6 h and in the presence of reducing agent.

EFFECT: higher selectivity.

5 tbl, 5 ex

FIELD: metallurgy.

SUBSTANCE: method of processing manganese oxide materials containing heterovalent manganese oxides comprises leaching crushed raw stock by sulfuric acid aqueous solution in the presence of bivalent iron sulphate, iron precipitation and manganese extraction from productional solution. Note here that said leaching is performed on adding reducing agent in the form of metal iron or iron sulphate (Fe2+) at 60-95°C for 60-300 min. Leaching is carried out at initial concentration of H2SO4 in leaching solution of up to 100 g/dm3 and final acidity in productional solution relative to hydrogen ion exponent pH<2.

EFFECT: higher manganese yield.

1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to methods of separating deactivated rare-earth elements during nitric acid treatment of apatite concentrate from nitrate-phosphate solutions. The method of treating a rare-earth phosphate concentrate isolated from apatite involves decomposition of the rare-earth phosphate concentrate with nitric acid, treating the obtained solution with oxalic acid with precipitation of rare-earth oxalates in two steps, at the first step of precipitation of oxalates of thorium and rare-earth elements, 5-10% oxalic acid in stoichiometric amount is added to rare-earth elements present in the solution, and at the second step of precipitation of rare-earth oxalates, 110-115% oxalic acid in stoichiometric amount is added to rare-earth elements present in the initial solution, and the rare-earth oxalates are then calcined to rare-earth oxides.

EFFECT: invention provides high economic efficiency of the process, which is achieved by avoiding the need to process and bury the precipitate containing thorium.

3 cl, 2 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises multistep leaching of red slag by the mix of sodium carbonate and bicarbonate on forcing annealing furnace flue gases containing carbon dioxide there through to obtained solution. Then, three-step holding of said solution at increased temperatures is performed along with selective separation of precipitates after every said step. At first step, said solution is heated to temperature not exceeding 80°C for, at least, 1 hour. Thereafter, it is settled for, at least, two hours at natural cooling. At second step, said solution is boiled and mixed for, at least, two hours. At third step, said solution is evaporated to 50% of initial volume to add 46%-solution of sodium hydroxide to concentration of Na2Ocaustic of 1.5-2.0 kg/m3. Now, it is boiled for, at least, 2 hours and precipitate containing scandium oxide is settled for 10-16 hours at natural cooling.

EFFECT: simplified process, higher yield of scandium oxide.

1 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises multistep leaching of red slag by the mix of sodium carbonate and bicarbonate on forcing annealing furnace flue gases containing carbon dioxide there through to obtained solution. Then, three-step holding of said solution at increased temperatures is performed along with selective separation of precipitates after every said step. At first step, said solution is heated to temperature not exceeding 80°C for, at least, 1 hour. Thereafter, it is settled for, at least, two hours at natural cooling. At second step, said solution is boiled and mixed for, at least, two hours. At third step, said solution is evaporated to 50% of initial volume to add 46%-solution of sodium hydroxide to concentration of Na2Ocaustic of 1.5-2.0 kg/m3. Now, it is boiled for, at least, 2 hours and precipitate containing scandium oxide is settled for 10-16 hours at natural cooling.

EFFECT: simplified process, higher yield of scandium oxide.

1 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises smelting initial material to produce vitreous arsenic trisulfide. Arsenic-bearing sulfide cake is subjected to neutralisation given its moisture content does not exceed 0.5%. Smelting is performed in protective capsule preformed from liquid dump slag at 350-400°C using the heat of said dump slag. Then, buffer layer of heat-insulation material is formed on the surface of obtained cake melt. Now, said protective capsule is sealed by coating its surface with buffer layer of liquid dump slag to be hardened thereafter. Aforesaid heat-insulation layer represents crushed slag and/or quartz sand and/or undersized crushed stone.

EFFECT: higher efficiency.

2 cl, 1 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: method of extracting rare-earth metals from solutions containing iron (III) and aluminium comprises sorption of rare-earth metals on sorbent. Ampholyte with iminodiacetic functional groups is used as said sorbent. Sorption is carried out after preliminary neutralisation or acidification of solution to pH 4-5 by whatever alkaline or acid agent to add ampholyte in obtained pulp with separation of solid fraction. Sorption is conducted at ampholyte:pulp ratio of 1:50-1:150, phase contact time of 3-6 h and in the presence of reducing agent.

EFFECT: higher selectivity.

5 tbl, 5 ex

Up!