Method of recovering rare-earth elements from eudialyte concentrate solution subjected to hydrochloric acid decomposition

FIELD: mining industry.

SUBSTANCE: invention relates to rare-earth element recovery technology in integrated processing of mineral stock, especially to hydrogen chloride technology of eudialyte concentrate. Method according to invention comprises introduction of nitrate ion into initial chloride solution containing rare-earth and impurity elements. Chloride-nitrate solution thus obtained is treated with tributyl phosphate extractant to transfer nitrates of rare-earth elements and a part of impurity elements into first organic phase, which is then separated from chloride-nitrate solution to form first extract and first raffinate containing major part of impurity elements. First extract is washed with nitrate solution and wash solution is then returned into initial chloride solution. Rare-earth element nitrates are reextracted with water and first reextract is separated. Concentrated 35-37% hydrochloric acid is added to the first raffinate to provide 5-10% excess of the acid relative to nitrate ion content. Raffinate is treated with tributyl phosphate to transfer nitric acid into second organic phase and to form chloride solution of the major part of impurity elements. Second organic phase is separated to form extract and second raffinate, after which nitric acid is reextracted from the second extract with alkali solution to form second reextract in the form of nitrate solution, which is used to wash the first extract.

EFFECT: increased rare-earth element recovery efficiency under better environmental conditions.

5 cl, 1 dwg, 3 ex

 

The invention relates to a process for the separation of rare earth elements (REE) in the complex processing of mineral raw materials, mainly cleaners containing hydrochloride technologies eudialyte concentrate.

There is a method of separation of rare earth elements from solutions of complex salt composition (see Norina T.M., Mikhlin E.B., V. Nikonov. and other Extraction recovery of REE from solutions of complex salt composition. Proceedings of Giredmet. - M., 1974, t, S-26), including extraction of carboxylic acids at pH 4.5 to 5.0 with translation in the organic phase REE, as well as calcium, iron, aluminum and other impurity elements and their subsequent reextraction nitric acid in the form of nitrates.

The disadvantage of this method is that from solutions of complex salt structure, which include the means of hydrochloric acid solutions decomposition eudialyte concentrate, carboxylic acids extracted all elements having a pH of precipitation is less than or close to the pH of the precipitation of REE. This method does not allow to solve the problem of selective extraction of REE and does not provide for the washing away impurities. In addition, extraction of carboxylic acids requires an equivalent to the extracted elements of alkali consumption and the corresponding number of nitric acid for Stripping REE, which complicates and increases the cost method. All this effectively reduces Yunosti method.

Closest to the claimed is a method of separation of REE from the solution means of hydrochloric acid decomposition eudialyte concentrate (see Lebedev V.N., Rudenko ALEXANDER the extraction of rare earth elements by means of hydrochloric acid from the decomposition of eudialyte. // Chemical technology. 2003. No. 1. P.26-29), including the introduction of the nitrate ion in the form of sodium nitrate in the amount of 1.5-3.0 g-EQ/l in the original chloride solution containing rare earth elements and impurities of calcium, iron, zirconium, etc., processing the obtained chloride-nitrate solution of tributyl phosphate (TBP) in 3-4 steps at A:B=1:1 translation in the organic phase of the nitrates of rare-earth elements and part of the impurity elements calcium, iron, and zirconium, separating the organic phase from the chloride-nitrate solution containing the major part of the impurity elements, with the formation of the extract nitrates rare earth elements and the raffinate output in the form of waste solution, washing the extract solution of sodium nitrate concentration of 4 g-EQ/l with the separation of impurities of calcium, iron, and zirconium, and the return of the leaching solution in the original chloride solution, reextraction nitrates of rare-earth elements water and the Department of reextract. The degree of REE extraction in the organic phase is 98.5-99.8%of the content of nitrate ions in the raffinate is 0.8 - 2.4 g-EQ/liter

The disadvantage of this SPO is both is its lack of effectiveness, as it doesn't involve the utilization of nitrate ions contained in the raffinate. This reduces the environmental friendliness of the way and expensive due to the irreversible flow nitrosoureas reagent.

The technical result of the invention is to improve the efficiency of the method of separation of rare earth elements from the solution means of hydrochloric acid decomposition eudialyte concentrate due to utilization of nitrate ions, while ensuring a high degree of REE extraction. The technical result is also more environmentally friendly way.

This technical result is achieved by the method of separation of rare earth elements from the solution means of hydrochloric acid decomposition eudialyte concentrate, including the introduction of the nitrate ion in the original chloride solution containing rare-earth elements and impurity elements, processing the obtained chloride-nitrate solution extractant in the form of tributyl phosphate with translation of nitrates of rare-earth elements and part of the impurity elements in the first organic phase, separating the first organic phase from the chloride-nitrate solution with formation of a first extract and a first raffinate containing the main part of the impurity elements, the first washing of the extract nitrate solution with the return of the leaching solution in the original chloride solution, R is the extraction of nitrates rare earth elements in water and separating the first reextract, according to the invention in a first raffinate injected with concentrated hydrochloric acid to ensure its excess in relation to the content of nitrate ions, the raffinate is treated with tributyl phosphate with translation of nitric acid in the second organic phase and education chloride solution the main part of the impurity elements, separating the second organic phase with the formation of the second extract and a second raffinate and are reextraction nitric acid from the second extract solution of an alkaline reagent with a second reextract in the form of nitrate solution, which is used as a washing solution for washing the first extract.

The technical result is also achieved by the fact that in the first raffinate enter 35-37% hydrochloric acid to ensure that it is 5-10% excess relative to nitrate ions.

The technical result is also achieved by the fact that the processing of the first raffinate with tributyl phosphate are in the ratio A:B=0,9-1,2:1.

On the technical achievement of the aims that reextraction nitric acid is carried out at the concentration of the alkaline reagent 4,5-8,0 g-EQ/l, with an alkaline reagent taken in stoichiometric quantity with respect to nitric acid.

The achievement of the technical result is strengthened by the fact that, as the alkaline reagent for Stripping nitric acid COI is lsout sodium hydroxide or calcium oxide, you get a second reextract in the form of a nitrate solution of sodium or calcium.

The invention consists in that in the raffinate obtained after REE extraction from chloride-nitrate solution by extraction with tributyl phosphate, introducing concentrated hydrochloric acid with an excess of in relation to nitrate ions and remove nitrate ions extraction of TBP in nitric acid, and a saturated organic phase by treatment with a solution of an alkaline reagent in the form of sodium hydroxide or Cao nitric acid extract in the form of a nitrate solution of sodium or calcium, which return in the process.

Introduction in the first raffinate of concentrated hydrochloric acid to ensure its excess in relation to the content of nitrate ions allows to provide conditions for the effective separation of the nitrate ions. While hydrochloric acid acts as vicariates nitric acid with subsequent extraction of the extract.

Processing the first raffinate with tributyl phosphate with translation of nitric acid in the second organic phase and education chloride solution the main part of the impurity elements driven by higher extractibility of nitric acid tributyl phosphate in comparison with hydrochloric acid and promotes recycling of nitrate ions contained in the first raffinate.

Reextracted azo is Noah acid from the second extract solution of an alkaline reagent caused by the necessity to produce a concentrated nitrate solution, used to wash the extract rare earth elements, which increases the efficiency of the method and reduces the cost of reagents.

Return nitrate solution of an alkaline reagent at the first stage leaching extract helps reduce the irreversible consumption nitrosoureas reagent, while limiting the dilution of the processed solution that reduces the amount of material flow.

The combination of the above features is necessary and sufficient to achieve the technical result of the invention consists in the utilization of nitrate ions, while ensuring a high degree of REE extraction from the solution means of hydrochloric acid decomposition eudialyte concentrate, and more environmentally friendly way. The result is improved efficiency of the method.

In specific cases the invention, it is preferable to use hydrochloric acid with a concentration of 35 to 37% in an amount to provide its 5-10% excess relative to nitrate ions. This allows you to more effectively remove nitrate ions from the first raffinate during treatment with tributyl phosphate. The excess of hydrochloric acid more than 10% leads to a more expensive way of taking into account the additional costs of hydrochloric acid and subsequent neutralization of the chloride solution in the form of the second raffinate.

The extraction of nitric acid by tributyl phosphate Ave is doctitle be carried out at the ratio of organic and aqueous phase 0:In=0,9-1,2:1. The choice of this ratio is due to the fact that with the increase in the ratio above 1 and 2:1 will be a decrease in the concentration of nitric acid in the second organic phase, which is undesirable. When the ratio of the phases is less than 0.9:1 would be undesirable increase speed and decrease the degree of extraction of the acid in the second extract.

Reextracted nitric acid from the second organic phase solution of an alkaline reagent, which is used as sodium hydroxide or calcium oxide with a concentration of 4.5-8.0 g-EQ/l in stoichiometric quantity with respect to nitric acid, due to the need for nitrate solution of sodium or calcium used for washing the first extract rare earth elements. Used the concentration of sodium hydroxide and calcium oxide (4,5-8,0 g-EQ/l) due to the fact that at a concentration of less than 4.5 g-EQ/l increase the volume of processed solutions, at a concentration of more than 8 g-EQ/l there is a risk of crystallization of sodium nitrate and calcium.

The above private features of the invention allow a method to optimally from the point of view of increasing the efficiency of the allocation of REE from the solution means of hydrochloric acid decomposition eudialyte concentrate due to utilization of nitrate ions, while ensuring a high degree of izvlecheniye, as well as improving the environmental performance of the method.

For a clearer understanding of the invention on the accompanying drawing shows a schematic diagram of the separation of rare earth elements from the solution means of hydrochloric acid decomposition eudialyte concentrate.

The method is as follows. In the original chloride solution 1, formed by means of hydrochloric acid decomposition eudialyte concentrate containing rare-earth elements and impurity elements calcium, aluminum, manganese, potassium, sodium, strontium, magnesium and iron, introducing the nitrate-ion 2 in the form of sodium nitrate or calcium nitrate and add nitrate solution 3 (sodium or calcium) from the first washing of the extract to ensure the content of nitrate-ion 1.5 to 3.0 g-EQ/l Obtained chloride-nitrate solution 4 is subjected to extraction processing 5 on a 5-speed counter-current with the use of the extractant 6 in the form of an 80% solution of TBP in dodecane O:=1:1,0-1,6 translation of nitrates of rare-earth elements and part of the impurity elements in the first organic phase. The main part of the impurity elements is in chloride-nitrate solution. After separation of the phases formed first extract 7 and the first raffinate 8. The first extract is washed 7 9 countercurrent on 2 levels nitrate solution 10 sodium or calcium concentration of 4.5-8.0 g-EQ/drug education spent leaching solution of 3, containing part of the impurity elements, and washed first extract 11. The spent leaching solution of 3 return to the original solution 1. Then washed from the first extract 11 are reextraction 12 nitrates of rare-earth elements in 3 counter-current stages with the use of water 13 as extragent. The first reextract 14, enriched REE, is separated from the depleted first organic phase, which is in the form of the extractant 6 return to extraction 5. The degree of REE extraction taking into account the return to the cycle of losses proryvnym solution is by 98.7 99.8 per cent.

Then in the first raffinate 8 impose concentrated 35-37% hydrochloric acid 15 to ensure its 5-10% excess with respect to the content of nitrate ions and subjected to extraction processing 16 extractant 17 in the form of an 80% solution of TBP in dodecane 4-8 stages countercurrent O:In=0,9-1,2:1. The extraction of nitric acid passes into a second organic phase, while the main part of the impurity elements remains in chloride solution. After separation of the phases formed in the second extract 18 and the second raffinate 19, which derive from the process and sent for recycling. The degree of extraction of nitric acid in the second extract is 97-98,5%. From the second extract 18 nitric acid extravert 20 at 1 step solution 21 of sodium hydroxide or calcium oxide is (lime milk) when the concentration of the alkaline reagent 4,5-8,0 g-EQ/l, which are taken in stoichiometric quantity with respect to nitric acid. Forming a second reextract in the form of a nitrate solution of 10 sodium or calcium concentration of 4.5-8.0 g-EQ/l is used as a washing solution for washing the 9 first extract 7. Depleted second organic phase in the form of the extractant 17 return on the extraction of nitric acid 16.

The essence of the proposed method can be explained by the following Examples.

Example 1.

In the solution means of hydrochloric acid decomposition eudialyte concentrate in the amount of 1000 ml, containing, g/l: Ln2About333,0; Cao 75,1; SrO 8,6; Al2About346,5; MnO224,6; Na2O 3.3V; K2O 10,9; MgO 4,6; Fe2About32,1, enter 85 g of sodium nitrate and 200 ml of the spent leaching solution containing 4.5 g-EQ/l of sodium nitrate and 6.8 g/l Ln2About3to ensure the content of nitrate-ion 1.5 g-EQ/l Obtained chloride-nitrate solution was processed for 5-speed countercurrent 1230 ml of extractant in the form of an 80% solution of TBP in dodecane O:In=1:1 translation of nitrates of rare-earth elements and part of the impurity elements in the first organic phase. The main part of the impurity elements is in chloride-nitrate solution. After separation of the phases formed first extract volume 1230 ml, containing, g/l: Ln2O326,5; Cao 1,8; SrO 0,2; Al2About 30,3; MnO20,36; Fe2About31,7; NO3-141,5, and the first raffinate volume 1230 ml, containing, g/l: Ln2About30,38; Cao 59,2; SrO 6,8; Al2About337,5; MnO219,6; Fe2About30,01; NO3-152,9 (0.84 g-EQ/l). The first extract is washed with a counter on 2 levels 250 ml of nitrate solution sodium concentration of 4.5 g-EQ/l (second reextract), with the formation of the spent leaching solution containing a part of the impurity elements, and washed first extract. The spent wash solution back into the original solution. Then washed from the first extract are reextraction nitrates of rare-earth elements in 3 counter-current stages of 800 ml of water. The first reextract containing 38,2 g/l Ln2O3separated from the depleted organic phase, which is in the form of the extractant return on extraction of REE. The degree of REE extraction taking into account the return to the cycle of losses proryvnym solution is 98,7%. Then in the first raffinate impose 85 ml of 35% hydrochloric acid to provide 5% of the excess in relation to the content of nitrate ions, and processed 1200 ml of 80% solution of TBP in dodecane on 4 stages with O:=0,9:1. The extraction of nitric acid passes into a second organic phase, while the main part of the impurity elements remains in chloride solution. After RA the division of the phases formed in the second extract a volume of 1200 ml, containing, g/l: Ln2O30,2; Cao 1,5; SrO 0,2; Al2About30,05; MnO20,3; Fe2About30,1; NO3-157,0, and the second raffinate volume 1315 ml, containing, g/l: Ln2O30,15; Cao 55,3; SrO 6,4; Al2About343,5; MnO223,0; Fe2O3less than 0.01; NO3-11,2, which derive from the process and sent for recycling. The degree of extraction of nitric acid in the second extract is 97%. From the second extract nitric acid extravert 1 stage 200 ml of a solution of an alkaline reagent in the form of sodium hydroxide at a concentration of reagent 4.5 g-EQ/l, which are taken in stoichiometric quantity with respect to nitric acid. Forming a second reextract in the form of a nitrate solution of sodium with a concentration of 4.5 g-EQ/l is used as a washing solution for washing the first extract. Depleted second organic phase in the form of the extractant return to the extraction of nitric acid.

Example 2.

In the solution means of hydrochloric acid decomposition eudialyte concentrate in the amount of 1000 ml of the composition, as in Example 1, enter 130 g of calcium nitrate and 250 ml of waste leaching solution containing 6.0 g-EQ/l calcium nitrate and 6.8 g/l Ln2O3to ensure the content of nitrate-ion 2 g-EQ/l Obtained chloride-nitrate solution was processed in 5 steps FR is the West 1000 ml of extractant in the form of an 80% solution of TBP in dodecane O:=1:1,3 translation of nitrates of rare-earth elements and part of the impurity elements in the first organic phase. The main part of the impurity elements is in chloride-nitrate solution. After separation of the phases formed first extract and a first raffinate. The content of REE in the first raffinate is 0.15 g/l, nitrate-ion - 1.35 g-EQ/L. the First extract is washed with a counter on 2 levels 250 ml of nitrate solution calcium concentration of 6.0 g-EQ/l (second reextract), with the formation of the spent leaching solution containing a part of the impurity elements, and washed first extract. The spent wash solution back into the original solution. Then washed from the first extract are reextraction nitrates of rare-earth elements in 3 counter-current stages of 800 ml of water. The first reextract containing 42.2 g/l Ln2O3separated from the depleted organic phase, which is in the form of the extractant return on extraction of REE. The degree of REE extraction taking into account the return to the cycle of losses proryvnym solution was 99.4%. Then in the first raffinate is injected 148 ml of 37% hydrochloric acid to ensure that it is 10% excess with respect to the content of nitrate ions, and processed 1450 ml of 80% solution of TBP in dodecane on 5-speed countercurrent O:In=1:1. The extraction of nitric acid passes into a second organic phase, while the main part of the impurity elements remains in chloride solution. The degree of extraction is possible nitric acid in the second extract is 98.5%. From the second extract nitric acid extravert 1 step 250 ml of a solution of an alkaline reagent in the form of calcium oxide at a concentration of reagent 6.0 g-EQ/l, which are taken in stoichiometric quantity with respect to nitric acid. Forming a second reextract in the form of nitrate solution calcium concentration of 6.0 g-EQ/l is used as a washing solution for washing the first extract. Depleted second organic phase in the form of the extractant return to the extraction of nitric acid.

Example 3.

In the solution means of hydrochloric acid decomposition eudialyte concentrate in the amount of 1000 ml of the composition, as in Example 1, enter 100 g of calcium nitrate and 380 ml of the spent leaching solution containing 8.0 g-EQ/l calcium nitrate and 3.2 g/l Ln2O3to ensure the content of nitrate-ion 3 g-EQ/l Obtained chloride-nitrate solution was processed for 5-speed countercurrent 890 ml of extractant in the form of an 80% solution of TBP in dodecane O:=1:1.6 translation of nitrates of rare-earth elements and part of the impurity elements in the first organic phase. The main part of the impurity elements is in chloride-nitrate solution. After separation of the phases formed first extract and a first raffinate. The content of REE in the first raffinate is 0.03 g/l, nitrate-ions at 2.45 g-EQ/L. the First extract is washed with n is tivotogo on 2 levels 250 ml of nitrate solution calcium concentration 8 g-EQ/l (second reextract), with the formation of the spent leaching solution containing a part of the impurity elements, and washed first extract. The spent wash solution back into the original solution. Then washed from the first extract are reextraction nitrates of rare-earth elements in 3 counter-current stages of 800 ml of water. The first reextract containing of 41.6 g/l Ln2O3, separated from the depleted organic phase, which is in the form of the extractant return on extraction of REE. The degree of REE extraction taking into account the return to the cycle of losses proryvnym solution is 99,8%. Then in the first raffinate is injected 290 ml of 37% hydrochloric acid to provide 5% of the excess in relation to the content of nitrate ions, and processed 2000 ml of 80% solution of TBP in dodecane 8 speed countercurrent with a:=1,2:1. The extraction of nitric acid passes into a second organic phase, while the main part of the impurity elements remains in chloride-dimensional solution. The degree of extraction of nitric acid in the second extract is 97,4%. From the second extract nitric acid extravert 1 step 380 ml of a solution of an alkaline reagent in the form of calcium oxide at a concentration of reagent 8.0 g-EQ/l, which are taken in stoichiometric quantity with respect to nitric acid. Forming a second reextract in the form of nitrate rest the RA calcium concentration of 8.0 g-EQ/l is used as a washing solution for washing the first extract. Depleted second organic phase in the form of the extractant return to the extraction of nitric acid.

From the above Examples show that the inventive method allows to increase the efficiency of separation of rare earth elements from the solution means of hydrochloric acid decomposition eudialyte concentrate due to utilization of nitrate ions at high (by 98.7 99.8 per cent) degree of REE extraction. The method is more environmentally friendly compared to the prototype.

1. The method of separation of rare earth elements from the solution means of hydrochloric acid decomposition eudialyte concentrate, including the introduction of the nitrate ion in the original chloride solution containing rare-earth elements and impurity elements, processing the obtained chloride-nitrate solution extractant in the form of tributyl phosphate with translation of nitrates of rare-earth elements and part of the impurity elements in the first organic phase, separating the first organic phase from the chloride-nitrate solution with formation of a first extract and a first raffinate containing the main part of the impurity elements, the first washing of the extract nitrate solution with the return of the leaching solution in the original chloride solution, reextraction nitrates of rare-earth elements with water and separating the first reextract, characterized in that first raffinate impose concentrated the th hydrochloric acid to ensure its excess in relation to the content of nitrate ions, the raffinate is treated with tributyl phosphate with translation of nitric acid in the second organic phase and education chloride solution the main part of the impurity elements, separating the second organic phase with the formation of the second extract and a second raffinate and are reextraction nitric acid from the second extract solution of an alkaline reagent with a second reextract in the form of nitrate solution, which is used as a washing solution for washing the first extract.

2. The method according to claim 1, characterized in that the first raffinate enter 35-37%hydrochloric acid to ensure that it is 5-10%excess relative to nitrate ions.

3. The method according to claim 2, characterized in that the processing of the first raffinate with tributyl phosphate is carried out at a ratio of O:W=0,9-1,2:1.

4. The method according to claim 1 or 3, characterized in that reextraction nitric acid is carried out at the concentration of the alkaline reagent 4,5-8,0 g-EQ/l, with an alkaline reagent taken in stoichiometric quantity with respect to nitric acid.

5. The method according to claim 4, characterized in that the alkaline reagent for Stripping nitric acid using sodium hydroxide or oxide of calcium, it reextract in the form of a nitrate solution of sodium or calcium.



 

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8 cl, 1 dwg, 1 ex

FIELD: metallurgy; reworking wastes of alumina production process.

SUBSTANCE: proposed method includes preparation of batch of charge containing red mud and carbon reductant, heating the charge in melting unit to solid-phase iron reduction temperature, three-phase reduction of ferric oxides in charge by carbon reductant and saturation of iron with carbon in charge thus prepared, melting the reduced charge for obtaining metal phase in form of cast iron and slag phase in form of primary slag, separation of cast iron from primary slag in melt heated to temperature of 40 C, reduction of silicon and titanium from oxides contained in primary slag by aluminum and removal of cast iron and primary slag from melting unit; during preparation of charge, concentrate of titanomagnetite ore containing titanium oxide in the amount from 1 to 15% is added to red mud; besides that, additional amount of carbon reductant and additives are introduced; after separation of primary slag from cast iron in melting unit, cast iron is heated to 1500-1550 C and product containing ferric oxide is added to it; iron is reduced by carbon of cast iron for converting the cast iron into steel at obtaining secondary slag; main portion of steel is removed from melting unit, secondary slag is added to primary slag and silicon and titanium are converted into steel residue in melting unit by reduction with aluminum, thus obtaining final slag-saturated slag and master alloy containing iron, titanium and silicon; main portion of master alloy is removed from melting unit; after removal of final slag for converting the master alloy residue to steel in melting unit, titanium and silicon are converted into slag phase by oxidation and next portion of charge is fed to slag phase formed after converting the master alloy residue to steel. Proposed method ensures high efficiency due to obtaining iron-titanium silicon master alloy in form of independent product and production of alumina from high-alumina final slag or high-alumina cement and concentrate of rare-earth metals.

EFFECT: enhanced efficiency due to avoidance of intermediate remelting of steel.

10 cl, 2 dwg

The invention relates to a technology developing concentrates of rare earth elements from natural phosphate concentrates

The invention relates to the technology of extraction of rare earth elements (REE) from phosphogypsum obtained by sulphuric acid processing of Apatite concentrate on mineral fertilizers

The invention relates to the metallurgy of rare metals, more specifically to the technology of aluminum alloys with rare-earth elements, scandium, yttrium and lanthanides

The invention relates to the hydrometallurgical processing of ore concentrates, and more particularly to the processing of loparite concentrate and can be used in complex extraction of compounds of titanium, niobium and tantalum

FIELD: methods of determination of content of palladium and platinum in ores containing considerable amount of iron, copper, zinc and other metals.

SUBSTANCE: proposed method includes decomposition of ore by hydrofluoric and nitric acids followed by further decomposition by aqua regia, boiling-off to moist salts, dissolving of them in hydrochloric acid and extraction. Determination of content of palladium is carried out in organic phase thus obtained and that of platinum is carried out in hydrochloric acid phase. Extractants used for such determination are s-alkylisothiouronium halides and alcohols of C5-C8 fractions, as well as kerosene, benzene, toluene and xylols used as diluents. Used as s-alkylisothiouronium halides are chlorides, bromides and iodides from C7 to C14 and their fractions.

EFFECT: extended range of reagents and inert diluents.

2 cl, 2 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

The invention relates to the processing orangutango raw materials

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 the extraction of substances organic extractants from aqueous solutions and can be used in ferrous and nonferrous metallurgy, as well as for the treatment of industrial and domestic wastewater

The invention relates to methods for determination of palladium and platinum ores containing large amounts of iron, copper, zinc and other metals

The invention relates to a method of extracting metal from ore or concentrate containing Nickel and/or cobalt and other metals

The invention relates to the field of non-ferrous metallurgy, in particular to the technology of rare and scattered elements, and can be used for the recovery of indium from zinc sulfate solutions with a high content of silica

FIELD: chemical industry; materials and the methods for the catalyst carrier manufacture.

SUBSTANCE: the invention is pertaining to the new mixed oxides produced from ceric oxide and zirconium oxide, which can used as the catalyzers or the catalyzers carriers for purification of the combustion engine exhaust gases. The mixed oxide possesses the polyphase cubical form of the crystallization and oxygenous capacity of at least 260/ micromoles of O2 /g of the sample and the speed of the oxygen extraction of more than 1.0 mg-O2/m2-minute, which are measured after combustion within 4 hours at the temperature of 1000°C. The invention also presents the substrate with the cover containing the indicated mixed oxide. The method of production of the polycrystallic particles of the indicated mixed ceric-zirconium oxide includes the following stages: i) production of the solution of the mixed salt which are containing, at least, one salt of cerium and, at least, one salt of zirconium in the concentration, sufficient for formation of the polycrystallic particles of the corresponding dry product on the basis of the mixed oxide. At that the indicated particles have the cerium-oxide component and zirconium-oxide component, in which these components are distributed inside the subcrystalline structure of the particles in such a manner, that each crystallite in the particle consists of a set of the adjacent one to another domains, in which the atomic ratios of Ce:Zr which are inherited by the adjacent to each other domains, are characterized by the degree of the non-uniformity with respect to each other and determined by means of the method of the X-ray dissipation the small angles and expressed by the normalized intensity of the dissipation I(Q) within the limits from approximately 47 up to approximately 119 at vector of dissipation Q, equal to 0.10 A-1; ii) treatment of the solution of the mixed salt produced in compliance with the stage (i),with the help of the base with formation of sediment; iii) treatment of the sediment produced in compliance with the stage (ii),using the oxidative agent in amount, sufficient for oxidizing Ce+3 up to Ce+4; iv) washing and drying of the residue produced in compliance with the stage (iii); and v) calcination of the dry sediment produced in compliance with the stage (iv),as the result there are produced polycrystallic particles of the oxide of ceric and zirconium in the form of the mixed oxide with the above indicated characteristics. The technical result is the produced mixed oxide possesses both the high oxygenous capacitance, and the heightened speed of the oxygen return in the conditions of the high temperatures.

EFFECT: the invention ensures production of the mixed oxide manufactured from ceric oxide and zirconium oxide and possessing the high oxygenous capacitance and the heightened speed of the oxygen return in the conditions of the high temperatures.

68 cl, 21 ex, 2 dwg

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