Method of producing vanadium pentoxide

FIELD: chemistry.

SUBSTANCE: invention refers to method of producing high-quality vanadium pentoxide from hydrated deposited industrial vanadium pentoxide. Method includes as follows. Deposit is filtered, washed with water with following reagent processing by calcium-containing salt solutions to recover it from manganese. Reagent processing is enabled in ratio 3.0-8.5 g Ca2 + per 1 g MnO. Produced is supplied to reagent processing of new portions of hydrated deposited industrial vanadium pentoxide in the same Ca2 + to MnO ratio. As manganese is accumulated in solution, it is regenerated with adding calcium hydroxide suspension, containing CaO, or slaked lime of consumption 1.0-1.45 g CaO per 1 g MnO in stirring. After that manganese concentrate is isolated. Liquid phase is delivered back to reagent processing of new portions of hydrated deposited industrial vanadium pentoxide.

EFFECT: production of the second end product - manganese concentrate, cost saving of production and enhanced ecology.

1 dwg, 4 tbl, 6 ex

 

The invention relates to metallurgy, in particular to methods of producing vanadium pentoxide from toxins and other vanadium-containing materials, and can be used in the production of vanadium products.

Purification of vanadium products from impurities is complex hydrometallurgical processes. Most of the known methods of cleaning concentrate vanadium pentoxide concerns impurities of phosphorus, silicon, which are mainly of vanadium-containing solutions in alkaline medium.

When mixing the solutions obtained by the two-stage leaching of vanadium from burnt slag in OAO Vanady-Tula" by washing the precipitate of hydrated vanadium pentoxide with water, solutions of salts of magnesium, iron and others, get fused vanadium pentoxide containing 90-95% V2O5and 2,6-1,0% MnO (Sirin ETC., V. Mizin, E.M. Rabinovich and other Extraction of vanadium and Nickel from waste power plants. Ekaterinburg: Ural branch of the Russian Academy of Sciences, 2001, str-153, RIS).

Of vanadium pentoxide such, it is impossible to obtain high-grade ferrovanadium brand FeV80 due to the high content of MnO, since, as shown, for smelting of this brand of ferrovanadium this indicator should not exceed 0,50% wt. In addition, with the substitution for the exchange reaction of manganese in hydrated precipitate vanadium pentoxide remain Katie the s reagent solutions, which reduce the quality of the finished product, and difficult disposal of waste solutions.

To reduce the content of impurities in technical vanadium pentoxide obtained from alkaline solutions of water leaching of vanadium after firing furnace slag with the addition of soda, developed processing technology alkaline vanadium pentoxide (obtained from solutions from water leaching) solutions of calcium chloride ("the Reduced content of impurities in technical vanadium pentoxide. // Proc. Dokl. VIII the age of three. proc. "Vanadium. Chemistry, technology, applications". Chusovaya, 2000, s). This method is used for the prototype.

When handling solutions of CaCl2vanadium pentoxide deposited from alkaline solutions containing, in wt.%: 89,3 V2O5; 0,81 MnO and 2.88 Na2O the precipitate with content, % wt.: 91,2-95,15 V2O5, of 0.045 to 0.14 MnO 0.16-0,47 Na2O.

Substitution of cations of calcium ions, manganese, sodium, etc. does not reduce the technological properties of the resulting vanadium pentoxide, as in the smelting of vanadium in the composition of the charge is injected lime and due to the presence of calcium in the composition of vanadium pentoxide becomes possible to reduce the consumption of lime in the smelting of vanadium and comprehensively to use reagent Supplement.

The disadvantages of the known technology are:

1. The inability to get high is artnow vanadium pentoxide from the total volume of the solution (alkaline/pH-governmental plus acid), which reduces the production efficiency.

2. High consumption of reagent CaCl2and , consequently, the increase in the cost of vanadium products, which is especially true when processing vanadium pentoxide with a high content of manganese, which currently produce both the manufacturer of the Russian Federation OAO Vanady-Tula", Chusovoy metallurgical plant". The increased content of manganese in the technical vanadium pentoxide was due to changes in the composition of the raw materials, which resulted in a change in the technology domain of smelting iron and stages of the Converter slag. The content of manganese oxide in the slag ranges from 11-22%, and in hydrated precipitate vanadium pentoxide sometimes reaches of 2.5-3.5% wt.

3. A large number of waste waste solutions containing manganese, which requires the cost of their disposal.

4. Loss of manganese as a second valuable macro-slag.

5. The instability of the process, because at lower flow CaCl2testing of reagent solutions did not provide the necessary required for the smelting of high-grade vanadium content of MnO in the finished product less than 0,50% wt. (see drawing).

6. High water consumption, because the processing of each new portion of the vanadium pentoxide is used, fresh solution.

7. The inability of the organization is SQL turnover reagent solution and its regeneration.

The objective of the invention is to design ensures high-efficiency, integrated technologies for the production of vanadium pentoxide higher quality, and hence high-grade vanadium products with simultaneous integrated use of raw materials, such as Converter slag, obtain a second product - manganese concentrate, lower production costs due to the regeneration of the reagent solution and improving the environment by circulation of the solution in the production cycle, reducing toxic waste and water consumption.

The problem is solved by the characteristics specified in the claims, in common with the prototype, such as the method of obtaining vanadium pentoxide higher quality of hydrated sediment technical vanadium pentoxide comprising filtering the precipitate, washing it with water and chemical treatment of solutions of calcium salts for removing manganese, and distinctive essential features, such as reagent treatment sludge technical vanadium pentoxide solutions of calcium salts, which is carried out at a ratio of 3.0-8.5 g of CA2+1 g of MnO, the resulting solution was sent for chemical treatment of new portions gidratirovannogo sediment technical vanadium pentoxide with the same ratio of CA2+to MnO, and pinakapani manganese in solution it regenerate the addition of a suspension of calcium hydroxide, containing Cao or pushonki with a flow rate of 1.0 to 1.45 g of Cao per 1 g of MnO, with stirring, separating the manganese concentrate and the liquid phase return for carrying out chemical treatment of new portions of hydrated sediment technical vanadium pentoxide.

Experiments have shown that carrying out chemical treatment of the precipitate of hydrated vanadium pentoxide solutions of calcium salts with a ratio of grams of CA2+/g MnO (next N) below 3.0 is not possible to obtain a final product of a vanadium pentoxide required quality with the content of MnO is less of 0.50% wt. The ratio of more than 8.5 g of CA2+/g MnO impractical, since the increase in chemical consumption does not lead to further significant decrease in the content of manganese (see the drawing), and costs increase. The solution obtained after chemical treatment and having a concentration of CaCl2providing a ratio of N=3-8,5, is used to process new portions of the vanadium pentoxide. This technique leads to a reduction in consumption of calcium-containing reagents approximately 2 times.

The removal of manganese from hydrated vanadium pentoxide passes through the reaction:

where R is polyvanadate - based technical vanadium pentoxide.

The accumulation of manganese in the solution during repeated use of the reagent solution reduces its reactionary act shall want to make, therefore, the manganese isolated in sediment and calcium reagent regenerate. Regeneration takes place according to the reaction:

Manganese enters the sediment, and calcium in soluble salts, such as calcium chloride or calcium nitrate, i.e. almost the regeneration of calcium-containing reagents. Consumption of calcium oxide is less than 1.0 g Cao per 1 g of MnO does not ensure complete removal of manganese from the regenerated solution, and the excess of consumption over 1,45 impractical, since increased consumption of Cao, and the degree of deposition of manganese remains almost at the same level (table 2). In addition, with the increasing consumption of Cao manganese concentrate is depleted according to the leading component is manganese and by co-precipitation of gypsum enriched sulfur, which reduces its commercial value.

The regenerated solution containing calcium-containing reagent in an amount to provide a ratio of N within the proposed method, used for treatment of new portions of hydrated sediment technical vanadium pentoxide. The lack of calcium reagent, reduction of N less than the 3.0 is feed-additive in the reagent solution of fresh powder calcium reagent.

The above set of features of both known and new poses which enables you to implement highly efficient integrated process for the production of vanadium pentoxide high quality, consequently, high-grade vanadium products with simultaneous integrated use of raw materials, such as Converter slag, obtain a second product - manganese concentrate, lower production costs due to the regeneration of the reagent solution and improving the environment by circulation of the solution in the production cycle, reducing toxic waste and water consumption.

The above distinctive features, each separately and all together, are aimed at solving the problem and are significant. The use of the proposed combination of essential distinctive features in the prior art was not found, therefore the proposed solution meets the patentability criteria of "novelty".

One set of new essential features of a General known provides a solution to the problem is not obvious to a person skilled in the art and demonstrates compliance of the claimed technical solution to the patentability criterion of "inventive step".

The invention is illustrated in the examples. Substantiation of the parameters of the proposed method are shown in examples 1-6, tables 1-4 and in the drawing.

Example 1

The hydrated precipitate technical vanadium pentoxide, the floor is built in the current production of Chusovoy metallurgical plant", after firing furnace slag with the addition of 7% ash, two-phase (water and acid) leaching, after filtration and water washing, containing 48,7% Rel. moisture in % wt. in dry weight: 84,9 V2O5, 1,17 MnO, divided into equal parts in 97.5 g of wet (50 g dry) and place on a Buechner funnel, processed reagent solution of CaCl2in the layer with respect to T:W=1:7, creating a ratio of Ca2+1 g of MnO (next N) in the range 2-10. Precipitates obtained after chemical treatment, washing with water and calcining the precipitate at 450°C for 1.0 hour and analyzed for the content of MnO. The results of the experiments shown in the drawing, show that when the ratio of N less than 3,0 impossible to get the MnO content in the treated vanadium pentoxide below to 0.50%. Increasing the ratio of N over 8.5 economically impractical, since no significant reduction of MnO in the final product.

Example 2

A portion 586 g wet (300 g dry) of hydrated sediment technical vanadium pentoxide, conditions of formation and the composition of which is shown in example 1, processed with respect to T:W=1:6 reagent solution of CaCl2containing 49 g/l reagent at a ratio of N=9.1 and washed with water at T:W=1:2. The resulting vanadium pentoxide meets the requirements for smelting of vanadium brand FeV80 and contains, in wt.%: 86,8 V2O5and 0.10 MnO. Spending the reagent - powder CaCl2was 0,294 g/g initial dry vanadium pentoxide (experiment 1, table 1 an example of the prototype). The solution after processing the first portion containing 37.5 g/l CaCl2and 0.72 g/l MnO, sent to the processing 400 g new portion such as vanadium pentoxide (experiment 2, table 1) without the addition of reagent, the ratio N=5,06. The composition of the vanadium pentoxide, % wt.: 86,7 V2O5; 0,29 MnO; 0,16 Na2O; 3,8 CaO; 4,3 Fe2O3; 0,02 MgO and Al2About3; 0,34 TiO2; 0,37 Cr2O3. This composition is quite consistent with the requirements for smelting high-grade ferrovanadium. Reagent consumption CaCl2for two experiments (powder) was 88,2 g 700 g of sediment and equal to 0.126 g/g, i.e. reduced by 2.3 times (experiments 1-2, table 1) in comparison with the experience of 1 of the prototype.

Thus the possibility of reducing chemical consumption when using the solution obtained after the first cycle of chemical treatment, to improve the quality of a new portion precipitate of hydrated vanadium pentoxide.

Example 3

The solution obtained after chemical treatment of sludge technical vanadium pentoxide containing, g/l: 32,1 CaCl2, 2,68 MnO and 0.31 V2O3divided into equal volumes of 0.2 l and to each portion was added a suspension of calcium hydroxide containing 80 g/l of Cao with a flow rate of 0.90-1.50 g of Cao per 1 g of MnO (table 2, experiments 1-5). The slurry was passed with stirring for 30 minutes, separated Argenteuil concentrate, washed with water and dried at 105°C to constant weight. The results of the experiments are given in table 2, show that the optimal additive is the consumption of 1 g of Cao per 1 g of MnO in the range from 1.0 to 1.45. By reducing consumption of less than 1.0 g of Cao/g of MnO manganese from solution stands out incompletely - the degree of deposition of 82.7% of Rel. Increase consumption of calcium oxide in the regeneration of the liquid phase to 1.45 g of Cao per 1 g of MnO allows not only to obtain a high degree of deposition of manganese vanadium, regenerate CaCl2by increasing its content from 32.1 to 36.0 g/l, and precipitate manganese concentrate with content of 49.3-76.8% of MnO and 0,10-0,25% S suitable for use in metallurgy or in the composition of the charge in the manufacture of welding electrodes. Increase flow rate to 1.50 g of Cao per 1 g of MnO is impractical because it does not lead to an improvement in process: reduced content of MnO in manganese concentrate, increased sulfur content, and the concentration of CaCl2in the liquid phase is not increased. In addition, due to the higher consumption of Cao in suspension increases the pH and the dissolution of the vanadium concentration of traces increases to 0.09 g/l

Example 4

The hinge 30 g (dry) wet technical vanadium pentoxide, the composition of which is given in example 1, was treated at T:W=1:6 in the layer of the liquid phase obtained after separation of manganese ore, images is segosa when regeneration of the reagent solution according to the conditions of example 3 (table 2, experience 4) containing CaCl236 g/l with a ratio of N=6,66, not adding fresh powder CaCl2(experiment 1, table 3). Then, the resulting solution having a content of CaCl230,9 g/l, returned to the processing of a new piece of technical vanadium pentoxide (experiment 2, table 3) on the second cycle of the reagent processing when N=4,04 received after processing solution with the content of CaCl2of 22.4 g/L. it added a powder of calcium chloride to a concentration of 40.4 g/l CaCl2and used it for chemical treatment of a new piece of technical vanadium pentoxide for N=3,47 (experiment 3, table 3). In the experiments all experiments received conditional vanadium pentoxide, suitable for smelting of vanadium brand FeV80 with the content of MnO is 0.22-0.37 per cent. Processing 90 g of vanadium pentoxide through the use of regenerated by the present method of solution added 3,24 g CaCl2or the reagent consumption was only 0.036 g CaCl2/g initial precipitate of hydrated vanadium pentoxide, which is 8.2 times lower in comparison with the experience, carried out under the terms of the prototype (table 1, experiment 1).

Example 5

Vanadium-containing slag containing, % wt.: 18,2 V2O5and 12.3 MnO, mixed with limestone in the ratio of CaO/V2O5=0.6 and annealed in an oxidizing atmosphere at 830°C for 1.5 hours. Baked mixture of wimalasiri vanadium and from the obtained solutions (the N-aqueous and acid leaching) besieged gidratirovannuyu vanadium pentoxide. The cake moisture of 45.3%, the content of V2O5and 86.8%, MnO - 2,65%.

The sediment was divided into two parts and held his chemical treatment with a ratio of N=8 at T:W=1:5 solution of CA(NO3)2two options within 30 minutes:

1 - if repulpable in the reagent solution;

2 - layer, flowing the reagent solution through a layer of sediment. The results of the experiments are shown in table 4, show that the proposed method can obtain the vanadium pentoxide with a low manganese content, in any scenario of firing the original BOF slag with the addition of soda (examples 1-4) and limestone, as well as the method of chemical treatment in the layer or repulpable.

Example 6

To 0.5 l of the solution obtained after the three-fold use of the reagent solution of CaCl2for processing precipitate of hydrated vanadium pentoxide obtained in the current production of OAO Vanady-Tula", containing in g/l: 55,0 CaCl2; 2,5 MnO and 0.35 V2O5added when mixing the powder of Cao lime (pushonku) with a flow rate of 1.35 g of Cao per 1 g of MnO and maintained for 0.5 hours. After separation of the liquid phase precipitate manganese concentrate was washed with water, dried and probalily at 700°C for 1 hour. Calcined manganese concentrate contained, % wt.: 50,3 MnO; 35,0 Cao; 5,3 V2O5; 0,26 S; 0,15 Cr2O3; 5,8 SiO2; 0,035 R. the structure of the liquid the basics of content CaCl 2increased to 60,4 g/l, the content of MnO and V2O5was at the level of traces.

So shows not only the regeneration of the reagent solution, which allows to use it for processing new portions precipitate of hydrated vanadium pentoxide to improve its quality, but also to obtain commercial manganese concentrate, suitable for use in the metallurgy and other industries.

Thus, the results presented in examples 1-6 show that the proposed method and its implementation can provide technical and vanadium pentoxide with a low manganese content, to reduce the cost of reagents at 2-8 times, water use and discharge of toxic solutions in the technological cycle, and complex use of raw materials - to bring the manganese in the form of saleable manganese concentrate, suitable for use in metallurgy, in the composition of the charge in the manufacture of welding electrodes or in other industries.

From the description and practical application of the present invention to specialists will be obvious and other private forms of its implementation. The description and examples are considered to illustrate the invention, the essence of which and the scope of patent claims is defined in the following claims scoop what prostu essential features and their equivalents.

Table 1
Humidity source of vanadium pentoxide, % Rel.=48,8. The composition of the initial vanadium pentoxide (dry), % wt.: 84,9 V2O5; 1,17 MnO. The ratio of T:W in the reagent processing 1:6; flushing 1:2.
No. of experimentsConditions of experimentsThe results of the experiments
Introduced, gThe composition of the solution, g/lThe composition of the vanadium pentoxide, % wt.Consumption g CaCl2on g ex. vanadium pentoxideNotes
Dry vanadium pentoxideMnOX)CaCl2Just CA2+Source CaCl2After the process.
on the reverse p-rumpowder onlyCaCl2MnOV2O5MnO
1300no88,288,2of 31.89,149,037,50,7286,80,190,294Example prototype
240090,0no90,032,49of 5.0637,532,11,3886,70,29noUse. the solution after processing in op
*) The numerator is entered into the composition of vanadium pentoxide, the denominator with a working solution

Table 2
Determination of the optimal flow rate g of Cao/ g of MnO in the regeneration of the reagent solution. The solution after chemical treatment of vanadium pentoxide: MnO of 2.68 g/l; CaCl2- 32.1 g/l; V2O5- 0.31 g/l
No. of experiments p/pConsumptionThe results of the experiments
The composition of the liquid phase, g/lThe composition of manganese concentrate, % wt.The degree of deposition of manganese, % Rel.
MnOV2O5CaCl2MnOV2O5S
10,900,450,1135,471,2-0,0982,7
21,000,22- 35,8of 76.8-0,1091,5
31,35traces0,0536,153,5the 5.70,20~100%
41,45the sametraces36,0to 49.33,20,25the same
51,50the same0,0936,037,20,47the same

Table 3
Humidity source of vanadium pentoxide, % Rel.=48,8. The composition of the initial vanadium pentoxide (dry), % wt.: 84,9 V2O5; 1,17 MnO. The ratio of T:W in the reagent processing 1:6; flushing 1:2.
Conditions of experimentsThe results of the experimentsNotes: for chemical treatment used
Introduced, gThe composition of the solution, g/lThe composition of the vanadium pentoxide, % may.Consumption g CaCl in g ex. vanadium pentoxide
Dry vanadium pentoxideMnOX)CaCl2Just CA2+Source CaCl2After the process.
on the reverse p-rumPowderonlyCaCl2MnOV2O5MnO
1306,48no 6,482,346,6636,030,90,8187,90,22noThe liquid phase after regeneration from op, table 2 (example 3)
2305,56no5,562,014,0430,922,42,2587,10,35noThe solution from op, table 3 (example 4)
3304,033,247,272,623,4740,434,82,6887,50,37to 0.108The solution from op table 3 (the example 4) with the addition of powder CaCl 2up to 40.4 g/l
Averagebeing 0.036
*) The numerator is entered into the composition of vanadium pentoxide, the denominator with a working solution

Table 4
The original vanadium pentoxide: humidity 45,3% Rel. Composition, % wt.: 86,5 V2O5, 2,65 MnO (dry). Hanging wet vanadium pentoxide: 27,42,
No. of experimentsConditions of chemical treatmentComposition, % wt. vanadium pentoxide
MethodIntroduced, gN
MnOCA++Ca(NO3)2V2O5MnO
1Repulpable0,3983,1813,028,094,90,12
2In the layer0,3983,1813,028,0for 95.20,09

The method of obtaining vanadium pentoxide higher quality of hydrated sediment technical vanadium pentoxide comprising filtering the precipitate, washing it with water and chemical treatment of solutions of calcium salts for removing manganese, characterized in that the chemical treatment of sludge technical vanadium pentoxide solutions of calcium salts is carried out in a ratio of 3.0-8.5 g of CA2+1 g of MnO, the resulting solution was sent for chemical treatment of new portions of hydrated sediment technical vanadium pentoxide with the same ratio of CA2+to MnO and the accumulation of manganese in the solution of his regenerate the addition of a suspension of calcium hydroxide containing Cao, or pushonki with a flow rate of 1.0 to 1.45 g of Cao per 1 g of MnO under stirring, separating the manganese concentrate and the liquid phase return for carrying out chemical treatment of new portions of hydrated sediment technical vanadium pentoxide.



 

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3 cl, 5 tbl, 9 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to method of metals heap leaching, notably, gold from ore. Method includes ore reduction, ore division into fractions, ore dump by uniform in fractions inclined layers with reduction of ore fineness from the low layer to top with separation of layers by perforated polymer film. Then it is implemented stack irrigation by leaching cyanide solution with concentration 0.2-0.8 g/l. Additionally after dump of each ore leaching it is implemented treatment of layer by cyanide solution with strengthen concentration and its standing. Concentration of cyanide solution and standing duration are reduced from low later to top from 2.0-4.0 g/l till 1.0-1.5 g/t and from 5-6 days till 2-3 days correspondingly.

EFFECT: leaching effectiveness increase.

1 dwg

FIELD: metallurgy.

SUBSTANCE: it is implemented treatment of copper-nickel sulfide concentrate by fluoride and/or ammonium bifluoride at the temperature 165-210°C during 2-3 hours with forming of hard fluorination products and emission of ammonia gas and water vapor. Fluoride and/or ammonium bifluoride are used in amount 1.0-1.2 from stoichiometric with respect to overall content in copper-nickel concentrate of silicates and pyrrhotine. Hard fluorination products exposed to water leaching at the temperature 40-60°C and S:L=1:5-6 during 1-2 hours with transformation to residue nickel sulfide, copper, cobalt, platinum metal and magnetite, and into solution - fluorine-ammonium silicon saline, magnesium, iron, aluminium and calcium. Residue is separated from solution and exposed to magnetic separation with magnetite extraction. Received solution is neutralised by ammonia water till providing of pH 8-10 with regeneration of fluoride and/or ammonium bifluoride and receiving of residue of magnesium, iron, aluminium, calcium and silica hydroxides. In the capacity of ammonia water for solution neutralisation can be used ammonia gas and water vapors from the stage of raw materials fluorination. Formed ammonium fluoride and/or bifluoride are returned to raw materials treatment stage.

EFFECT: energy content reduction and providing of selectivity sulfide crude ore treatment at less number of operations.

5 cl, 1 dwg, 4 ex

FIELD: metallurgy.

SUBSTANCE: method of metal extraction recovery from solid-phase of raw-materials includes crushing of raw materials, leaching by means of direct microemulsion, consisting of aqueous phase and organic phase, containing kerosene in the capacity of extractant di-(2-ethylhexyl) sodium phosphate, separation of solid phase and re-extraction of recovered metals. At that leaching is implemented by microemulsion, consisting of 30-75% turn of aqueous phase and containing in organic phase di-(2- ethylhexyl) sodium phosphate in amount 1.0-2.0 mole/l and additionally introduced di-(2-ethylhexyl) phosphoric acid in amount 0.3-0.6 mole/l. Into compound of organic phase of microemulsion i can be additionally introduced aliphatic alcohols in amount till 5% turns.

EFFECT: ability of selective extraction of nonferrous and rare metals raw at leaching stage, without usage of concentrated acid and expensive organic solvent.

9 tbl, 7 ex

FIELD: metallurgy.

SUBSTANCE: invention concerns methods of residue utilisation. Particularly it concerns method of copper extraction from sulphate containing dust of copper production. Method includes water leaching of dust with copper and impurity elements conversion into leaching solution, separation of solution from insoluble residue, liquid solvent extraction of copper by oximne extractant with receiving of copper-bearing extract and raffinate, containing impurity elements. After extraction it is implemented copper re-extraction, cleaning of received re-extract from extragent and electro-extraction of copper with receiving of commercial copper and reversible electrolyte. At that water leaching of dust is implemented at temperature 60-100°C and H:L=1:2-4. Leaching solution is cooled with crystallisation of copper main part in the form of vitriol and forming of mother solution, containing residual part of copper. Vitriol is separated from mother solution, dissolved in sulphuric solution and fed to electro-extraction, and liquid solvent extraction is implemented from mother solution.

EFFECT: receiving of qualitative cathode copper of grade MOOK with yield into commercial product up to 98% of copper at high (90,5-93,5%) yield by stream, and also in reduction of material flow volume and deep separation of copper from impurity elements.

9 cl, 3 ex

FIELD: metallurgy.

SUBSTANCE: invention concerns processing method of copper manufacturing dust. Method includes dust leaching at elevated temperature with transferring of copper and iron into solution, separation of solution from insoluble residue, separation of copper and iron. Than it is implemented evaporation of solution, containing basic quantity of copper, blue copperas crystallisation, separation of blue copperas crystals from growth solution and extraction from growth solution of residual quantity of copper. At that solution evaporation is implemented till providing of its density 1.30-1.36 g/cm3. Separation of copper and iron is implemented during the process of blue copperas crystallisation. Received blue copperas crystals are dissolved in sulfuric solution till providing of sulfuric acid concentration 100-250 g/l. Formed solution of blue copperas is exposed to basic electro- extraction with receiving of cathode copper and gate-type electrolyte. Extraction of copper residual quantity from growth solution is implemented by additional electro- extraction. Copper extraction degree from dust into solution at leaching is defined by content of copper in dust in oxidised form and reach 99.4%. Total copper extraction into cathodic metal is 89.4-95.2%.

EFFECT: receiving of qualitative cathode copper of grades MOOK, MOK, M1K, and also copper sponge at outlet by current on basic electro- extraction till 93,3% and at additional - till 74,6%.

10 cl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention can be used for production of high-purity silicon dioxide within integrated processing of magnesium-chrome crude ore that is mixed serpentinite, chromite, pyroxene and other minerals. Method of integrated processing of magnesium-chrome crude ore includes as follows. Crude ore is decomposed by solution of mineral acids. Produced suspension is filtered, and insoluble residue is processed. Filtrate neutralisation is accompanied with sedimentation of contained metal hydroxides with washing and drying of produced end-products. Processing of insoluble residue includes annealing at temperature 350-600°C, following dissolution in caustic soda to residual alkalinity 40-60 g/l NaOH, filtering of prepared suspension, washing of residue that is chrome ore concentrate and sedimentation of silicon dioxide from produced filtrate with solution of hydrochloric acid to residual acidity 2-15 g/l HCl.

EFFECT: higher separation integrity of silica component with simultaneous integrated extraction of other components of crude ore that provides extended application of base mixtures.

6 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: invention concerns industrial sanitation and environmental protection field, at usage in manufacturing and in domestic conditions of metallic mercury, its containing devices and facilities, and also of amalgams, and is intended for neutralisation of mercury at its ingress both on surfaces of different materials and into volumes (material, brick, concrete and so forth). Neutralisation technique of metallic mercury by immobilisation includes its oxidation by means of treatment by water solution of hydrogen peroxide. At that additionally to oxidation it is implemented mercury deposition by means of simultaneous or successive treatment by water solution of reagent, transferring metallic mercury into insoluble or sparingly soluble in water compound of natural or anthropogenic composition. In the capacity of reagent there are used water-soluble compounds of alkaline or alkaline-earth metals for instance, sulphates, phosphates or carbonates.

EFFECT: effectiveness increase of process at excluding of mercury - organic compounds formation.

5 cl, 5 ex

FIELD: metallurgy.

SUBSTANCE: method includes leaching of material with water solution of chemical reagent and successive treatment of produced pulp for extraction of germanium and zinc. At that leaching is carried out with mechanical, grinding and disintegrating effect, using as solution chemical reagent of solution, containing oxidant at amount from 1.8 to 2.5 kg per 1 kg of germanium contained in source material and hydroxide of alkali metal at amount maintaining medium pH from 12 to 14 at ratio of solid and liquid phases 1:(3-8). Germanium is sorption settled out of produced pulp by means of transmission of pulp through ion exchanging resin; alkali at amount facilitating 13.5-14 pH of medium and water at amount facilitating ratio of solid and liquid phases 1:(5-8) are added to pulp. Product received after sorption sedimentation of germanium is treated in autoclave at temperature of 120-250°C and pressure of 6-40 atm. Then liquid phase is separated out of which zinc is extracted while germanium is eluated out of ion exchanging resin. Germanium is extracted out of produced eluate.

EFFECT: increased degree of germanium and zinc extraction.

4 cl, 2 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to extraction and concentration of thorium out of process waste of loparit concentrates treatment - spent melt of saline sprinkler filter (SSF) of loparit concentrate chlorination process. The method includes preparation of suspension by means of discharge of spent melt of saline sprinkler filter (SSF) into water, incorporation of high molecular flocculant, of holding, filtering, separation of sediment, obtaining of chloride solution, and of treatment with steel scrap and metal magnesium. Prior to obtaining chloride solution the source suspension is heated to 60-90°C and treated with solution of sodium hydroxide to pH 1.5-2.0 and to 0.1-0.3% solution of high molecular flocculant at amount of 3-5% from the source volume of suspension; then suspension is held for 2-4 hrs. Chloride solution is received by means of filtration of spent suspension obtaining sediment of rare metals; chloride solution is then treated with steel scrap and metal magnesium; at that the solution is successively treated first with the steel scrap at amount of 3-5 mass fractions of iron per 1 fraction of iron ions (III) in chloride solution at 80-100°C for 1-3 hrs till achieving the value of pH in a pulp equal to 3.0-3.5. Then the pulp is separated from the non-reacted portion of the steel scrap and is treated with metal magnesium to pH 3.5-4.5, and further with 0.1-0.3% solution of high molecular flocculant taken at amount of 5-20% from the volume of chloride solution. Thus produced pulp is held without mixing for 1-4 hrs and filtered producing thorium containing sediment; the said sediment is washed at filter first with solution containing 1-5 g/dcm3 of sodium sulphite, then with water. Washed out sediment is repulped in solution of sodium hydroxide with concentration of 50-150g/dcm3 at a ratio of "Ж:Т"=3-5 at 60-90°C for 2-3 hrs, after what the pulp is filtered with separation of alkaline filtrate. Thorium containing sediment at the filter is washed with water, pressed at the filter and dried; the alkaline filtrate and process water are merged and mixed, then heated to 80-90°C, and treated with solution of sodium hydroxide to pH 11-13 with production of hydroxide pulp. Hydroxide pulp is filtered and then radioactive sediment is produced at the filter; it is washed out with water and transferred to a special wastes depositary, while filtrate is mixed with 10-20 volumes of shop flush water, heated to 80-90°C and again treated with solution of sodium hydroxide to pH 11-13. Obtained pulp is held and filtered thus producing sediment of rare metals and deactivated chloride solution which is discharged to drainage. Sediment of rare metals is unloaded from the filter, merged with sediment of rare metals extracted from the source suspension, dried, washed out and then transferred for preparation of charge for its further chlorination together with the loparit concentrate.

EFFECT: upgraded efficiency of thorium extraction and simultaneously solving problem of neutralisation and utilisation of process waste.

1 dwg, 1 ex

FIELD: metallurgy.

SUBSTANCE: invention refers to non-ferrous metallurgy and can be used for extraction of vanadium out of ashes which is waste produced by burning of sulphuric vanadium containing black oil in heat engines of heat and hydropower stations. The method consists in the following: source ashes are mixed with sodium carbonate and water at a weight ratio of 100:(10-60):(30-50), then produced mixture is held at temperature of 100-150°C, preferably 115-120°C, during 2 hours. Vanadium is leached out of produced self-diffusing cake with water at temperature of 95-100° and a ratio of liquid: solid = (1.5-3):1.

EFFECT: avoiding of generating harmful gas exhausts at extraction of vanadium and implementation of available equipment.

1 tbl, 2 ex

FIELD: chemistry, technological processes.

SUBSTANCE: method of obtaining nanotubular structures includes mixing of oxygen-containing organic compound - oxalic acid hydrate with vanadium oxide gel or oxygen-containing compound of respective metal. As oxygen-containing compound of respective metal, peroxide molybdenum or tungsten oxides are used.

EFFECT: reduction of interlayer distance in structure of nanotubular structures of said oxides due to absence in structure of extraneous radicals of organic compounds.

2 cl, 5 dwg, 5 ex

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