Method of recovery of valuable metals from superalloys (versions)

FIELD: metallurgy.

SUBSTANCE: proposed method consists in valuable metals are decomposed in salt melt containing 60-95 wt % of NaOH and 5-40 wt % of Na2SO4. Then, melt decomposition product is converted into solid phase by cooling to room temperature. After cooling, minced melt decomposition product is converted in water at temperature lower than 80°C to produce water suspension and water fraction is separated by filtration for components to be extracted therefrom.

EFFECT: higher efficiency of extraction.

22 cl, 1 dwg, 3 tbl

 

The invention relates to a method of decomposition of superalloys, in particular scrap metal superalloys in molten salt of an alkali metal with subsequent extraction of valuable metals.

The superalloys are alloys with a complex structure, stable at high temperatures, Nickel-based and cobalt with the addition of other metals, such as, for example, aluminum, chromium, molybdenum, tungsten, tantalum, niobium, manganese, rhenium, platinum, titanium, zirconium and hafnium, as well as non-metals such as boron and/or carbon. Super alloys are hard and especially abrasion-resistant alloys, which are used in motoro - and engine-building, power engineering, and also in aviation and space technology. Special properties of these alloys can be achieved, in particular, the addition of rare earth and noble metals, such as rhenium, tantalum and niobium, or even platinum. A good overview about the composition, properties, and applications of superalloys are shown in Ullmann''s Encyclopedia of Industrial Chemistry, vol A13, fifth edition, 1989, p.55-65 and in Kirk-Othmer Encyclopedia of Technology, volume 12, fourth edition, str-458.

Super alloys differ from conventional alloys with high melting point such as W-Re alloy or Mo-Re alloys, its special resistance to oxidation, respectively, corrosion. So, the details of superalloys because of their full-time is good resistance to oxidation are used in the manufacture of the blades in a turbine aircraft. After a time of operation such details are an important source of raw material for extraction of rare metals, in particular rhenium, tantalum, niobium, tungsten, molybdenum and platinum.

Recovery of the alloying metals of superalloys is of great commercial interest because of the high stakes in them expensive metals. So, special superalloys contain metals such as rhenium, up to 12 weight. percent tantalum, up to 12 weight. percent niobium, up to 5 weight. percent, tungsten and molybdenum to 12 weight. percent. Other metals, which are the main metals in the superalloys are Nickel and cobalt. The superalloys are and for these metals is an important source of raw materials, from which it can be best economic recovery of these metals.

There are a number of hydro - and pyrometallurgical and electrochemical methods for the recovery of metal components of superalloys, which, due to the complexity of their implementation and high energy costs may not be applied on a large scale for economic reasons because of the constantly increasing energy prices.

Recovery of metal components of superalloys carried out according to the prior art melting them in a protective gas atmosphere and subsequent transformation into a fine powder in the result R is sbrazhivanija through the nozzle. The disadvantage of this method of processing is that super alloys melt at high temperatures of 1200-1500°C. the recovery of superalloys is carried out only at the second stage in the processing of the obtained powder acids. Experience shows that this requires a few days. According to another method, scrap metal superalloys pre-make fragile, for example, at low temperatures, and then crushed the energy-intensive grinding, and then decompose the wet chemical means at an elevated temperature in mineral acids with a certain concentration and composition (Potter and others, Eff. Technol. Recycling Metal, 1971, .35ff).

In addition, there are also ways in which provided by the decomposition of scrap metal superalloys using electrochemical processes.

According to US 3649487 scrap of alloy Fe/Ni/Co/Cu-base containing refractory metals such as tungsten, molybdenum and chromium, is first subjected to melt with the addition of non-metallic compounds of groups III, IV or V and transferred to the borides, carbides, nitrides, silicides or phosphides, viplava of them anodes, and finally subjected to anodic oxidation. While metals such as Ni, Co and Cu are moving initially in the solution and then stand out from the solution at the cathode, while the refractory metals, for example, stauts is in the form of borides, carbides, etc. in the anode sludge. Although the patent and it is reported that metals such as Ni, Co, Cu separated from the refractory metals W, Mo or Cr, but not full information, whether complete separation of these metals. In addition, in the patent there is no information about the efficiency of the method.

In WO 96/14440 described by way of electrochemical decomposition of superalloys in the anodic oxidation of the alloy in an electrolytic bath with an organic component of the solvent. In the patent it is reported that the electrolyte solution can be added up to 10% of water, so that the method could be implemented according to the invention. On the other hand, it is possible passivation of the anode due to the formation of gel or firmly adhered oxide layer, which may lead to interruption of the electrolysis. The processing and separation of valuable substances from a suspension resulting from electrolysis, followed by filtration. Separated at the same time, containing part of the alloying metals residue filtering further thermally treated through calcination and in conclusion, conventional hydrometallurgical methods.

In DE 10155791 C1 describes an electrochemical method for the decomposition of superalloys. When this process of superalloys first cast plates, which are then subjected to electrolytic decompose in oxygen-free near hanicheskih acids. With the problem of anode passivation here fighting the polarity of the electrodes. Both the last method can be economically carried out only under certain boundary conditions, in particular at high content of rhenium in the superalloys.

In DE 19521333 C1 described pyrometallurgical decomposition of scrap solid or heavy metal containing tungsten. Decomposition occurs at a temperature of from 800 to 1000°C in the molten salt, which consists of NaOH and Na2SO4. This way we obtain a melt of sodium tungstate, which after cooling is dissolved in water.

As in the present invention, there is alkaline, containing the sulfate melt scrap that contains tungsten and solid metal, is subjected to almost complete decomposition in an oxidizing conditions with the formation of sodium tungstate. This is not surprising due to the fact that metallic has a high stability and reactivity conditions dissolved in NaOH-melt, which ensures complete dissolution of the solid scrap metal.

The objective of the invention is to provide a method for decomposition and recovery of superalloys, in particular scrap registergui superalloys, processing and retrieving contained valuable substances as a cost-effective alternative compared to recuperation, westleymou by anodic oxidation or acid digestion.

This problem is solved by a method for the recovery of valuable metals from super alloys and super alloys corrode in the salt melt, which contains 60-95 weight. percent NaOH and 5-40 weight. percent Na2SO4and formed by the product of decomposition in the melt in conclusion hydrometallurgical process intended for easy separation of the individual precious metals. Preferably, the decomposition is carried out in a molten salt consisting of 65-85 weight. percent NaOH and 15-35 weight. percent Na2SO4, more preferably from 70 to 80 weight. percent NaOH and 20-30 weight. percent Na2SO4.

In the case of superalloys, the decomposition of which is relevant to this invention, more than 50% of metal components such as Nickel or cobalt, in the reaction conditions, proposed in DE 19521333 C1, do not form Metallistov and was unexpected that the decomposition could take place. Next was unexpected that almost all of the Nickel and cobalt after decomposition was metal that was possible, therefore, it is preferable processing decomposed in the molten product using magnetic separation. This should clear economic preference in comparison with the cited electrochemical methods of decomposition of superalloys. The superalloys according to data from the WMD invention are alloys, which as the main component contains from 50 to 80 weight. percent Nickel, from 3 to 15 weight. percent of at least one or more of the elements cobalt, chromium, and optionally aluminum and from 1 to 12 weight. percent of one or more of the elements rhenium, tantalum, niobium, tungsten, molybdenum, hafnium and platinum.

The method according to the invention is particularly suitable for registergui superalloys that contain up to 12 weight. percent rhenium. The decomposition of the superalloys according to the invention is preferably carried out so that the molten salt add up to 10 weight. percent soda (Na2CO3), preferably up to 8 weight. percent ash, more preferably up to 5 weight. percent ash calculated on the weight of the molten salt.

Preferred compositions of the molten salt are shown in table 1.

Table 1
NaOH (weight. percent)Na2SO4(the weight. percent)Na2CO3(the weight. percent)
85510
801010
70 255
80155
75205
72208

The superalloys can be submitted or in the form of pieces of debris, or in the form of powders (products of the milling or grinding of powders).

Decomposition superalloys may be carried out in furnaces with direct heating, for example in furnaces with gas or oil heating and ovens with indirect heating continuously or intermittently. Suitable for this furnace is a rotary kiln and rotary tube furnace.

Thus, it is preferable decomposition of superalloys in the movable alkaline melt intermittently working directly heated tubular rotary oven.

Decomposition according to this invention is conducted in such a way that 1 kg of supersplash take at least 1 kg of salt melt, preferably at least 1.5 kg and more preferably at least 2 kg of molten salt. In the case of such superalloys, the content of rhenium which is more than 8%, use up to 5 kg melt for every 1 kg of supersplash.

The decomposition of the superalloys according to D. nomu invention occurs from the point of view of the space-time yield is particularly preferable in the case when in the molten salt leak air and/or oxygen. Preferably through the molten salt flow mixture of air and oxygen, which contains from 25 to 95 volume percent of air and from 5 to 75 volume percent oxygen, preferably from 35 to 80 volume percent of air and from 20 to 65 volume percent of oxygen.

The decomposition of the superalloys according to the invention is carried out at a temperature from 800 to 1200°C. Preferably, the decomposition is carried out at a temperature of from 850 to 1100°C., even more preferably at a temperature of from 900 to 1050°C. Good conditions exist in the case when the melt is additionally injected oxidant. As the oxidizing agent can be used, for example, nitrates, peroxodisulfate, peroxides of alkali metals and/or mixtures thereof. Preferably as oxidant use potassium nitrate, sodium nitrate, sodium peroxide, potassium peroxide, peroxodisulfate sodium, peroxodisulfate potassium and/or mixtures thereof. Especially good speeds decomposition is achieved in the case when the melt add from 5 to 25 weight. percent oxidizing component, calculated on the weight of the melt.

Preferred compositions of the molten salt are shown in table 2.

Table 2
NaOH (weight. percent)Na2SO4(the weight. percent)Na2CO3(the weight. percent)The oxidant (the weight. percent)
7010-20 (NaNO3)
775-18(K2S2O8)
805510 (Na2O2)
602086 (NaNO3)
6 (Na2S2O8)
8510-8 (Na2O2)

Particularly preferably in this case, when the decomposition in the melt is carried out in such a way that there is a partial oxidation of supersplash, or when, after approximately complete oxidation at some time ask reducing conditions. In the case of the method of decomposition according to this the invention in the melt pre-formed three factions, consisting of:

soluble in water oxometalates metals 6 and/or 7 of the side groups and/or 3rd main group of the periodic system of elements with alkali metals and/or mixtures thereof;

- water-insoluble components from the group of metals such as Co, Ni, Fe, Mn or Cr and/or their mixtures;

- oxides and/or insoluble in water oxometalates metals 4 or 5 side groups of the periodic system of elements with alkali metals and/or mixtures thereof.

These three factions in conclusion hydrometallurgical process. The subject of this invention is, therefore, a method of processing a decomposition product of melt supersplash, which includes the following stages:

a) a translation product of the decomposition of the melt in the solid phase in the cooling to room temperature;

b) grinding the hardened product of the decomposition of the melt;

c) transformation of the crushed product of the decomposition of the melt in water at a temperature less than 80°C to obtain aqueous slurry, which contains:

a solution consisting of a mixture of sodium compounds from the group that includes NaOH, Na2SO4, NaAl(OH)4and/or Na2CO3and Metallistov elements 6 and/or 7 a side group of the periodic system of the elements with alkaline metals,

- solid metal phase consisting of the metals Co, Ni, Fe, Mn and Cr,

- solid is ABC, consisting of hydroxides and/or metal oxyhydrates 3 main groups and metals 4 and/or 5 a side group of the periodic system of elements;

d) separating the aqueous fraction by filtration;

e) separation of the water-insoluble fraction of magnetic separation of metal components;

f) separation of the oxide fraction.

The method according to this invention is schematically presented in the attached figure 1. In accordance with figure 1, the product of decomposition of the melt supersplash (2) after cooling to room temperature, crushed, then ground in the mill and finally leached in water. Leaching is carried out preferably at a temperature less than 60°C, more preferably at a temperature less than 40°C. a characteristic of the product decomposition of the melt is that it is already pre-formed three factions, which during leaching in the water there as easily separated fractions:

the filtrate (4), which substantially contains the elements molybdenum, tungsten and rhenium in the form of Metallistov alkali metals

- insoluble in water balance (3), which contains the magnetic fraction consisting of almost all of the Nickel and cobalt shares alloy and about 1/3 of the chromium present in the metallic form, while other elements are presented in the form of side components which if present in trace quantities and

- non-magnetic fraction (5), which includes the elements aluminum, chromium, titanium, zirconium, hafnium, niobium and tantalum in the form of their oxides (e.g., Al2O3, Cr2O3, TiO2, ZrO2, HfO2Ta2O5, Nb2O5) or hydroxides (for example, Al(OH)3, Cr(OH)3, Ti(OH)4, Zr(OH)4, Hf(OH)4, Ta(OH)5, Nb(OH)5)or nitrides (e.g., AlN, CrN, TiN, HfN, NbN, and TaN), or tungsten (e.g., AlC, Cr2C3, TiC, ZrC, HfC, NbC and TaC).

Further processing of these fractions can be performed by known methods. So, rhenium after filtration can be distinguished from the filtrate (4) using a strongly basic ion exchanger, as described in DE 10155791. Does not contain rhenium solution, which contains a considerable degree of sodium molybdate and sodium tungstate, can be added to the process for extracting molybdenum, respectively, of tungsten.

Non-magnetic residue, which contains up to 15% tantalum, can be used as raw materials in tantalum metallurgy.

Magnetic residue is preferably used to produce cobalt and Nickel.

The method according to the invention is particularly suitable for the recovery of rhenium from superalloys. The subject of this invention further is a method for the recovery of rhenium from superalloys, which includes the following stages:

a) decomposition of supersplash to melt the salt, containing 60-95 weight. percent NaOH and 5-40 weight. percent Na2SO4;

b) cooling the melt to room temperature;

c) grinding the product decomposition of the melt;

d) transformation of the crushed product of the decomposition of the melt in water at a temperature less than 80°C and the receiving water suspension, which contains:

a solution consisting of a mixture of sodium compounds from the group that includes NaOH, Na2SO4, NaAl(OH)4and/or Na2CO3and Metallistov elements 6 and/or 7 a side group of the periodic system of the elements with alkaline metals,

- solid metal phase consisting of the metals Co, Ni, Fe, Mn and Cr,

- solid phase consisting of the hydroxides and/or metal oxyhydrates 3 main groups and metals 4 and/or 5 a side group of the periodic system of elements;

e) separating the aqueous fraction by filtration;

f) extraction of rhenium from aqueous fractions in accordance with DE 10155791.

The method of extraction of rhenium from superalloys according to this invention is preferably carried out so that the molten salt add up to 10 weight. percent soda (Na2CO3), preferably up to 8 weight. percent ash, more preferably up to 5 weight. percent ash calculated on the weight of the molten salt. The selection of rhenium from aqueous suspension is preferably carried out using a strongly basic ion exchange is the IR.

The advantage of the method according to this invention is that the reaction of the decomposition of supersplash in NaOH-Na2SO4the melt is exothermic. The process is well managed in the transmission of air or mixture of air and oxygen. Another advantage is that it is possible to almost completely remove all valuable substances.

The invention is explained in more detail by the examples below.

Examples

In a drum oven, directly heated by the flame of natural gas, load 1,97 t grinding dust supersplash (1) together with 2,50 t NaOH and 0.45 t Na2SO4is heated for 4 hours at a temperature of 1110°C and leave for another 1 hour at this temperature. The composition of the grinding dust supersplash are shown in table 3.

Thereafter, the resulting liquid-thick decomposition product of supersplash in the melt completely poured from the furnace. The cooled melt is first subjected to coarse grinding and then to grind sizes less than 2 nm. Get 5,26 t powdered product (2), which for leaching mingle 7.5 m3water. After submitting continue to mix for another 2 hours, and then filtered in a press filter and washed with 0.5 m3water. Get 2,10 t residue after filtration (3) and 9.3 m3the filtrate (4). The residue after filtrivahetusest in water and a metal magnetic components is separated from the oxide and hydroxide components, pumping the suspension is pumped through the circulation loop of the magnetic separator. Largely exempt from metals, the suspension is then passed through a press filter, the filtrate used for the next leaching. Get 1,46 tons of sludge metal (5) and 0.56 t sludge hydroxides (6). Sludge hydroxides (6) for the recovery of tantalum send tantalum factory, sludge metal (5) for further processing and sent to the Nickel factory. The filtrate, containing rhenium (3), served in the ion exchange columns for the extraction of rhenium. Further enrichment and purification of rhenium carried out by standard methods according to the prior art. Free of rhenium flow ion-exchange columns to send on tungsten factory for use as a pre-load when the leaching WO3. Extraction of rhenium is 94%.

The compositions of the grinding dust superalloys, as well as an important intermediate products are shown in table 3.

td align="center"> 4,4 29,0
Table 3
%kg%kg%kgg/lkg %kg%kg
Al9.28 are1834,472351,4630,5of 21.92040,121,7of 5.0528,4
Co7,091402,59136of 6.731410,00,09,461380,372,1
Cr7,171412,621386,691400,00,03,1646,216,4of 92.7
Hf0,220,084,30,214,30,00,00,091,40,522,9
Mo1,0520,60,3920,40,010,1of 2.2120,50,010,10,00,0
Ni51,3100119,099947,910000,00,068,810063,1417,7
Re1,5330,10,5830,50,091,93,120,131,80,010,0
Ta4,2082,81,5581,33,9382,00,00,01,9428,4of 9.5553,8
Ti1,5330,20,5830,51,4730,60,00,00,6810,03,5920,2
Wof 4.3886,21,6486,10,040,99,1685,30,060,90,00,0
Zr2,3345,90,8745,52,15450,00,00,9714,35,531,0
The nonmetal. components9,92
The amount of metals90,081775180714763391249249

1. Method of recovery of valuable metals from superalloys, superalloys which decompose in the molten salt containing 60-95 wt.% NaOH and 5-40 wt.% Na2SO4p is item in the melt pre-formed three factions, consisting of:
soluble in water oxometalates metals 6 and/or 7 of the side groups and/or 3rd main group of the Periodic system of the elements with alkali metals and/or mixtures thereof,
water-insoluble components from the group of metals such as Co, Ni, Fe, Mn or Cr and/or mixtures thereof,
oxides and/or insoluble in water oxometalates metals 4 or 5 side groups of the Periodic system of the elements with alkali metals and/or mixtures thereof.

2. The method according to claim 1, characterized in that the molten salt add up to 10 wt.% soda.

3. The method according to claim 2, characterized in that the molten salt contains 75-90 wt.% NaOH and 5-20 wt.% Na2SO4and/or 5-10 wt.% soda.

4. The method according to claim 1, characterized in that the superalloys contain as the main component one or more metals from the group including Ni, Co, Cr, or Al, and as a side component one or more elements from the group including Re, Mo, TA, Nb, W, Hf or Pt.

5. The method according to claim 4, characterized in that superslow contains 0.5-12 wt.% rhenium.

6. The method according to claim 1, characterized in that 1 kg of supersplash use at least 1 kg of molten salt.

7. The method according to claim 1, characterized in that the decomposition is carried out in the movable melt.

8. The method according to claim 1, characterized in that the decomposition is carried out in periodically or continuously operated tubular rotary furnace.

9. The method according to claim 1, Otley is audica fact, through the melt leak air and/or oxygen or a mixture.

10. The method according to claim 1, characterized in that the melt add oxidizing components from the group of such compounds as nitrate, peroxodisulfate, peroxides of alkali metals and/or mixtures thereof.

11. The method according to claim 10, characterized in that the melt add 5-25 wt.% oxidizing components in terms of the molten salt.

12. The method according to claim 9, characterized in that a melt flow mixture of air and oxygen, consisting of about 25-95% by air and 5-75% vol. the oxygen.

13. The method according to claim 10, characterized in that the decomposition is carried out at a temperature from 800 to 1200°C.

14. The method according to claim 10, characterized in that the superalloys partially oxidized.

15. The method according to one of claims 1 to 14, characterized in that the superalloys are scrap metal superalloys.

16. Method of recovery of valuable metals from superalloys, which includes the following stages:
a) a translation product of the decomposition of the melt according to claim 1 in a solid phase in the cooling to room temperature,
b) grinding the hardened product of the decomposition of the melt,
c) transformation of the crushed product of the decomposition of the melt in water at a temperature less than 80°C to obtain aqueous slurry that contains
a solution consisting of a mixture of sodium compounds from the group that includes NaOH, Na2SO4, NaA(OH) 4and/or Na2CO3and Metallistov elements 6 and/or 7 a side group of the Periodic system of the elements with alkaline metals,
solid metal phase consisting of the metals Co, Ni, Fe, Mn or Cr and/or mixtures thereof.
solid phase consisting of the hydroxides and/or metal oxyhydrates 3 main groups and metals 4 and/or 5 a side group of the Periodic system of elements,
d) separating the aqueous fraction by filtration,
e) separation of the water-insoluble fraction of magnetic separation of metal components,
f) separation of the oxide fraction.

17. The method according to item 16, wherein the transformation of the product of decomposition of the melt is carried out in water at a temperature less than 60°C.

18. The method according to item 16, wherein the transformation of the product of decomposition of the melt is carried out in water at a temperature less than 40°C.

19. The method according to one of PP-18, characterized in that the superalloys are a scrap of superalloys.

20. Method of recovery of valuable metals from superalloys, which includes the following stages:
a) decomposition of superalloys in molten salt containing 60-95 wt.% NaOH and 5-40 wt.% Na2SO4,
b) cooling the melt to room temperature,
c) grinding the product decomposition of the melt,
d) transformation of the crushed product of the decomposition of the melt in water at a temperature less than 80°C and receive in the ne suspension, which contains:
a solution consisting of a mixture of sodium compounds from the group that includes NaOH, Na2SO4, NaAl(OH)4and/or Na2CO3and Metallistov elements 6 and/or 7 a side group of the Periodic system of the elements with alkaline metals,
solid metal phase consisting of the metals Co, Ni, Fe, Mn or Cr and/or mixtures thereof,
solid phase consisting of the hydroxides and/or metal oxyhydrates 3 main groups and metals 4 and/or 5 a side group of the Periodic system of elements,
e) separating the aqueous fraction by filtration,
f) separation of rhenium from aqueous fractions.

21. The method according to claim 20, characterized in that the molten salt add up to 10 wt.% soda.

22. The method according to claim 20 or 21, characterized in that the superalloys are a scrap of superalloys.



 

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4 cl, 1 dwg

FIELD: metallurgy.

SUBSTANCE: procedure consists in separation of coal electrode and zinc cylinder, in flushing and dissolving in sulphuric acid. Also, flushing from ammonia chloride and zinc hydroxide is carried out with 0.2 M solution of sulphuric acid (H2SO4). Upon flushing residue of manganese oxide (IV) (MnO2), oxy-hydroxide of manganese (MnOOH) and coal mass (C) is crumbled in ball mills. Crumbled residue is dissolved in sulphuric solutions of concentration 0.05 mole/l containing 0.05-0.1 mole/l of oxalic acid at ratio of concentrations of ions of manganese and oxalic acid 1:5 at pH=1-2.2 and temperature of solution 80°C. Upon dissolving solution is filtered for removal of coal mass. Residues of zinc ions are removed from solution with isoamyl alcohol of 200 ml volume at presence of 2 M solution of ammonia thiocyanate and 0.5 M HCl, and there is performed neutralisation with 0.5 M solution of caustic soda (NaOH). Further, produced solution is evaporated at temperature 100°C to obtaining mass of crystalline compounds of composition sodium trioxalomanganate (IV) Na4[Mn(C2O42-)3] and salt of sodium oxalate (Na2C2O4). Produced mass is baked in atmosphere containing oxygen at temperature 400-500°C with production of MnO2 as a final product.

EFFECT: raised efficiency and ecological safety of procedure.

4 dwg, 3 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: procedure consists in mixing preliminary prepared iron containing waste of metallurgical production with crumbled carbon containing substance at amount of 15-60% of carbon from weight of waste and binding. Produced mixture is treated with water solution of Na2O·n·SiO2, pressed and dried. Also, iron containing waste is preliminary treated with suspension of system Ca(OH)2-H2O produced by roasted lime slaking with wader and containing 50-60% of calcium hydroxide and dried. As iron containing waste there is used oiled or not oiled scale of various origin.

EFFECT: reduced content of phosphorus in alloys on base of iron melted with fluxed briquettes.

3 cl, 3 tbl, 3 ex

FIELD: metallurgy.

SUBSTANCE: method involves simultaneous extraction of platinum and rhenium from acid solutions by introducing to the solution of sulphur-containing reducing agent (sodium thiosulfate). Then, deposit of sulphides and other connections of rhenium and platinum is separated from the solution. At that, sodium thiosulfate is added in the form of water solution by its uniform continuous supply to hot acid solution containing platinum and rhenium at the ratio of masses of reagent and soluble rhenium and platinum of 15 to 23.

EFFECT: reducing the flow of sulphur-containing reagent and increasing the extraction degree of platinum from acid solution to the concentrate owing to changing the procedure of introducing the precipitator reagent to acid solution containing platinum and rhenium.

1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: method involves acid leaching under the effect of alternating current to obtain a precipitate and a solution containing perrhenic acid and nitrates of non-ferrous metals, followed by precipitation of the obtained solution with sodium or ammonium sulphide in the presence of a reducing agent - hydroxylamine sulphate and washing with water and treating the sulphide precipitate with aqueous hydrochloric acid solution. The insoluble rhenium sulphide remaining after treatment with hydrochloric acid is filtered and dissolved in ammonia solution of hydrogen peroxide. The obtained solution is taken for extraction of the desired product.

EFFECT: extraction of rhenium with high output and degree of purity using a technologically simple and cheap method.

4 cl, 1 dwg, 2 ex

FIELD: metallurgy.

SUBSTANCE: procedure for extraction of mercury out of mercury-selenium final tailings consists in introduction of mercury selenium final tailings into pulp of calcium hydroxide and in re-pulping produced mixture, in burning in tubular furnace and in withdrawing process gases of burning containing vapours of mercury into condenser, in condensing mercury out of process gases, in production of stupp and in removing mercury from stupp. Also, mixture re-pulping is performed at ratio of hydroxide of calcium and selenium in final tailings Ca(OH)2:Se final tailings=(3.0-3.5):1. First, there is burned re-pulped mixture producing process gases not containing elementary selenium, further there is burned stupp upon its removal. Burning is carried out in a rotating tubular furnace at excess of oxygen. Output of mercury comes to 99 %. There is produced mercury-less ash with maximal content of bound selenium suitable for successive extraction of selenium.

EFFECT: increased output of mercury facilitating further extraction of selenium due to elimination of mercury losses owing to complete selenium binding with excess of calcium hydroxide at oxidising burning.

1 ex

FIELD: metallurgy.

SUBSTANCE: procedure for extraction of rhenium consists in leaching rhenium from catalyst with diluted solution of sulphuric acid, in sorption of rhenium on low-base anionite and in its de-sorption with solution of ammonia. Also, sodium thiosulphate at amount of 0.002-0.01 mole/l is added into diluted solution of sulphuric acid before rhenium leaching. Upon rhenium extraction non-dissolved residue is directed to extraction of platinum by known procedures.

EFFECT: reduced expenditures for extraction and purification of rhenium; reduced amount of platinum in material-in-process due to reduced extraction of platinum into solution of selective rhenium leaching.

1 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: procedure consists in processing wastes with sulphuric acid at raised temperature, in supplying hydrogen peroxide, in introducing rhenium, nickel and cobalt into leaching solution and in concentrating tungsten, niobium and tantalum in insoluble residue. Further, solution is separated from insoluble residue; extraction of rhenium from solution is leached with secondary aliphatic alcohol. Extract is washed and rhenium is re-extracted with leaching solution upon extraction. Hydrogen peroxide is supplied after main part of nickel and cobalt have passed into solution at maintaining redox potential in interval of 0.50-0.75 V relative to a saturated chlorine-silver electrode, while extraction of rhenium, extract washing and rhenium re-extraction are carried out on 2-5 steps.

EFFECT: increased extraction of rhenium at reduced consumption of oxidant, increased safety of procedure due to separated in time operations followed with release of hydrogen and oxygen.

6 cl, 4 ex

FIELD: metallurgy.

SUBSTANCE: sorption method of rhenium (VII) from water solution involves contact of the solution and absorbent at pH<5. At that, activated bone coal pre-treated with water or acid is used as absorbent.

EFFECT: effective extraction of Re ions from water solution.

4 dwg, 3 ex

FIELD: metallurgy.

SUBSTANCE: method for extraction of rhenium (VII) from the solutions containing non-ferrous metals involves preparation of solution and sorption of rhenium (VII). Sorption is performed from sulphate solutions containing cations of non-ferrous metals of nickel, cobalt or copper. The process is performed at mixing with AM-2"б" anionite or with absorbent bone coal at pH value of solutions, which is less than pH value of hydrolytic deposition of cations of non-ferrous metals.

EFFECT: increasing efficiency of selective extraction of rhenium from solutions of non-ferrous metals.

4 dwg, 3 tbl, 3 ex

FIELD: metallurgy.

SUBSTANCE: method involves contact of solution and anionite as absorbent. Sorption is performed at mixing. As anionite there used is porous anionite of mixed basicity of AM-2"б" grade, which is pre-treated with water, acid or alkali, and containing exchange groups CH2-N(CH3)2, .

EFFECT: optimisation of conditions of quick and effective extraction of rhenium ions from water solutions.

4 dwg, 3 ex

FIELD: metallurgy.

SUBSTANCE: proposed method comprises dissolving wastes in acid electrolyte by applying AC electric field thereto. Dissolving is performed in nitrate or sulphate electrolyte on applying half-wave asymmetric AC industrial-frequency current and on using second electrode made from tantalum or niobium plates. Note here that anodic dissolution is carried at acidity of nitrate electrolyte at the level of 200-250 g/l HNO3, while that of sulphate electrolyte making 150-200 g/l H2SO4 at 20-40°C and current of at least 1 kA.

EFFECT: increased process rate, better ecology.

3 cl, 3 tbl, 3 ex

FIELD: metallurgy.

SUBSTANCE: method involves dissolution of Tc-Ru alloy, extraction of ruthenium fraction in the form of hydroxide, conversion of ruthenium hydroxide by means of annealing to RuO4 ruthenium oxide and its hydrogen reduction to metal. Alloy is dissolved in acid solution in presence of catalyst at bubbling through solution of ozone-oxygen or ozone-air mixture. Reduction of ruthenium oxide to metal is performed in hydrogen-inert gas mixture. As catalyst there used are argentum salts Ag(I) or cobalt salts Co(II).

EFFECT: reducing the quantity of nuclear waste formed during extraction of ruthenium, and explosion safety of that process.

5 cl, 1 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: manganese dioxide obtaining method involves dilution of manganese-containing raw material in nitric acid so that solution of manganese nitrates and nitrates of calcium, potassium, magnesium and sodium impurities contained in the ore is obtained. Then, thermal decomposition of nitrates in autoclave is performed. Thermal decomposition is performed at constant pressure drop in autoclave, starting from pressure of 0.6 MPa and reducing it to the end of the process to 0.15 MPa. At that, pulp is constantly mixed at thermal decomposition with the mixer rotating at speed of 1-15 rpm and with superimposition of vibration on it with frequency of 20-50 Hz. Method can be implemented at chemical plants provided with pressure autoclaves.

EFFECT: obtaining manganese dioxide of improved quality.

2 tbl, 2 ex

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