Method of products reprocessing, containing chalcogenides of base metals, lead, platinum metals, gold and silver

FIELD: metallurgy.

SUBSTANCE: invention relates to noble metals metallurgy and can be used for reprocessing of different wastes of refining, such as dust-fumes or water-insoluble residues of dust-fumes. Method of products reprocessing, containing chalcogenides of base metals, lead, platinum metals, gold and argentum includes leaching of initial product in solution of caustic soda, separation of received alkaline solution from insoluble residue. Insoluble residue is subject to melting with addition of manufactured products of refining, sodium-bearing flux and carbonaceous reductant. After melting it is implemented grinding of separated bottom heavy phase into the powder and its treatment as a concentrate of refining. Into received during leaching initial products alkaline solution it is added sulfuric acid up to pH=4-6, it is separated laid-down from the solution deposit of hydroxides on the basis of tellurium dioxide. Solution after the sediment separation is again treated by sulfuric acid up to pH=1-2, it is added sodium sulfite and separated laid-down deposit of metal selenium, and mother solution is subject to finishing de-refining.

EFFECT: cost cutting while de-refining of received during the reprocessing solutions.

1 ex

 

The invention relates to the metallurgy of noble metals (BM) and can be used in the technology of refining of platinum group metals (PGM).

At affinage inevitably formed of various non-target products and waste containing PGM, silver, gold, in particular, such as Paleochora or water-insoluble residues Perevozchikov (the concentration of Perevozchikov), the incoming dust and gas in the tunnel and into the gas purification system with different technological areas and areas.

A characteristic feature of Perevozchikov or the concentration of Perevozchikov is that their base is provided with a large number of different chemical elements and their compounds, mainly highly volatile chalcogenides base metals, ammonium chloride and silver, lead, soot carbon. This intermediate contains from 0.5 to 3% MPG (combined), from 0.05 to 0.2% gold, from 3 to 10% silver, 10 to 20% of lead, 4 to 8% of selenium, from 6 to 10% tellurium, from 2 to 4% of arsenic. Processing Perevozchikov or the concentration of Perevozchikov is very difficult and involves high material and labor costs.

From publicly available literature it is known that processing of Perevozchikov can be carried out by pyrometallurgical - melting blend containing as fluxes soda, borax, glass, and in some cases coal, and as to the of lectora noble metals used copper [fundamentals of metallurgy. V.5. - M.: metallurgy, 1968. S].

The disadvantages of this method is similar when it is used for processing Perevozchikov refining production, containing, along with BM significant amount of chalcogenides base metals, as follows:

- education in melting of large quantities of secondary Perevozchikov enriched with a highly volatile chalcogenides containing BM in need of recycling;

- transition chalcogenides smelting in the target alloys BM, which increases their mass consumption of reagents and work on refining.

There is a method of processing products containing chalcogenides base metals, lead, platinum group metals, gold and silver, according to which the original product is leached in a solution of caustic soda, separating the obtained alkaline solution from nerastvorimogo balance, melted the last with the addition of middlings refining, sodium fluxes and carbon reductant, defend and cooling the melt before solidification, share the cured product according to the phase boundaries, crushed and processed bottom heavy phase as the concentrate processing facilities [RF Patent №2291212, Efimov V.N., Temirov S.A., Moskalev A., Churkin, VA, Gubin MV - BI No. 1, 2007]. This method is the closest in technical essence to savla is the PTO method and adopted as a prototype.

Using the prototype method for processing Perevozchikov or the concentration of Perevozchikov refining production along with a number of positive features associated with the following negative consequences. In the leaching of the raw product in a solution of caustic soda in the alkaline solution is transferred not only a large part of the contained halogeno (selenium, tellurium and arsenic, - which is a useful enrichment directed to the melting of nerastvorimogo balance, but some, relatively small (20-30 mg/l) number of PGM.

In this regard, all the obtained alkaline solutions are inevitably subject to the finish obezobragivanii by the cementation process. However, the high saturation of the solutions with chalcogenide (tellurium and selenium) leads to increased consumption of cementing agent, the increase in the mass returned to the refining of the target product - cementite, undesirable contamination of the latest chalcogenide, arsenic and lead, and, as a consequence, great work on the finishing obezobragivanii solutions and processing the received cementation.

The proposed method aims to obtain a technical result, which consists in reducing the cost of finishing obezobragivanii solutions obtained by leaching products containing chalcogenides base metals, lead is C, the platinum group metals, gold and silver in a solution of caustic soda.

The achievement of the technical result is ensured by the fact that obtained by leaching of the raw product in caustic soda alkaline solution, after its separation from nerastvorimogo residue, add sulfuric acid until the solution pH environment of pH 4-6, separating precipitated from solution, the precipitate of hydroxides on the basis of tellurium dioxide, then the solution is again treated with sulfuric acid until the solution pH environment of pH 1-2, add salt sodium sulfite, separating the precipitation of metallic selenium, and the mother liquor is subjected to finishing obezobragivanii.

Thus, from the alkaline solution before operation obezbalivaniya gradually extract the first precipitate of hydroxides on the basis of tellurium dioxide, then metallic selenium, and finish obezobragivanii expose the remaining mother liquor. This reduces the flow of cementing agents, the output obtained cementation, the costs of recycling. From the cycle of refining can be derived two new products: a mixture of hydroxides on the basis of tellurium dioxide and metallic selenium.

Example usage.

Took 63 g wet (W=42,8%) of the original product (the concentration of Perevozchikov - the so-called "concentrate the dust electrify trow"), containing chalcogenides base metals, lead, platinum group metals, gold and silver. According to analysis of the original product (by dry weight) contained, wt.%: Pt - 0,53; Pd - 0,79; Rh - 0,03; Ir - 0,01; EN - 0,04; MPG (combined) - 1,40%; Au - 0,13; Ag - 5,8; Te - 7,2; Se - 6,5; Sn - 4,5; As-2, 6; Pb - 14, 5; Cu - 0,96; Sb - 2,9; Fe - 3,9%.

The original product was subjected to leaching in a solution of caustic soda, separated by filtering the alkaline solution from nerastvorimogo balance. It was obtained two products - alkaline solution in the amount of 300 ml, nerastvorim balance. The yield of the latter (by dry weight) was 20.0 g or 55.6% of running on the leaching of the original product. According to the analysis, the content of BM in the concentration amounted, %: Pt - 0,93; Pd - 1,40; Rh - 0,05; Ir - 0,017; EN - 0,067; Au - 0,23; Ag - 10,44. Thus, the content of PGMs, gold and silver (total) increased 13,13%, 1.79 times greater than it was in the source material prior to leaching.

In a solution of caustic soda from the original product moved base elements. Their concentration in the solution according to the results of the analysis was, g/l: Te - 7,11; Se - 6,23; Sn - 2,21; As - 2,55; Pb - 5,39; MPG (combined) - 17 mg/L. Thus, the solution of the original product has passed 82.2% of tellurium, 79.8 per cent of selenium, 40.9% of tin, 81,6% arsenic and 31.0% of lead. Copper, iron and antimony remained mainly in nerastvorim residue.

The alkaline solution was treated with concentri vannoy sulfuric acid to establish a pH of medium pH 5 and separated by filtration of precipitated from solution residue on the basis of tellurium dioxide. Thus obtained 300 ml and 5.38 g (dry weight) of sediment, which contained, per cent: The - 38,5; Se - 6,3; Sn - 11,7; As - 1,8; Pb - 27,8.

The concentration of base elements in the solution after separation of the hydroxide was, g/l: Te - 0,2; Se - 5,1; Sn - 0,1; As - 2,3; Pb - 0,4; PGM (total) - 14 mg/L.

To the resulting solution was added concentrated sulfuric acid to establish a pH of medium pH of 1.5, then added 6 g of sodium sulfite. The solution was passed with stirring for 2 h and separated by filtration of precipitated from solution precipitate metallic selenium. It was obtained 1.39 g (dry weight) of selenium containing 99.4% of the basic substance, and 300 ml of solution, which contained according to the analysis, g/l: Those To 0.19; Se - 0,44; Sn - 0,1; As - 1,9; Pb - 0,4; PGM (total) - 11 mg/L. This solution is aimed at finishing obezobragivanii.

Thus, the original alkali solution and, therefore, from the cycle of refining in the besieged two products, in aggregate, receive 97,2% tellurium, 93,0% selenium, or 95.5% tin, 25.8% of the arsenic and 92.6% of lead.

Proposed in the present method pre-treatment to be obezobragivanii solution from most of the impurities base elements greatly simplifies finishing the deposition of PGM cementation. It reduces the consumption of cementing agent, as the latter is not consumed in the deposition of halogeno, swint and tin, increases the PGM content in the received samantatah that the costs for subsequent refining.

The precipitate selenium can be used in the production of additional marketable products - metal selenium.

Nerastvorim in caustic soda the remainder of the original product (the concentration of Perevozchikov) was further processed according to the technology provided by the method of the prototype (without any differences).

For this nerastvorim in caustic soda residue was mixed with addition of concentrate refiner produced by the cementation processing solutions refining production (so-called cemented containing copper and iron, along with PGM).

This cemented contained, wt.%: Pt - 1,11; Pd - 1,59; Rh - 0,18; Ir - 0,08; EN - 0,24; MPG (combined) - 3,20%; Au - no; Ag - no; Se - 6,5; Those to 2.5; Cu - 18,2; Fe - 10,1%.

Additive cementate took in the amount of 20 g, i.e. to 100% by weight of nerastvorimogo in caustic soda source product (the so-called "concentrate electrostatic dust). It is taken two products added sodium fluxes (8 g of crushed silikatnogo glass, 4 g of sodium carbonate and 2 g of carbon reductant - Corsica. All components of the mixture were mixed and loaded into a melting alongby the crucible. The crucible was placed in the mine laboratory electric furnace and subjected to isothermal aging (heat) for 5 minutes at a temperature of 1300°C. At the end of the melting crucible was unloaded from the furnace.

After cooling, extracted from the crucible of the hardened product, which is divided by the formed interfaces. When this was received:

- 2.64 g of bottom heavy phase is the target of an alloy of platinum metals and gold at the following content of the analyzed elements (ICP data), %: Pt - 15,28; Pd - 21,55; Rh - 1,70; Ir - 0,70; EN - 2,08; MPG (combined) - 41,31%; Au - 1,14; Ag - 3,45; Se - 0,76; Te - 1,6; Sn - 6,29; As - 2,12; Pb - 7,95; Cu - 5,42; Sb - 22, 0mm Fe - 0,20%;

- was 12.75 g stenopogoninae light alloy, containing (according to the ICP), %: Pt - Being 0.036; Pd - 0,225; Rh - 0,007; Ir - 0,007; EN - 0,047; MPG (combined) - 0,322%; Au - 0,12; Ag - 15,65; Se - 10,82; Te - 5,17; Sn - 4,35; As - 0,63; Pb - 18,95; Cu - 29,17; Sb - 1,31; Fe - 8,21%;

- of 21.7 g of silicate-sodium slag, containing (according to the spectral analysis of platinum group metals and gold.

In a target rich alloy extracted, %: Pt - 98,85; Pd - 95,20; Rh - 97,94; Ir - 95,11; EN - 89,52; the amount of PGM - 96,36%. This target alloy is pulverized into a powder and processed as concentrate refining production.

Stenopogoninae light alloy, in which the extracted about 78% of selenium, 69% of tellurium, 94% copper, 81% of lead and 31% iron (from running in the heat quantities), processed using known methods.

Thus, using the proposed method of processing products containing chalcogenides base metals, lead, platinum group metals, gold and Orebro, including leaching of the raw product in a solution of caustic soda and providing pre-phased cleanup to be obezobragivanii alkaline solution from most of the impurities base elements (mainly from selenium and tellurium), - greatly simplifies finishing the deposition of PGM cementation, reduces the cost of cementing agent, to increase the PGM content in the received samantatah, to reduce the cost of their subsequent refining and to obtain a sediment selenium, which can be used in the production of additional commercial products.

A method of processing products containing chalcogenides base metals, lead, platinum group metals, gold and silver, including the leaching of the raw product in a solution of caustic soda, the Department received the alkaline solution from nerastvorimogo residue, melting of nerastvorimogo balance with the addition of middlings refining, sodium fluxes and carbon reductant, settling and cooling of the melt before solidification, separation of the hardened product on the phase boundaries, grinding dedicated bottom heavy phase in the powder and its processing as concentrate refining production, characterized in that obtained by leaching of the raw product in the couse is practical soda alkaline solution after its separation from nerastvorimogo balance add sulfuric acid until the solution pH environment of pH 4-6, separating precipitated from solution, the precipitate of hydroxides on the basis of tellurium dioxide, the solution after the precipitate was again treated with sulfuric acid until the solution pH environment of pH 1-2, add sodium sulfite, separating the precipitation of metallic selenium, and the mother liquor is subjected to finishing obezobragivanii.



 

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1 dwg

 // 2350667

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8 cl, 3 dwg

FIELD: noble metal hydrometallurgy.

SUBSTANCE: invention relates to method for acid leaching of platinum method from secondary raw materials, in particular from ceramic support coated with platinum metal film. Target metals are leached with mixture of hydrochloric acid and alkali hypochlorite at mass ratio of OCl-/HCL = 0.22-0.25 and redox potential of 1350-1420 mV.

EFFECT: decreased leaching temperature, reduced cost, improved platinum metal yield.

2 ex

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