Precious metal concentrate preparation method

FIELD: precious metal hydrometallurgy.

SUBSTANCE: invention relates to methods for sorption-assisted recovery of metals from materials containing them. Method of invention proposes recovering precious metals from solution in redox mixture with involvement of sorption of these metals by added sorbent, which is further burnt down. Sorbent is added portionwise and weight of each portion constitutes 0.11-0.50 total weight of added sorbent. Portions are added in time moments between the beginnings of two consecutive additions within a time range constituting 0.14-0.86 total sorption time period. Moreover, number of sorbent portions is selected between 2 and 9.

EFFECT: increased degree of precious metal recovery.

4 cl, 16 ex

 

The present invention relates to hydrometallurgy of precious metals, in particular, to methods for producing concentrates of these metals from the aqueous solution by sorption.

A method of obtaining concentrates of precious metals in the platinum group metals from acidic solutions in which they are present in the form of complex anions of acids by contacting the solution with an anion exchange material "Emeraldine" in static or dynamic modes, followed by the separation of precious metals from the anion exchange material by burning the past (US 2371119, CL 75/108, 1945). The disadvantage of this method is not a high degree of extraction of precious metals and the low capacity of the sorbent with respect to palladium.

The method for extracting noble metals in the form of platinum from spent catalysts by treating the crushed catalyst solutions of concentrated mineral acids and oxidizing agents (HCl+HNO3HCl+Cl2HCl+H2O2) and then passing the resulting solution through a layer of anion exchange resin Duolite A101D and burning last at 800° (US 3999983, CL 75/365, 01 G 55/00, With 22 In 61/00, 1976). The disadvantage of this method is a multi-stage, duration of operations, low capacity anion exchange resin with respect to the noble metals and,as a consequence, significant energy costs for incineration.

The method for extracting noble metals from solutions after leaching of ores and tailings by passing the solution through a layer of anion exchange resin "PAZ 4" and burning the past (US 5215575, CL 75/744, 01 G 005/00, 1993). The disadvantage of this method is the low degree of extraction of gold.

The closest in technical essence and the achieved result to the present invention is a method of obtaining a concentrate of precious metals from their solution in acid-oxidation mixture by adsorption of these metals from solution was injected once into it sorbent and subsequent burning of the sorbent (EN 2116362, C22 In 3/24, 11/00, 01 J 23/96, 1998). In a known way as a sorbent using 1-hydroxy-2-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of gold and palladium, respectively 98,5 and 97.1%.

The main disadvantages of this method are:

- not a high degree of extraction of gold and palladium from the source material, which are used catalysts based on silica gel and aluminum oxide;

the relatively high consumption of sorbent-exchanger per unit mass of metal being recovered;

- the absence of unequivocal recommendations on how the introduction of sorbent-exchanger in the solution from the treatment of precious metals.

The technical problem, which is aimed at solving the present invention are getting the highest possible degree of recovery of precious metals from solution in the concentrate of each sorbent, reducing consumption of sorbent per unit mass of metal being recovered.

These technical problems are solved in the method of obtaining a concentrate of precious metals from their solution in acid-oxidizing mixture comprising the sorption of these metals from solution was injected him with a sorbent and subsequent combustion of the sorbent, the sorbent is injected into the solution in portions, and the weight of each portion is 0.11-0.50 to of the total mass of the injected sorbent, and the portions are inserted through the period of time between the beginning of the inputs of the preceding and following portions lying in the range of 0.14-0,86 of the total period of time of sorption. In addition, portions of the sorbent is injected periodically and the number of portions is chosen in the range from 2 to 9, as the acid-oxidizing mixture using HCl and/or H2O2HCl and/or Cl2HCl and/or Br2HCl and/or NaClO3HCl and/or HNO3mixtures of HF and HCl and/or HNO3mixtures of H2SO4and HCl and/or H2O2mixtures of HCl and HBr and/or H2O2mixtures of HCl and HI and/or NaClO3and I2HCl and/or Cl2and Br2and as sorbent using 1,2-bis-(perhydro-1,3,5-Dityatin-5-yl)ethane, 1-hydroxy-2-(Perg is draw-1,3,5-Dityatin-5-yl)ethane, 2-(perhydro-1,3,5-Dityatin-5-yl)acetic acid, politician. (Here and below the title sorbents are given in the Geneva nomenclature).

The main distinguishing features of the method according to the present invention consist in that the sorbent is injected into the solution in portions, and the weight of each portion is 0.11-0.50 to of the total mass of the injected sorbent, and the portions are inserted through the period of time between the beginning of the inputs of the preceding and following portions lying in the range of 0.14-0,86 of the total period of time of sorption.

Additional distinguishing features of the proposed method lies in the fact that portions of the sorbent is injected periodically and the number of portions is chosen in the range from 2 to 9, the acid and/or oxidant using HCl and/or H2O2HCl and/or Cl2HCl and/or Br2HCl and/or NaClO3HCl and/or HNO3mixtures of HF and HCl and/or HNO3mixtures of H2SO4and HCl and/or H2O2mixtures of HCl and HBr and/or H2O2mixtures of HCl and HI and/or NaClO3and I2HCl and/or Cl2and Br2and as sorbent using 1,2-bis-(perhydro-1,3,5-Dityatin-5-yl)ethane, 1-hydroxy-2-(perhydro-1,3,5-Dityatin-5-yl)ethane, 2-(perhydro-1,3,5-Dityatin-5-yl)acetic acid, politician.

The present invention meets the condition of patentability - novelty", as in the prior art failed to find technical solutions, it is vital to the E. signs which would coincide with all the signs, available in independent claim of the present invention.

The present invention meets the condition of patentability - "inventive step", since the prior art has failed to find technical solutions, the essential features of which would perform the same technical problem on which the present invention is directed.

The invention is illustrated by the following examples.

Example 1. To obtain a concentrate of platinum and palladium use their solution in the acid-oxidizing a mixture of 0.5 l, containing 70 vol.% aqueous HCl (35 wt.%) and 30 vol.% aqueous solution of H2About2(30 wt.%). The concentration of platinum and palladium in the solution of acid-oxidizing mixture, respectively 4.8 and 0.5 g/l Solution of acid-oxidizing mixture is placed in a glass reactor with a volume of 1 l with agitator, connected with a return condenser, heated to a temperature of 90-100°C. as a sorbent use politician, which is injected portions, and the mass of each portion is 0,294 g (0,11 on the total weight of the sorbent), the total mass of the injected sorbent equal to 2.65 g, and the portions are inserted through the period of time 6,67 minutes Number of servings of sorbent equal to 9, the total sorption time is 1 hour. After processing is complete, the sorbent is separated from the solution by filtration, washed the t water dried and burned in a muffle furnace at a temperature of 600-650°C. the content of platinum and palladium in the resulting concentrate determines that the degree of extraction of platinum and palladium respectively to 98.6% and 98.3%. Consumption of sorbent was 1.07 g/g (Pt+Pd), which is 12% less compared to the flow of the sorbent when a single dose.

Example 2. The treatment is carried out as in example 1, with the difference that portion of the sorbent is injected through a period of time equal to 0,86 of the total period of time of sorption of 1 hour. The number of portions of the sorbent is 2. The degree of extraction of platinum and palladium, respectively, which accounted for 98.9% and 98.7 per cent. Consumption of sorbent was 1.02 g/g (Pt+Pd), which is 15% less compared to the flow rate of the sorbent when a single dose.

Example 3. The treatment is carried out as in example 1, with the difference that portion of the sorbent is injected through a period of time equal to 0.5 of the total period of time of sorption of 1 hour. The number of portions of the sorbent is 2. The degree of extraction of platinum and palladium, respectively 99.5% and 99.1 per cent. Consumption of sorbent amounted to 0.96 g/g (Pt+Pd), which is 20% less compared to the flow of the sorbent when a single dose.

Example 4. The treatment is carried out as in example 1, with the difference that the mass of each portion of the sorbent is 0,098 of the total mass of the injected sorbent, i.e. below the lower limit in the claims, and portions inserted through periodinane, equal is 0.135 of the total period of time of sorption 1.75 hours, i.e. less than the lower limit in the claims. The degree of extraction of platinum and palladium, respectively 97,2% and 96.8 per cent. Consumption of sorbent was 1,09 g/g (Pt+Pd), which is 9% less compared to the flow rate of the sorbent when a single dose.

Example 5. The treatment is carried out as in example 1, with the difference that the mass of the first portion of sorbent is 0,51 of the total mass of the injected sorbent, i.e. above the upper limit in the claims, and portions inserted through the period of time equal to 0.87 from the total period of time of sorption 0.25 hour, that is more than the upper limit in the claims. The degree of extraction of platinum and palladium, respectively 97.3% and 97.4%of. Consumption of sorbent was 1,08 g/g (Pt+Pd), which is 10% less compared to the flow of the sorbent when a single dose.

Example 6. The treatment is carried out according to example 3, with the difference that the acid used 350 ml of 35 wt.% HCl solution, the oxidant - 25 ml liquid Cl2. The gold concentration in the solution of acid-oxidizing mixture of 0.05 g/L. as sorbent used 1-hydroxy-2-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of gold is 98.5%. Consumption of sorbent was 4.15 g/g Au, which is 17% less compared to the flow rate of the sorbent when a single dose.

Example 7. The treatment is carried out on the to example 6, with the difference that portion of the sorbent is injected periodically and the number of portions is equal to 3. The degree of extraction of gold of 99.5%. Consumption of sorbent was of 3.85 g/g Au, which is 23% less compared to the flow rate of the sorbent when a single dose.

Example 8. The treatment is carried out according to example 6, but the number of portions of the sorbent equal to 9. The extent of the gold recovery is 97, 5%. Consumption of sorbent was of 4.45 g/g Au, which is 11% less compared to the flow rate of the sorbent when a single dose.

Example 9. The treatment is carried out according to example 7, with the difference that the acid used 350 ml of 35% HCl, oxidant - 25 ml Br2and as sorbent 1,2-bis-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of gold is 98,9%. Consumption of sorbent was 0.84 g/g Au, which is 16% less compared to the flow rate of the sorbent when a single dose.

Example 10. The treatment is carried out according to example 7, with the difference that the acid used 350 ml of 35% HCl, oxidant - 100 ml of 30% NaClO3and as a sorbent - 2-(perhydro-1,3,5-Dityatin-5-yl)acetic acid. The degree of extraction of gold amounts to 98.6%. Consumption of sorbent was 0.71 g/g Au, which is 20% less compared to the flow of the sorbent when a single dose.

Example 11. The treatment is carried out according to example 7, with the difference that the acid used 350 ml of 35% HCl, oxidant - 150 ml 45% HNO 3and as a sorbent - 1-hydroxy-2-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of gold was 99.4%. Consumption of sorbent was 1.6 g/g Au, which is 13% less compared to the flow rate of the sorbent when a single dose.

Example 12. The treatment is carried out according to example 7, with the difference that the acid used 30 ml of 40% HF and 320 ml of 35% HCl, oxidant - 150 ml 45% HNO3and as sorbent 1,2-bis-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of gold is 99,3%. Consumption of sorbent was 0,81 g/g Au, which is 19% less compared to the flow rate of the sorbent when a single dose.

Example 13. The treatment is carried out according to example 7, with the difference that the acid used 25 ml of 93.5% N2SO4and 300 ml of 35% HCl, oxidant - 100 ml of 30% H2About2and as a sorbent - 2-(perhydro-1,3,5-Dityatin-5-yl)acetic acid. The degree of extraction of platinum and palladium, respectively 98,7% and 98.3%. Consumption of sorbent was 0.76 g/g (Pt+Pd), which is 14% less compared to the flow of the sorbent when a single dose.

Example 14. The treatment is carried out according to example 7, with the difference that the acid used 300 ml of 35% HCl and 30 ml of 46.8% HBr, oxidant - 100 ml of 30% H2About2and as a sorbent - 1-hydroxy-2-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of platinum and palladium, respectively 99,0% and 98.8 per cent. Consumption is armenta was 1.4 g/g (Pt+Pd), 21% less compared to the flow rate of the sorbent when a single dose.

Example 15. The treatment is carried out according to example 7, with the difference that the acid used 350 ml of 35% HCl and 25 ml of 45.3% HI, oxidant - 100 ml of 30% NaClO3and 3 g of crystalline I2and as a sorbent - 1,2-bis-(perhydro-1,3,5-Dityatin-5-yl)ethane. The degree of extraction of platinum and palladium respectively to 99.2% and 99.3%. Consumption of sorbent was 0.82 g/g (Pt+Pd), which is 18% less compared to the flow rate of the sorbent when a single dose.

Example 16. The treatment is carried out according to example 7, with the difference that the acid used 300 ml of 35% HCl, oxidant - 25 ml liquid Cl2and 25 ml Br2and as a sorbent - 2-(perhydro-1,3,5-Dityatin-5-yl)acetic acid. The degree of extraction of platinum and palladium respectively to 98.6% and 98.7 per cent. Consumption of sorbent 0.85 g/g (Pt+Pd), which is 15% less compared to the flow rate of the sorbent when a single dose.

From the comparison results, the degree of extraction of precious metals from examples 1-3 with similar results from examples 4 and 5 show the following. When the amount of the sorbent below the lower limit in the formula of the invention (example 4), the degree of extraction of platinum and palladium decreases with 99.5% and 99.1 per cent respectively (example 3) to 97,2% and 96.8 per cent respectively (example 4). When increasing the number of injected sorbent and the time between the beginning of the inputs of the preceding and following portions above the upper limit in the claims with insufficient time sorption degree of extraction of platinum and palladium is reduced a 98.9% and 98.7 per cent, respectively (example 2) to 98.1% 97,4%, respectively (example 5). The sorbent in the first place, extracts from solutions of noble metals, however, excess, excessive contact times and higher temperatures may incidentally remove heavy metals. The lack of sorbent does not fully extract the precious metals from the solution.

From the comparison of the results of examples 1 to 3 and 6 to 16 of the present invention and the method of the prototype shows that the degree of extraction of precious metals according to the present invention (98,6÷99,5%) exceeds the degree of extraction of precious metals in the method-prototype (97,1÷98,5%) 1÷1,5%.

In addition, portions introduction of the sorbent in the acid-oxidizing mixture according to the present invention allows to reduce the consumption of 9-23%.

Thus, the present invention can be realized most effectively applied for the recovery of precious metals from the containing solutions.

1. A method of obtaining a concentrate of precious metals from their solution in acid-oxidizing mixture comprising the sorption of these metals from solution was injected him with a sorbent and subsequent combustion of the sorbent, wherein the sorbent is injected into the solution in portions, and the mass of each portion is 0.11-0.50 to the total mass of the injected sorbent, and the portions are injected through the PE the iodine of time between the beginning of the inputs of the preceding and following portions, lying in the range of 0.14-0,86 total period of time of sorption.

2. The method according to claim 1, characterized in that portion of the sorbent is injected periodically and the number of portions is chosen in the range from 2 to 9.

3. The method according to claim 1, characterized in that the acid-oxidizing mixture using HCl and/or H2O2HCl and/or Cl2HCl and/or Br2HCl and/or NaClO3HCl and/or HNO3mixtures of HF and HCl and/or HNO3mixtures of N2SO4and HCl and/or H2O2mixtures of HCl and HBr and/or H2O2mixtures of HCl and HI and/or NaClO3and I2HCl and/or Cl2and Br2.

4. The method according to claim 1, characterized in that the sorbent using 1,2-bis-(perhydro-1,3,5-Dityatin-5-yl)ethane, 1-hydroxy-2-(perhydro-1,3,5-Dityatin-5-yl)ethane, 2-(perhydro-1,3,5-Dityatin-5-yl)acetic acid, politician.



 

Same patents:

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3 cl, 11 tbl, 11 ex

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The invention relates to the processing of uranium ores
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FIELD: mining and metallurgy industry.

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5 cl, 3 dwg, 5 tbl, 1 ex

FIELD: nonferrous metallurgy and precious metal technology.

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1 tbl, 18 ex

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3 cl, 3 tbl, 1 ex

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9 cl, 1 dwg, 1 tbl, 3 ex

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1 tbl, 1 ex

FIELD: separation of palladium from waste mangani-palladium catalyst and cleaning of palladium.

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EFFECT: enhanced purity of metallic palladium at minimum losses of catalyst at all stages of chemical treatment.

4 ex

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EFFECT: increased extraction of antimony and precious metals.

15 cl, 3 tbl, 1 ex

FIELD: noble metal hydrometallurgy.

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

2 ex

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