Method to process metal-containing sulphide mineral raw materials with extraction of metals

FIELD: metallurgy.

SUBSTANCE: invention relates to the method for extraction of metals from metal-containing sulphide mineral raw materials. The method includes leaching with mixing of a sulphuric acid solution in presence of trivalent iron ions in at least two serially connected tubs, separation of leaching products into liquid and solid phases, iron oxidation in a liquid phase, return of the liquid phase after iron oxidation into leaching reservoirs, intermediate extraction of metals from liquid phases. At the same time the initial raw materials prior to leaching are exposed to preliminary acid treatment at PH=0.8-1.4, S:L=1:1. Leaching is carried out in two stages at the temperature of 75-95°, PH=1.0-1.2 and S:L=1:(3-6), concentration of trivalent iron ions of 30-45 g/l at each stage with separation of leaching products after each stage into liquid and solid phases and iron oxidation in a liquid phase after each stage and with extraction of metals at each stage from liquid phases after iron oxidation. To the first stage raw materials exposed to preliminary acid treatment are sent, and to the second stage - a solid phase is sent, produced after separation of leaching products at the first stage. The liquid phase, which was produced after oxidation of iron at the second stage, is returned to the last leaching reservoir of the same stage.

EFFECT: higher extent of extraction of all precious metals into a solution and reduction of process duration by 1,2-1,5 times.

4 ex, 1 dwg

 

The invention relates to the metallurgy of non-ferrous and noble metals, in particular to the extraction of metals from sulfide mineral products, waste products of mining and metallurgical enterprises, industrial mineral raw materials, namely, middlings and tailings, slag, sludge, Ogarkov and others

There is a method of processing metal-containing sulfide mineral raw materials extraction of metals, including canovai leaching of the feedstock in at least two series-connected tanks with stirring with a solution of sulfuric acid at a pH value below 1.8, the solids content of 10-60%, the concentration of ferric ions more than 3 g/l, temperature 50-99°C. After leaching the slurry from the last tank is sent to the clarifier-thickener to the division of solid and liquid phase, the solid phase is returned to the leaching in the first VAT, the liquid phase is directed to the bacterial oxidation of iron in a separate reactor, from which the oxidized liquid phase continuously displayed in the first VAT leaching. The oxidation of iron occurs at pH=1,4-2,2, temperatures up to 90°C with aeration by air, with the addition of batteries bacteria. From the clarifier-thickener periodically the liquid phase is displayed on the extraction of metals, and then it is used as a solution for veselaj is found.

When this pulp from the last VAT leaching is displayed in continuous mode in the separation of the solid and liquid phases, on bacterial oxidation of the liquid phase, and returning the liquid phase to leaching. Mineral products subjected to leaching, have a particle size of 60-100% of the class minus 0,071-0,074 mm When the separation of the slurry into solid and liquid phase portion of the slurry fraction of the solid phase and the colloidal particles oxidation products are in the liquid phase. For bacterial oxidation of liquid phase using Association cultures Glazovskaya and serratissima bacteria or bacteria immobilized on a neutral carrier. Leaching of metal-containing products and bacterial oxidation is performed with the use of vibration stirring. Metal-containing products before leaching are subjected to ultrasonic processing. In the leaching of metal-containing products by ultrasonic treatment (Application for invention of the Russian Federation No. 2009117574, CL SW 3/04, SW 3/08, SW 3/18, publ. 20.11.2010,)

The disadvantage of this method is its low efficiency, because after leaching and separation of the solid phase, which contains small amounts of precious metals, return in the first VAT leaching. Processing it in a single operation with the raw material is not effective. Also what about the, raw material that is sent to the leaching contains alkalizing substances that contribute to the deposition of iron. The decrease in the concentration of Fe+3leads to loss of speed leaching and in General to decrease the efficiency of the method. After leaching for the extraction of metals liquid phase, which contains a large number of bivalent iron ions, which makes the selective extraction of metals from it.

The objective of the invention is to increase the efficiency of the method of processing metal-containing sulfide mineral raw materials extraction of metals by increasing the rate of oxidation and reduce the duration of extraction of metals from metal-containing sulfide minerals and completeness of extraction of all valuable metals in solution.

This object is achieved in that in the known method of processing metal-containing sulfide mineral raw materials extraction of metals, including leaching of the feedstock by mixing a solution of sulfuric acid in the presence of trivalent iron in at least two series-connected tanks, separation of the products of the leaching liquid and solid phases of iron oxidation in the liquid phase, the return of the liquid phase after oxidation of iron in tanks for leaching, intermediate extraction of metal is from liquid phases, according to the invention, the feedstock prior to leaching is subjected to a preliminary acid treatment at pH=0,8-1,4, T:W=1:1, the leaching is carried out in two stages at a temperature of 75-95°, pH=1.0 to 1.2 and T:W=1:(3-6), the concentration of ferric ions 30-45 g/l at each stage of separation of leachate after each stage liquid and solid phase and the oxidation of iron in the liquid phase after each stage and with the extraction of metals on each phase from the liquid phase after oxidation of iron, with the first stage is directed metallsoderjasimi the raw material is subjected to a preliminary acid treatment, and the second phase - solid phase obtained after separation of leachate in the first phase and the liquid phase, which was obtained after oxidation of iron in the second stage, return in the last VAT leaching the same stage.

Preliminary acid treatment at T:W=1:1 and pH=0,8-1,4 neutralizes alkalizing substances included in the composition of raw materials, thereby reducing the possibility of precipitation of ferric leaching. The presence in the slurry a sufficient amount of ferric ions increases the rate of oxidation and extraction of metals in solution. In addition to the neutralization of alkalizing substances acid treatment promotes partial destruction of the material already on this about what erali, hence, the leaching time is significantly reduced, which increases the efficiency of the method.

Conditions T:W=1:1 and pH=0,8-1,4 optimal, because the density of the pulp is achieved maximum performance and the intensity of the acid treatment.

The leaching in two stages allows to process the solid phase obtained in the first stage, and a part of the liquid phase obtained after the oxidation in the second stage, individual process scheme, the first stage in a continuous mode served metallsoderjasimi the raw material is subjected to acid treatment, which also increases the efficiency of the method.

The same parameters and conditions of leaching on stage 1 and 2 do not require any operations for the preparation of material to the second stage.

It is known that the increase of temperature, the concentration of sulfuric acid, ferric ions increase the rate of oxidation and extraction of metals in solution. The leaching conditions: temperature of 75-95°, pH=1.0 to 1.2 and T:W=1:(3-6), the concentration of iron 30-45 g/l optimal and can effectively carry out the leaching of metal-containing sulfide minerals.

On extraction of metals enter the solution after the oxidation of the iron, because the extraction of metals in the presence of ferric ions is easier, which also increases the efficiency with the person.

Method of leaching the metal-containing sulfide mineral raw materials shown in the drawing, where 1 Chan for preliminary acid treatment, 2, 3 - vats for the first leaching stage, 4 - thickener to separate the solid and liquid phases of the first stage, 5 - regeneration column for the first stage of oxidation of iron, 6, 7 - tanks for leaching the second stage, 8, 9 - thickeners second stage, 10 - regeneration column for iron oxidation of the second stage.

The method is as follows.

Crushed metallsoderjasimi sulfide mineral raw materials to a particle size of not less than 80% of the class minus 0.44 mm goes to Chan 1 on the preliminary acid treatment at pH=0,8÷1,4, a temperature of 25-35°C to neutralize alkalizing substances included in the composition of the material, the pulp density of not less than T:W=1:1, duration of surgery - 30 minutes

After a preliminary acid treatment the pulp is sent to the first stage of leaching at least two series-connected tank 2, 3. Conditions and the following parameters: temperature of 75-95°, pH=1,0-1,2, T:W=1:(3-6), the concentration of ferric ions 30-45 g/l, duration of operation at least 5 hours. Unloading tanks leaching occurs in continuous mode, to ensure the free volume of fresh solution of ions of trivalent jelly is and after its oxidation in the regeneration column 5 and pulp - after the acid treatment in the VAT 1.

The solid phase after separation of the products leaching into the thickener 4 is fed to stage 2 in the cascade of installed tanks 6, 7 and at least 2 pieces. The liquid phase after separation from the thickener 4 is supplied to the oxidation in the regeneration column 5, where the oxidation of ions of bivalent iron to ferric iron. As the oxidant used either acidophilus zhelezookisnye thiobacteria from acidithiobacillus genus, or chemical oxidizing agents include oxygen, ozone, chlorine. At the outlet of the regenerator column 5, approximately 40% of the solution is directed to the extraction of metals, as in the first stage leach is the most active oxidation of metal-containing sulfide minerals and the concentration of metals is sufficient to highlight them. Selective separation of non-ferrous metals is easier from a solution of ferric than divalent. The rest of the solution is directed to the first stage leach.

The second stage leaching is carried out under the same conditions and parameters, only used as the raw material of the solid phase after leaching in the first stage and part of the liquid phase of the second stage obtained after oxidation of iron in the regeneration column 10. After leaching at least two series-connected Chan is x 6, 7, the pulp is sent in two series set thickener 8, 9, where the separation into solid and liquid phases. The liquid phase is directed to the oxidation of the bivalent iron ions in the regeneration column 10. As oxidizing agents are used either acidophilus zhelezookisnye thiobacteria from acidithiobacillus genus, or chemical oxidizing agents include oxygen, ozone, chlorine. Then part of the liquid phase (about 15%) from the regenerator column 10 is directed to the extraction of metals, and the second part (about 85%) - the second stage leach tank 7. The solid phase of the two thickeners 8, 9 merged, and depending on the composition is either dumped or additional extraction from it of useful components.

The invention is illustrated by examples of implementation of the method.

Example 1 (the prototype)

Extraction of zinc from sulphide copper-zinc-pyrite middlings grain size of 80% minus 0,074 mm, containing 15.6% zinc, 1.5% copper. Processing of concentrate include the following:

- loading and leaching the product in two consecutive vats with vibration stirring at a temperature of 85°C, the concentration of sulfuric acid corresponding to the value of pH=1,3, the concentration of ferric ions 8-14 g/DM3the pulp density of 60% solids;

- a continuous output from the second VAT of pulp in the tank-shasti the spruce, continuous return of condensed solid phase from the tank into the first VAT leaching;

the liquid phase from the settling tank with a temperature of 60°C and a concentration of ions of bivalent iron 16-19 g/l enters the bacterial oxidation in a tubular bioreactor continuous displacement from immobilized on the fiber biomass Glazovskaya and serratissima thermophilic bacteria from which the oxidized liquid phase is continuously withdrawn from the bioreactor in the first VAT leaching;

from clarifier-thickener periodically the liquid phase is displayed on the extraction of metals, the solid phase is displayed on the subsequent processing cycle enrichment;

- the return of the liquid phase after extraction of metals by leaching.

In the leaching of copper-zinc-pyrite of concentrate with an average duration of 18 hours, the extraction of zinc in the solution was 92.6%.

Example 2 (the proposed method)

The extraction of copper and zinc from sulfide copper concentrate flotation containing 9,3% zinc and 1.2% copper. The processing of such raw materials include the following:

- preliminary acid treatment when the concentration of sulfuric acid corresponding to the value of pH=0,8, T:W=1:1, 25°C, duration - 30 minutes;

- leaching of concentrate at T:W=1:3, a temperature of 75°C, when the concentration of the sulfuric acid thus is estoya value pH=1,0 for 8 hours, the ferric ion concentration 30 g/l in several vats of 3 units from the output of the last of the pulp in a continuous mode;

- thickening of the pulp of the third Chan;

- thickening filtrate through the heat exchangers is directed to the oxidation of ferrous iron (concentration of 26 g/l) in the regeneration column, the regeneration is carried out acidophilus zhelezookisnye tinavie by bacteria of the genus from acidithiobacillus;

- the return part of the solution of oxidized iron in the leaching (60%), the other part on the extraction of metals by cementation or by extraction (40%);

- loading of the solid phase of the thickener in the second stage of leaching in several vats of 3 pcs. Conditions and parameters as in stage 1 (T:W=1:3, temperature 75°C, pH=1.0, time 8 hours, the concentration of ferric 30 g/l);

- thickening of the pulp of the second stage leaching;

- thickening filtrate through the heat exchangers is directed to regeneration;

- the return part of the solution of oxidized iron in the leaching (85%), the other part on the extraction of metals by cementation (15%).

When the leaching of concentrate on the proposed method, the average duration of 15.5 hours removing the zinc in the solution amounted to 94%, and copper 90%.

Example 3 (the proposed method)

The extraction of copper and zinc from copper smelting slag plant size of 80% minus 0,044 mm, containing by weight of 0.55% copper, 5.5% zinc. PE is arabada slag includes the following operations:

- preliminary acid treatment at pH=1.4 and T:W=1:1 for 30 min;

- leaching slag at T:W=1:6, at 95°C, pH=1.2 V for 7 hours, the concentration of ferric ions 45 g/l in three tanks installed in series with the output of the last of the pulp in a continuous mode;

- thickening of the pulp of the third Chan;

- thickening filtrate through the heat exchangers is directed to the oxidation of the bivalent iron ions (concentration of 26 g/l) in the regeneration column, the regeneration is carried out acidophilus zhelezookisnye tinavie by bacteria of the genus from acidithiobacillus;

- the return part of the solution of oxidized iron in the leaching (60%), the other part on the extraction of metals by cementation (40%);

- loading of the solid phase of the thickener in the second stage of leaching in 3 tanks installed in series. Conditions and parameters as in stage 1 (T:W=1:6, the temperature of 95°C, pH=1,2, 7 hours, the concentration of ferric 45 g/l);

- thickening of the pulp of the second stage leaching;

- thickening filtrate through the heat exchangers is directed to regeneration;

- the return part of the solution of oxidized iron in the leaching (85%), the other part on the extraction of metals by cementation or by extraction (15%).

Leaching of slag on the proposed method, the average duration of 13 hours removing C the NCA solution was 84%, and copper 86%.

Example 4 (the proposed method)

The extraction of copper and zinc from sulfide copper concentrate flotation containing 9,3% zinc, 1.2% of copper. Processing involves the following steps:

- preliminary acid treatment when the concentration of sulfuric acid corresponding to the value of pH=0,8, T:W=1:1, 25°C, duration - 30 minutes;

leach T:W=1:3, a temperature of 75°C, at a concentration of sulfuric acid corresponding to the value of pH=1,0 for 8 hours, the concentration of ferric ions 30 g/l in several vats of 3 units from the output of the last of the pulp in a continuous mode;

- thickening of the pulp of the third Chan;

- thickening filtrate through the heat exchangers is directed to the oxidation of the bivalent iron ions (concentration of 23 g/l) regeneration capacity, regeneration is carried out by blowing the filtrate concentrated oxygen;

- the return part of the solution of oxidized iron in the leaching (60%), the other part on the extraction of metals by cementation or by extraction (40%);

- loading of the solid phase of the thickener in the second stage of leaching in several vats of 3 pcs. Conditions and parameters as in stage 1 (T:W=1:3, temperature 75°C, pH=1.0, time 8 hours, the concentration of ferric 30 g/l);

- thickening of the pulp of the second stage leaching;

the filtrate thickening through heat e is mennike is sent for regeneration;

- the return part of the solution of oxidized iron in the leaching (85%), the other part on the extraction of metals by cementation (15%);

When the leaching of concentrate on the proposed method, the average duration of 15.5 hours removing the zinc in the solution amounted to 94.5%, and copper 89,8%.

Thus, it is shown that the processing of metal-containing sulfide mineral raw materials on the proposed method allows you to translate zinc and copper in the solution of the concentrate with high rates of extraction of zinc 94-94,5%and copper up to 90%, the duration of the method of 15.5 hours. The prototype extraction of zinc from middlings 92,6%, copper remains in the solid phase leaching and to extract the necessary additional technological operations (diplomacia copper minerals, and others), the duration of the method 18 hours. Recycling of slag with a low content of useful components in the proposed method allows for only 13 hours to extract more than 80% zinc and copper in solution.

The proposed method is more effective since it allows a high degree to retrieve all of the precious metals in solution, increase the rate of their oxidation and reduce the duration of the process 1.2-1.5 times.

The method of processing metal-containing sulfide mineral raw materials extraction of metals, including leaching with agitation RA is tworoom sulfuric acid in the presence of ferric ions in at least two series-connected tanks, separation of the products of the leaching liquid and solid phase, the oxidation of iron in the liquid phase, the return of the liquid phase after oxidation of iron in tanks for leaching, intermediate extraction of metals from the liquid phase, characterized in that the feedstock prior to leaching is subjected to a preliminary acid treatment at a pH of 0.8 to 1.4, T:W=1:1, the leaching is carried out in two stages at a temperature of 75-95°, pH of 1.0-1.2 and T:W=1:(3-6), the concentration of ferric ions 30-45 g/l at each stage of separation of leachate after each stage liquid and solid phase, the oxidation of iron in the liquid phase after each stage and the extraction of metals at each stage of the liquid phase after oxidation of iron, with the first stage direct metallsoderjasimi the raw material is subjected to a preliminary acid treatment, and the second phase - solid phase obtained after separation of leachate in the first phase and the liquid phase obtained after the oxidation of the iron in the second stage, return in the last VAT leaching the same stage.



 

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4 cl, 3 tbl, 1 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to a method for treatment of low-grade oxidized zinc ores and concentrates with zinc, manganese, iron, lead, silver, calcium and silicon dioxide recovery. The method comprises crushing, fine crushing, lixiviating, settling-down of the above components from solutions, wherein the lixiviating shall be performed in stages: during the first and the second stage - lixiviation by sulphuric acid solution over the reducing substance, the oxidation-reduction potential φ (ORP): at the first stage φ=380-420 mV, at the second stage φ=420-460 mV. At the third stage lixiviation is performed by an ammonium carbonate solution with the composition (g/dm3): 60-110 NH3 general 30-65 C02 general while at the fourth stage it is performed by nitric acid NHO3. At the fifth stage sulphating roasting with H2SO4 term with further water leaching is performed, the sixth stage being lixiviation with ammonium fluoride aqueous solution of acid NH4HF2. The obtained soutions shall be puriied and used for zinc, manganese, iron, lead, silver, calcium, silicon dioxide and sodium sulfate, ammonium nitrate recovery. EFFECT: enhanced zinc recovery and rational utilization of the stock.

16 cl, 1 dwg, 3 ex

FIELD: metallurgy.

SUBSTANCE: procedure consists in charging wastes of zinc into crucible of furnace, in their re-melting at temperature equal or higher, than temperature of melting at presence of anhydride of boric acid produced in furnace at thermal decomposition of boric acid. The distinguished feature of the procedure is charging boric acid on a bottom of the furnace crucible before charging wastes of zinc. Weight of boric acid is calculated by formula: y=25.1(100-x), where y is weight of boric acid per 1000 kg of zinc wastes, kg, x is content of metal zinc in wastes, %. When temperature of melt of zinc wastes reaches 700-750°C, it is conditioned in the furnace for 45 min. Also, height of melt of zinc wastes in the crucible of the furnace is maintained as 800 mm. The furnace consists of a case, of lining with refractory bricks, of the crucible for melting wastes of zinc laid with refractory bricks, of gas dead-end burners positioned in chambers and communicated with the crucible of the furnace through channels in mason-work of furnace crucible, of a cover of the furnace crucible, of two notches, one of which is located at height of 80 mm from the bottom of the furnace crucible designed for casting refined melt of zinc into moulds, while the second one is located at the level of the bottom of the furnace crucible and is designed for casting melt of zinc containing inter-metallic compounds or true solutions of impurity metals in melt of zinc into moulds.

EFFECT: reduced capital and operational expenditures.

5 cl, 1 dwg, 1 ex, 2 tbl

FIELD: process engineering.

SUBSTANCE: invention relates to hydrometallurgy of metals and may be used for production of metal oxides. Proposed method comprises heating of hydroxides at the temperature of their decomposition. Note here that hydroxide heating is carried out in autoclave without evaporation of water bulk provided that pressure of hydroxide dissociation exceeds that of saturated water vapors at said temperature.

EFFECT: lower costs of dehydration.

4 dwg, 1 ex

FIELD: metallurgy.

SUBSTANCE: there are performed following stages: ore leaching at presence of hydrochloric acid with formation of soluble chloride of metal in solution for leaching, addition of sulphuric acid and/or sulphur dioxide into solution for leaching, regeneration of solid sulphate of metal or sulphate of metal from solution for leaching, regeneration of hydrochloric acid and continuous transformation of at least part of hydrochloric acid from solution into vaporous phase. Further, vaporous hydrochloric acid is absorbed and returned to the leaching stage. The sulphuric acid and/or sulphur dioxide are added to solution for leaching during process of leaching or after it. Valuable metal is usually chosen from group including Zn, Cu, Ti, Al, Cr, Ni, Co, Mn, Fe, Pb, Na, K, Ca, metals of platinum group and gold. Metal in sulphate of metal or sulphite of metal corresponds to valuable metal or less valuable metal in comparison with metal leached from ore, for example, magnesium.

EFFECT: raised efficiency of procedure.

14 cl, 27 dwg, 1 tbl

FIELD: metallurgy.

SUBSTANCE: procedure consists in leaching crumbled minerals with water solution of hydrochloric acid, in separation of solid phase and liquid phase products and in successive extraction of target components. As source minerals there are used poly-metallic slag of lead production additionally containing compounds of germanium. Leaching is performed with solution of hydrochloric acid of concentration from 6 to 30 wt % at ratio of solid and liquid phases 1:(1-5). Before separation of solid phase and liquid phase products ratio of solid and liquid phases is brought to 1: (8-20) by addition of water with transition of iron, zinc, and calcium into liquid phase product, while silicon and germanium - into solid phase product.

EFFECT: simplified extraction of target components.

3 cl, 2 ex

FIELD: metallurgy.

SUBSTANCE: method involves supply of solution with high content of cobalt, which contains cobalt, nickel and copper; sorption by means of contact of the above solution with N-(2-hydroxypropyl)picoline amino resin. Selective elution of cobalt, nickel and copper is performed after sorption by means of continuous gradient acidic elution. At that, pH of the above solution is less than or equal to 2.

EFFECT: reducing the costs and increasing the efficiency of the method.

2 cl, 1 ex

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