Method of processing zinc and germanium containing solid phase polymetallic mineral material

FIELD: metallurgy.

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

EFFECT: increased degree of germanium and zinc extraction.

4 cl, 2 ex

 

The invention relates to the field of metallurgy of non-ferrous metals, and in particular to methods of hydrometallurgical processing of zinc - and germanium-containing solid phase polymetallic mineral materials with the purpose of allocation of them germanium and zinc.

At present, the urgent task is the development of technological processes for extraction of valuable man-made elements, such as germanium and zinc from low-grade ores, as well as from secondary products pyrometallurgical production of non-ferrous metals (toxins, dust, and other wastes pyrometallurgical production).

As mentioned above, the initial products are difficultly soluble solid materials containing germanium and zinc in the form of a range of chemical compounds, as well as many other related chemical elements and compounds, it is necessary to develop a special multi-stage methods of selective extraction of zinc and Germany, the main purpose of which is to increase the degree of extraction.

A method of refining slag copper production with the aim of obtaining them from Germany and zinc [Angelican, Bggarden. Metallurgy of rare metals. M., 1991, 258], which includes blowing through rasplavlennyi slag coal dust from the air (the capacity of fuming process), in which Germanii zinc are extracted in the form of oxides and concentrated in action.

This method is characterised by a high degree of extraction of target components, however, it requires high energy costs.

More economical from the point of view of energy costs are hydrometallurgical processing methods above source materials in order to obtain the desired products, in particular Germany and zinc, including the dissolution of the extracted component in the leachate selectively applicable reagent, if possible without affecting the other components of the feedstock.

Thus, in particular, a method of refining copper dust production with the purpose of allocation of the specified material is germanium and zinc [Izv. Non-ferrous metallurgy, No. 3, 2006, s.43], selected by the authors as the nearest equivalent.

According to this method is carried out leaching of the source material with a solution of sulfuric acid of a concentration of 0.2 mol/DM3when the ratio of the solid and liquid phases of 1:3, and then the resulting slurry is used for the selective extraction of germanium and zinc.

This method extracts the 65-85% Germany and 75-85% of zinc, which is not high enough, high indicator.

The task of the invention is to provide a method of processing solid-phase polymetallic mineral material on specialsee the extraction of germanium and zinc to enhance retrieval.

The invention consists in that in the method of processing zinc and germanium-containing solid phase polymetallic mineral material comprising leaching the material with an aqueous solution of a chemical reagent at a certain ratio of solid and liquid phases and the subsequent processing of the pulp with the aim of obtaining products used to allocate Germany and zinc, according to the invention in the process of leaching the material to have a mechanical attrition and dezintegriruetsja effects as a chemical reagent use a solution comprising an oxidizing agent in an amount of from 1.8 to 2.5 kg per 1 kg of Germany contained in the composition of the material, and the alkali metal hydroxide in an amount to provide a pH environment from 12 to 14, the process of leaching is carried out at a ratio of solid and liquid phases 1:(3-8), then perform the sorption precipitation of Germany from the obtained slurry by passing through the ion exchange resin when added to a slurry of alkali in an amount to provide a pH environment of 13.5-14, and water in an amount to provide a ratio of the solid and liquid phases 1:(5-8), obtained after sorption deposition Germany product is treated in an autoclave at a temperature of 120-250°and the pressure 6-40 ATM, followed by the separation of the liquid phase, which is used for the ejecta is it zinc and germanium elute from the ion exchange resin and use the resulting eluate to highlight Germany from it.

In the particular case of carrying out the invention germanium elute 1,1-5,0 N. hydrochloric acid and the resulting eluate produce germanium as germanium dioxide by heating the eluate to a temperature of not more than 90°, separation of the gas phase, washing it in the column for carrying out hydrolysis and drying of the precipitated sludge.

As a result of experimental studies by the authors of the claimed invention was developed multistage process of processing various types of polymetallic mineral materials, providing a selection of them germanium and zinc to enhance retrieval.

According to the proposed method the leaching process of starting material chemical reagent is carried out in conditions providing dezintegriruetsja and abrasive effect on the material being processed, resulting in the development and activation of the surface of its particles, and a quick update of the contact surface of the liquid and solid phases, which contributes to the intensification occurring during leaching of chemical reactions.

Selected by the authors for leaching as a chemical reagent solution comprising an oxidizing agent in an amount of from 1.8 to 2.5 kg per 1 kg of Germany, containing the gosia in the composition of the material, and the alkali metal hydroxide in an amount to provide a pH environment from 12 to 14, and the ratio of solid and liquid phases, is equal to 1:(3-8), which is in the process of leaching, determine the course of chemical processes, providing at this stage is extremely high degree of extraction of germanium in the form of water-soluble compounds of Germany, formed in the leaching process and output at this stage in the liquid phase.

Selected conditions the leaching also provide extraction from the source material, a significant part of the zinc in the form of its water-soluble compounds.

As shown by the results of the tests, the leaching of the source material in compliance with the totality of the above conditions provides already at this stage of the process of selective extraction into the liquid phase before (97-99)% in Germany and 60% zinc.

Dezintegriruetsja and abrasive effect on the treated material during leaching can be achieved, in particular, by conducting the process in a planetary mill.

As part of the chemical oxidant may be used, in particular, sodium hypochlorite, hydrogen peroxide.

Welcome sorption deposition Germany resulting from the leaching process of the pulp by her about what Askania through ion-exchange resin allows you to selectively separate the compounds of germanium from other components of the pulp. This process conditions the sorption deposition Germany, namely the value of pH of 13.5-14 and the ratio of solid and liquid phases 1:(5-8), selected by the authors experimentally and are optimal from the point of view of completeness sorption Germany on the surface of the ion-exchange resin. These values of pH and the ratio of solid and liquid phases is provided by adding to the pulp of the necessary amounts, respectively, of alkali metal hydroxide and water.

For sorption deposition Germany can be used in a variety of ion-exchange resin capable of selectively adsorb germanium, in particular ion exchange resin is a weakly basic type with a secondary or tertiary amine active functional groups, macroporous polystyrene chelate weakly basic anion exchange resin, and others.

When the autoclave is received after sorption deposition Germany product, which is passed through an ion-exchange resin mixture is dissolved in the leaching of solid particles and the liquid phase, the process of hydrothermal allocation remaining in the solid phase composition of zinc in a liquid phase. Modes of autoclave processing of the specified product, namely the temperature of 120-250°and pressure 6-40 ATM chosen by the authors experimentally and are protected areas the normal from the point of view of completeness and selectivity excretion of zinc in a liquid phase.

The Department specified the liquid phase from the solid phase products, for example, by filtering allows to obtain a liquid product containing the extracted at the previous stages of the process the zinc and continue to use this product for separation of zinc in various known ways.

The extraction of the ion-exchange resin Germany carried by leaching from the surface of the ion-exchange resin with a solution of chemicals, providing desorption Germany, and further isolated germanium obtained from the eluate of various known methods.

The target product in the process of separating zinc according to the claimed method may be zinc oxide, which is obtained by carbonization separated after autoclave treatment product liquid phase, separating precipitated sludge, the process of decarbonization precipitated product and drying.

The target product in the process of allocation of Germany according to the claimed method may be Germany dioxide, which is obtained by desorption Germany from the surface of the ion-exchange resin with alkali solution with a concentration of from 5 to 30 wt.%, acidification of the resulting eluate to a pH of 6.5-7.5, the Department dropped the precipitate and drying.

Dioxide Germany as the target product can be obtained by desorption Germany from the surface of incommen the second resin 1,1-5,0 N. solution of hydrochloric acid, heating the resulting eluate to a temperature of not more than 90°, separation of the gas phase, washing the obtained gas-phase product in the column and drying of the precipitated sludge.

The method is as follows.

The original zinc - and germanium-containing solid phase polymetallic mineral material subjected to leaching under conditions providing mechanical attrition and dezintegriruetsja effect on the material. The process, in particular, is carried out in a planetary mill, which serves lump or powdered source material, and an aqueous solution including the oxidant in an amount of from 1.8 to 2.5 kg per 1 kg of Germany contained in the composition of the material, and the alkali metal hydroxide in an amount to provide a pH environment from 12 to 14. In the mill on the material affected by high dynamic loads (>20 G)with heating of the reaction mass up to 70-95°and crushing, grinding and abrasion of the processed material, as a result he goes in fine condition (degree of dispersion of the order of 10-40 μm). The leaching process is carried out at a ratio of solid and liquid phases 1:(3-8), that is, the estimated amount of water in solution. During the leaching process is from 5 minutes to 4 hours.

The pulp obtained n the stage of leaching, passed through ion-exchange resin in order sorption deposition Germany, for example through the cassette with ion exchange resin, is installed in the reactor. The process is carried out by adding to the pulp alkali in an amount to provide a pH environment of 13.5-14, and water in an amount to provide a ratio of the solid and liquid phases 1:(5-8). When this slurry is passed through a cartridge in the mode of counter-current relative to the flow of an aqueous solution of alkali.

Received after sorption deposition Germany product is fed into the autoclave, where it is held hydrothermal treatment at a temperature of 120-250°and the pressure 6-40 psi for 40 min - 4 h received after autoclave treatment product is separated liquid phase, for example, by vacuum filtration. The liquid phase used for separation of zinc from it.

Germanium elute from the ion exchange resin and use the resulting eluate to highlight Germany from it.

The possibility of the method shown in the examples of specific performance.

Example 1.

As source material used conveyor polymetallic lead slag production, containing according to mass spectral analysis 5 wt.% zinc and 0.04 wt.% Germany.

In the planetary mill downloaded the original slag in the amount of 100 kg was applied an aqueous solution containing 10 g/l of hypochlorite is the atrium, in the amount determined at the rate of 2 kg of sodium hypochlorite for 1 kg of Germany contained in the composition of the slag. In the planetary mill was also downloaded sodium hydroxide in an amount to provide a pH environment of 13.5. The ratio of solid and liquid phases in the reaction medium was 1:4. During the leaching process was about 50 minutes

The pulp obtained in the leaching step, was sent into the reactor by passing it through a set in the reactor cassette with macroporous weakly basic polystyrene anion exchange resin brand D403, when it comes to the slurry was added sodium hydroxide in an amount to provide a pH environment is equal to 14, and water in an amount to provide a ratio of the solid and liquid phases of 1:6. The slurry was passed through a cartridge in the countercurrent mode with respect to aqueous alkali solution.

Received after sorption deposition Germany product was applied to the autoclave, where it was held by hydrothermal treatment at a temperature of 220°and a pressure of 30 psi for 2 hours. Received after autoclave treatment product was separated liquid phase by vacuum filtration.

The filtered liquid phase is sent to a two-column carbonization working in the froth regime. As carbonizing agent used carbon dioxide. As a result of carbonization received Zn(OH)sub> 2CO3, which was subjected to decarbonization by heating up to 300°and obtained as the final product is zinc oxide. The output of zinc in relation to its content in the original slag was of 99.97%.

To extract the precipitated resin Germany cassette with anion exchange resin was soaked in a 20% sodium hydroxide solution, and then washed the cartridge with water. The obtained eluate was acidified to pH=7, while in the sediment fell dowolny dioxide, Germany. The precipitate was filtered, was carried out by drying and calcination at t=300°C.

The quality of the final product was obtained dioxide, Germany. The output of Germany in relation to its content in the original slag was 99.95%.

Example 2.

Used the same raw material as in example 1.

In the planetary mill downloaded the original slag and filed an aqueous solution containing 30% hydrogen peroxide solution in an amount determined based 2.4 kg of hydrogen peroxide per 1 kg of Germany, in the composition of the slag. In the planetary mill was also downloaded sodium hydroxide in an amount to provide a pH environment of 13.8. The ratio of solid and liquid phases in the reaction medium was 1:5. During the leaching process was 30 minutes

The pulp obtained in the leaching step, was sent into the reactor by passing it through a set is left in the reactor cassette with macroporous weakly basic polystyrene anion exchange resin brand D403, to the slurry was added sodium hydroxide in an amount to provide a pH environment is equal to 14, and water in an amount to provide a ratio of the solid and liquid phases of 1:6. The slurry was passed through a cartridge in the countercurrent mode with respect to aqueous alkali solution.

Received after sorption deposition Germany product was applied to the autoclave, where it was held by hydrothermal treatment at a temperature of 220°and a pressure of 30 psi for 2 hours. Received after autoclave treatment product was separated liquid phase by vacuum filtration.

The filtered liquid phase is sent to a two-column carbonization working in the froth regime. As carbonizing agent used carbon dioxide. As a result of carbonization received Zn(OH)2CO3, which was subjected to decarbonization by heating up to 300°and obtained as the final product is zinc oxide. The output of zinc in relation to its content in the original slag was 99,90%.

To extract the precipitated resin Germany cassette with anion exchange resin was soaked in 1.5 N. hydrochloric acid, and then washed the cartridge with water. The obtained eluate was heated to a temperature of 85-90°C, resulting in the tetrachloride Germany was allocated in the form of gas, which is sent to a column for carrying out the process of the Hydra is Lisa with subsequent separation of the precipitated precipitate and drying.

As of the end product received dioxide, Germany. The output of Germany in relation to its content in the original slag was of 99.97%.

1. A method of processing zinc and germanium-containing solid phase polymetallic mineral material comprising leaching the material with an aqueous solution of the chemical reagent and the subsequent processing of the obtained slurry for separation of germanium and zinc, wherein the leaching is carried out with mechanical, abrasive and dezintegriraat the impact of using the solution of the chemical reagent solution containing an oxidizing agent in an amount of from 1.8 to 2.5 kg per 1 kg of Germany contained in the original material, and the alkali metal hydroxide in an amount to provide a pH environment from 12 to 14, when the ratio of the solid and liquid phases 1:(3-8), from the obtained pulp perform sorption deposition Germany by passing it through an ion-exchange resin when added to a slurry of alkali in an amount to provide a pH environment of 13.5-14, and water in an amount to provide a ratio of the solid and liquid phases 1:(5-8), obtained after sorption deposition Germany product is treated in an autoclave at a temperature of 120-250°and the pressure 6-40 ATM and separate the liquid phase from which secrete zinc, and ion-exchange resin elute germanium and from the obtained eluate in the really germanium.

2. The method according to claim 1, characterized in that the zinc is isolated in the form of zinc oxide by carbonization of the liquid phase and separating precipitated sludge, its decarbonisation and drying.

3. The method according to claim 1, characterized in that the germanium elute with alkali solution with a concentration of from 5 to 30 wt.% and separated from the eluate germanium as germanium dioxide by acidification of the eluate to a pH of 6.5-7.5, the Department dropped the precipitate and drying.

4. The method according to claim 1, characterized in that the germanium elute 1,1-5,0 N. hydrochloric acid and the resulting eluate produce germanium as germanium dioxide by heating the eluate to a temperature of not more than 90°, separation of the gas phase, washing it in the column for carrying out hydrolysis and drying of the precipitated sludge.



 

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3 cl, 6 tbl, 5 ex

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1 tbl, 7 ex

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