A kind of preparation method of complex precipitant and method for electrolyte purification

Abstract

The invention provides a complexation-precipitation agent preparation method. The complexation-precipitation agent preparation method comprises the following steps of 1, making a sulfuric acid solution and barium chloride react with lead sulfate, so that a first reaction solution is obtained; 2, making the first reaction solution react with antimony trioxide, then conducting vacuum suction filtration for the first time, mixing obtained filter residues with water, adjusting pH for the first time, then conducting vacuum suction filtration for the second time, mixing obtained filter residues with water once again, adjusting pH for the second time, and then conducting vacuum suction filtration for the third time; and 3, mixing filter residues obtained in step 2 with a sulfuric acid solution, and after a reaction is completed, conducting vacuum suction filtration for the fourth time, so that a complexation-precipitation agent is obtained. The invention further provides a copper electrolyte purification method. The complexation-precipitation agent prepared through the method is actually a combination of a complexation agent and a precipitation agent, and therefore arsenic, antimony and bismuth in a copper electrolyte can be removed at the same time; and the arsenic purification rate and the bismuth purification rate are high.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a preparation method of a complex precipitation agent and a method for purifying an electrolyte. Background technique [0002] During the copper electrolytic refining process, harmful impurities As, Sb, and Bi gradually accumulate in the electrolyte. When the content of As, Sb, and Bi in the electrolyte accumulates to a certain concentration, floating anode slime may be formed and mechanically adhered to the surface of the cathode. , What's more, it is discharged and precipitated on the cathode, which seriously affects the quality of cathode copper. Therefore, in order to maintain the stability of the electrolyte composition, ensure the normal progress of electrolysis and the quality of cathode copper, it is necessary to regularly purify the electrolyte. [0003] At present, the most widely used method of copper electrolyte purification process is the induced decopper an...

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Problems solved by technology

[0003] At present, the most widely used method of copper electrolyte purification process is the induced decopper and arsenic electrodeposition method, which was invented by Sumitomo Metal Mining Co., Ltd. It has been significantly improved, but it cannot fundamentally solve the defects of this process method, such as the use of insoluble anode electrowinning, which consumes a lot of electric energy; black copper powder and sponge copper need further processing, the processing cost increases, and arsine hydrogen is inevitably produced toxic gas

[0004] There are also solvent extraction methods for electrolyte purification. Although solvent extraction has high efficiency, good environment, and continuous operation, it has not found an extraction agent that can extract arsenic, antimony, and bismuth at the same time, which has become the biggest limitation for the development of extraction methods; electrolysis There are also ion exchange methods for liquid purification. The ion exchange method can reduce the impurities in the electrolyte to a certain concentration without changing other components. The process is simple, but the inherent defects of ion exchange are still inevitable, such as small exchange capacity and large amount of waste water. , not suitable for industrial production; there are also chemical precipitation methods for electrolyte purification, that is, adding a precipitant to the copper electrolyte to precipitate impurities, such as sulfate precipitation, lime-iron salt precipitation, sulfide precipitation, and seed crystal precipitation Chemical precipitation method can effectively precipitate impurities, but the precipitated arsenic-containing substances cannot be processed, and most of them are landfilled, causing economic losses and polluting the environment; there are also adsorption methods for electrolyte purification. , that is, using activated carbon, activated aluminum, hematite, wollastonite, etc. as adsorbents, but the adsorption effect is not good, and the adsorption products are difficult to handle

[0005] At present, the electrolyte purification technology that has been studied more is self-purification technology, which includes arsenic-added self-purification technology, antimony-added self-purification technology and bismuth-added self-purification technology; among them, arsenic-added self-purification technology is to add copper arsenate to the electrolyte solution, copper arsenite solution, arsenic acid solution, arsenous acid solution and other high-arsenic solutions, maintain the concentration of As in the electrolyte at 10-15g / L, and control the mass ratio of As to electrolyte (Sb+Bi) at 1.3-2.2 In between, impurities As, Sb, and Bi form supersaturated crystalline substances to precipitate out. This process makes the concentration of arsenic in the electrolyte at a high limit, and the surface particles at the bottom of the cathode copper increase significantly, which affects the quality of the cathode copper, and the content of impurities sinking into the anode slime increases. , which has a great impact on the anode slime treatment in the later stage; antimony self-purification technology is to control the antimony concentration in the electrolyte at 1.2g / L, so that antimony and bismuth self-purify and precipitate, or add antimony-containing substances to the electrolyte for adsorption , but it cannot adsorb arsenic, antimony and bismuth impurities at the same time and the adsorption effect is not ideal; bismuth-added self-purification technology is to add basic bismuth sulfate or bismuth oxide to the electrolyte to form a white precipitate to remove arsenic, antimony, and bismuth in the electrolyte Bismuth impurities, the self-purification effect is not significant, and it is easy to cause the remelting of bismuth, increasing the concentration of bismuth in the electrolyte

Although people have done a lot of attempts and research on self-purification, none of them can achieve the desired effect. At the same time, these self-purification mechanisms have certain defects, and no unified conclusion has been formed, so that the self-purification technology cannot be applied in industry.

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