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A kind of preparation method of the composite fluoride removal material applied to the electrolytic zinc sulfate solution to remove fluorine

A technology of zinc sulfate solution and sulfuric acid solution, which is applied in the direction of electrolysis process, electrolysis components, chemical instruments and methods, etc., and can solve the problems of precipitation and redissolution, increase of antimony content in solution, increase of fluorine concentration, etc.

Inactive Publication Date: 2016-05-25
CENT SOUTH UNIV
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Problems solved by technology

However, there is a problem that the fluoride ion content in the zinc sulfate solution is too high in the hydrometallurgy zinc smelting process. Excessive fluoride ions in the zinc electrodeposition process will cause corrosion of the cathode aluminum plate, causing the electrodeposited zinc to stick to the aluminum plate and be difficult to peel off. At the same time, the aluminum plate cannot be used repeatedly, and these problems hinder the continuous production
In order to make the cathode plate easy to peel off, some people use the method of adding antimony potassium tartrate, but this method will easily cause the antimony content of the solution to increase, which will cause precipitation and remelting or even burn the plate
Therefore, the high fluorine content has caused many adverse effects on the production process, and these adverse effects are difficult to overcome
[0003] At present, the commonly used method for excessive fluorine content in zinc hydrometallurgy is: multi-hearth furnace roasting, but this method consumes high energy, causes great environmental pollution, and the effect is not obvious; in addition, there are goethite method and calcium carbonate defluoridation, However, these methods cannot meet the requirements of the open circuit of fluorine in the system, resulting in a further increase in the concentration of fluorine; in addition, there is a vacuum evaporation method to volatilize the fluorine in the electrolytic zinc solution; the extraction agent TBP removes the fluorine in the zinc sulfate solution; silica gel is used as the adsorbent to remove the electrolytic zinc Fluorine in solution; using Fe 2 o 3 Wait for the oxide to adsorb fluorine in the zinc sulfate solution; make the solution generate K 2 SiF 6 Precipitation to remove fluorine in zinc sulfate solution, etc., these methods have their own shortcomings, such as difficult technical operation, high production cost, etc.
[0004] And because there is too much sulfate ion in the zinc sulfate liquid, the sulfate ion has a great influence on the defluoridation, so that the defluoridation material originally suitable for water treatment has basically no effect in the zinc sulfate liquid
[0005] In summary, the existence of fluoride ions in zinc sulfate solution has a great adverse effect on zinc hydrometallurgy, and the existing methods cannot effectively remove it, so it is urgent to use new technologies or better adsorption materials to remove it. break the bottleneck

Method used

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  • A kind of preparation method of the composite fluoride removal material applied to the electrolytic zinc sulfate solution to remove fluorine

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) After the bamboo charcoal is crushed, 2kg of 100-120 mesh bamboo charcoal is sieved, heated to 400°C in an air furnace, and kept for 8 hours;

[0028] (2) Take 1L of sulfuric acid to treat the heat-treated bamboo charcoal according to the solid-to-liquid ratio of 2kg / L. The treatment temperature is 80°C, then wash with a large amount of deionized water until the pH is close to 7, and dry at 60°C after filtration for 24 hours;

[0029] (3) Prepare 1 L of aluminum sulfate solution with a concentration of 2 mol / L, add pretreated bamboo charcoal, and soak for 10 h at a temperature of 50°C. Bamboo charcoal was dried in an oven at 120°C for 12 hours after impregnation;

[0030] (4) Further use 1 L concentration of 20% by mass sodium hydroxide solution for impregnation treatment, stir evenly and let it stand for 24 hours, wash with a large amount of deionized water until the liquid is clarified, filter, and dry at 70°C for 24 hours to obtain the aluminum-loaded bamboo char...

Embodiment 2

[0033] (1) After the bamboo charcoal is crushed, take 2kg of 150-200 mesh bamboo charcoal, heat it to 400°C in an air furnace, and keep it warm for 5 hours;

[0034] (2) Take 2L of sulfuric acid to treat the heat-treated bamboo charcoal at a solid-to-liquid ratio of 1kg / L. The treatment temperature is 80°C, then wash with a large amount of deionized water until the pH is close to 7, and dry at 60°C after filtration for 24 hours;

[0035] (3) Prepare 1 L of aluminum sulfate solution with a concentration of 2 mol / L, add pretreated bamboo charcoal, and soak for 10 hours at a temperature of 50 degrees Celsius. Bamboo charcoal was dried in an oven at 120°C for 12 hours after impregnation;

[0036] (4) Further use 1 L concentration of 20% by mass sodium hydroxide solution for impregnation treatment, stir evenly and let it stand for 24 hours, wash with a large amount of deionized water until the liquid is clarified, filter, and dry at 70°C for 24 hours to obtain the aluminum-loaded b...

Embodiment 3

[0039] (1) After the bamboo charcoal is broken, sieve 2kg of 100-120 mesh bamboo charcoal, heat it to 400°C in an air furnace, and keep it warm for 3 hours;

[0040] (2) Take 1L of sulfuric acid to treat the heat-treated bamboo charcoal according to the solid-to-liquid ratio of 2kg / L. The treatment temperature is 80°C, then wash with a large amount of deionized water until the pH is close to 7, and dry at 60°C after filtration for 24 hours;

[0041] (3) Prepare 1 L of aluminum sulfate solution with a concentration of 2 mol / L, add pretreated bamboo charcoal, and soak for 8 hours at a temperature of 45 degrees Celsius. Bamboo charcoal was dried in an oven at 120°C for 12 hours after impregnation;

[0042] (4) Further use 1 L concentration of 20% by mass sodium hydroxide solution for impregnation treatment, stir evenly and let stand for 24 hours, wash with a large amount of deionized water until the liquid is clarified, filter, and dry at 70° C. for 24 hours to obtain bamboo char...

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Abstract

The invention relates to a preparation method of a composite defluorination material used in an electrolytic zinc sulphate solution. Particularly, the method is as below: pretreating bamboo charcoal by high temperature heating and sulfuric acid soaking; impregnating the treated bamboo charcoal with metal salt solution; and drying and treating with alkali to precipitate the metal salt in pores of the bamboo charcoal material. The preparation method is simple and low-cost; the prepared composite defluorination material loaded with metal salt can be used in defluorination of electrolytic zinc sulfate solution, has strong selective adsorption, high defluorination capacity, good and stable defluorination effect; after defluorination, the composite defluorination material can be effectively separated from the electrolytic zinc sulfate solution, and be reused after regeneration. The method is convenient for application and applicable to industrialized production.

Description

technical field [0001] The invention relates to a preparation method of an electrolytic zinc sulfate solution defluorination material in zinc hydrometallurgy, in particular to a preparation method of a composite defluorination material applied to electrolytic zinc sulfate solution defluorination. Background technique [0002] With the rapid development of social economy, the demand for raw materials is becoming more and more urgent. As a major zinc producer in the world, my country occupies a dominant position in zinc production, and the requirements for safe and efficient zinc production technology are self-evident. At present, the main production technology of zinc is zinc hydrometallurgy, and its main advantages are environmental friendliness, high recovery rate and low cost. However, there is a problem that the fluoride ion content in the zinc sulfate solution is too high in the hydrometallurgy zinc smelting process. Excessive fluoride ions in the zinc electrodeposition...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01J20/30B01D15/08C25C1/16C25C7/06
CPCB01D15/08B01J20/20B01J20/30B01J2220/4806C25C1/16C25C7/06Y02P10/20
Inventor 杜柯张亮胡国荣彭忠东曹雁冰华传山
Owner CENT SOUTH UNIV
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