CN109930010B - Method for removing organic matters in zinc hydrometallurgy solution - Google Patents
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Abstract
The invention relates to a method for removing organic matters in a zinc hydrometallurgy solution, and belongs to the technical field of chemical metallurgy. Stirring the wet-process zinc smelting solution containing the organic matters, gradually cooling to-20-10 ℃, reacting for 10-60 min, forming crystal precipitates containing the organic matters by utilizing the induced nucleation effect of the organic matters, and after the reaction is finished, carrying out solid-liquid separation on the crystal precipitates containing the organic matters by adopting centrifugal filtration to obtain the zinc sulfate solution without the organic matters. The method comprises the steps of utilizing the difference of large specific surface area of macromolecular organic matters and the properties of the micromolecular organic matters and zinc sulfate solution in a cooling reactor, forming crystallization precipitation containing the organic matters through the induced nucleation effect of the organic matters, and removing the organic matters through a solid-liquid separation method to obtain qualified zinc sulfate solution. The method has the advantages of simple process, easy operation, high organic matter removal efficiency and the like.
Description
Technical Field
The invention relates to a method for removing organic matters in a zinc hydrometallurgy solution, and belongs to the technical field of chemical metallurgy.
Background
The zinc sulfate solution produced by zinc hydrometallurgy has high organic content, which can bring adverse effect to the solution purification and electrodeposition processes, and causes the harm of rising zinc powder consumption in the purification process, reducing current efficiency in the zinc electrodeposition process, increasing power consumption, exceeding standard of cathode zinc and lead, and the like. Therefore, how to remove organic matters in the zinc sulfate solution is always an important concern in the zinc hydrometallurgy industry.
The method for removing the organic matters in the solution comprises the following steps: (1) activated carbon adsorption method. The porous structure of the active carbon provides a larger surface area, has stronger adsorption capacity to organic matters, and can be activated and regenerated by steam after reaching the penetration capacity by adsorbing and removing the organic matters in the solution. (2) Air-float method. The air floatation method is to make use of the hydrophobic property of organic matters in solution to blow a great deal of micro bubbles into the solution to make the organic matters adsorbed on the micro bubbles and make the organic matters float up together by the buoyancy of the bubbles. A three-phase foam layer consisting of bubbles and hydrated organic matters is formed on the liquid surface, and the foam layer is separated from the solution body, so that the aim of removing the organic matters is fulfilled. (3) Liquid membrane filtration method. By constructing a filter membrane, the organic matter and the solution are separated by utilizing the inverse difference of different concentrations. (4) And (3) demulsifying and removing oil by ultrasonic waves. The micro oil drops in the solution vibrate with the medium under the action of ultrasonic waves, but the examples with different sizes have different vibration speeds, oil particles collide with each other, are adhered and coalesce to form large oil drops, float upwards to form floating oil, and are separated from the solution. (5) Ozone oxidation and photo-oxidation. The ozone oxidation method decomposes organic substances by utilizing the strong oxidizing property of ozone. Photo-oxidation is the decomposition of organic pollutants by using free radicals with strong oxidizing power generated by an oxidizing agent under the irradiation of light.
Patent application No. 201810707518.7 discloses a method for removing organic matters in zinc sulfate solution by wet smelting through photo-oxidation, which comprises mixing zinc sulfate solution with hydrogen peroxide uniformly, and carrying out photo-oxidation reaction under an external light source to decompose and remove the organic matters.
Patent application No. 201510456786.2 discloses a method for removing organic matters in zinc sulfate solution by using supergravity and ozone, which comprises heating zinc sulfate solution, adding oxygen, atomizing, and allowing the atomized zinc sulfate solution to react with ozone sufficiently in supergravity issuing equipment. And then keeping the circulation of the oxygen and the solution of the super-gravity field generator to obtain the qualified zinc sulfate solution with the organic matters removed.
Although the method can remove the organic matters in the zinc sulfate solution, the method mainly removes the soluble organic matters with smaller molecular weight, and has the defects of poor removal effect, complex operation, large equipment investment and the like on the organic matters with large molecular weight, such as bone glue, gelatin, bovine glue and the like. Therefore, the development of a new method for removing organic matters from a zinc sulfate solution with high efficiency and simplicity is still a technical problem to be further solved in the zinc hydrometallurgy industry.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a method for removing organic matters in a zinc sulfate solution. The method comprises the steps of utilizing the difference of large specific surface area of macromolecular organic matters and the properties of the micromolecular organic matters and zinc sulfate solution in a cooling reactor, forming crystallization precipitation containing the organic matters through the induced nucleation effect of the organic matters, and removing the organic matters through a solid-liquid separation method to obtain qualified zinc sulfate solution. The method has the advantages of simple process, easy operation, high organic matter removal efficiency and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for removing organic matters in a wet-process zinc smelting solution comprises the steps of stirring the wet-process zinc smelting solution containing the organic matters, gradually cooling to-20-10 ℃, reacting for 10-60 min, forming crystal precipitates containing the organic matters by utilizing the organic matter induced nucleation, and after the reaction is finished, carrying out centrifugal filtration liquid-solid separation on the crystal precipitates containing the organic matters to obtain the zinc sulfate solution without the organic matters.
The organic matter-containing zinc hydrometallurgy solution is produced by zinc hydrometallurgy, wherein the concentration of zinc is 40-155 g/L, and the concentration of sulfuric acid in the solution is 0.01-180 g/L.
The organic matters in the wet zinc smelting solution containing the organic matters are calculated by total organic carbon, and the total organic carbon is more than 35 mg/L.
The temperature of the wet-process zinc smelting solution containing the organic matters is 35-65 ℃.
The stirring speed is 10-120 r/min.
The specific process of gradually cooling is as follows: the temperature is reduced to 25-30 ℃ at a cooling speed of 1-2 ℃/min at the beginning, and then the temperature is reduced to-20-10 ℃ at a cooling speed of 2-5 ℃/min.
The invention has the beneficial effects that: the method adopts a cooling reactor, utilizes the difference of large specific surface area of macromolecular organic matters and the property of the micromolecular organic matters and the zinc sulfate solution, forms crystal sediment containing the organic matters through the induced nucleation of the organic matters, and removes the crystal sediment containing the organic matters under the condition of rapid liquid-solid separation to obtain the qualified zinc sulfate solution. The method does not need to add chemical reagents, and has the advantages of simple process, easy operation and high organic matter removal efficiency.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The method for removing the organic matters in the wet-process zinc smelting solution comprises the steps of putting 1000mL of wet-process zinc smelting solution containing the organic matters (waste electrolyte with the temperature of 38 ℃ produced by wet-process zinc smelting of the wet-process zinc smelting solution containing the organic matters, the zinc concentration of 40g/L and the sulfuric acid concentration of 180 g/L), wherein the organic matters in the wet-process zinc smelting solution containing the organic matters are calculated according to the total organic carbon, the total organic carbon is 95.3mg/L, the organic matters comprise macromolecular organic matters such as bone glue and mineral oil and micromolecular organic matters such as ethyl xanthate and fatty acid, stirring in a cooling reactor (120 revolutions per minute), gradually cooling to-20 ℃, and the specific process comprises the following steps: the temperature is reduced to 25 ℃ at the cooling speed of 1 ℃/min at the beginning, then the temperature is reduced to-20 ℃ at the cooling speed of 2 ℃/min continuously, the reaction is carried out for 10min, the crystallization precipitation containing the organic matters is formed by utilizing the induced nucleation of the organic matters, and after the reaction is finished, the crystallization precipitation containing the organic matters is separated by adopting centrifugal filtration liquid-solid separation, and 982mL of zinc sulfate solution with the organic matters removed is obtained.
The detection result shows that the total organic carbon content in the zinc sulfate solution for removing the organic matters is 18.5mg/L, and the removal rate of the organic matters is 80.9 percent.
Example 2
The method for removing the organic matters in the wet-process zinc smelting solution comprises the steps of putting 1000mL of wet-process zinc smelting solution containing the organic matters (the wet-process zinc smelting solution containing the organic matters is waste electrolyte with the temperature of 37 ℃ produced by wet-process zinc smelting, the concentration of zinc is 46g/L, the concentration of sulfuric acid is 165g/L, the total organic carbon of the organic matters in the wet-process zinc smelting solution containing the organic matters is 89.1mg/L calculated according to the total organic carbon, the types of the organic matters comprise macromolecular organic matters such as gelatin and lubricating oil, and micromolecular organic matters such as ethylxanthate, fatty acid and the like into a cooling reactor for stirring (80 revolutions per minute), gradually cooling to-10 ℃, and carrying out the specific process that the temperature is reduced to 25 ℃ at the cooling speed of 1 ℃/min at the beginning, then the temperature is reduced to-10 ℃ at the cooling speed of 3 ℃/min for reaction for 30min, and forming, after the reaction is finished, the solution is subjected to liquid-solid separation by centrifugal filtration to obtain 975mL of zinc sulfate solution from which the organic matters are removed after crystallization and precipitation.
The detection result shows that the total organic carbon content in the zinc sulfate solution for removing the organic matters is 22.0mg/L, and the removal rate of the organic matters is 75.9 percent.
Example 3
The method for removing the organic matters in the wet-process zinc smelting solution comprises the steps of carrying out wet-process zinc smelting on 1000mL of organic matters (the wet-process zinc smelting solution containing the organic matters is a zinc-hydrometallurgy electrolysis front liquid with the temperature of 35 ℃, the zinc concentration is 52g/L, the sulfuric acid concentration is 153g/L, the organic matters in the wet-process zinc smelting solution containing the organic matters are calculated according to the total organic carbon, the total organic carbon is 58.6mg/L, and the organic matters comprise macromolecular organic matters such as gelatin and the like and micromolecular organic matters such as ethyl xanthate, fatty acid and the like). Stirring in a cooling reactor (50 rpm), gradually cooling to-5 ℃, and the specific process is as follows: the temperature is reduced to 25 ℃ at the cooling speed of 2 ℃/min at the beginning, then the temperature is reduced to-5 ℃ at the cooling speed of 5 ℃/min continuously, the reaction is carried out for 30min, the crystallization precipitation containing the organic matters is formed by utilizing the organic matter induced nucleation, after the reaction is finished, the crystallization precipitation containing the organic matters is separated by adopting centrifugal filtration liquid-solid separation, and 962mL of zinc sulfate solution with the organic matters removed is obtained.
The detection result shows that the total organic carbon content in the zinc sulfate solution for removing the organic matters is 20.6mg/L, and the removal rate of the organic matters is 62.9 percent.
Example 4
The method for removing the organic matters in the wet-process zinc smelting solution comprises the steps of putting 1000mL of wet-process zinc smelting solution containing the organic matters (the wet-process zinc smelting solution containing the organic matters is a three-stage purified solution of wet-process zinc smelting, the temperature is 65 ℃, the zinc concentration is 155g/L, the solution acidity is 5.4, the organic matters in the wet-process zinc smelting solution containing the organic matters are calculated according to the total organic carbon, the total organic carbon is 35.2mg/L, the organic matters comprise macromolecular organic matters such as bone glue and mineral oil and micromolecular organic matters such as ethyl xanthate and fatty acid) into a cooling reactor for stirring (10 r/min), and gradually cooling to 10 ℃, wherein the specific process comprises the following steps: the temperature is reduced to 30 ℃ at the cooling speed of 2 ℃/min at the beginning, then the temperature is reduced to 10 ℃ at the cooling speed of 2 ℃/min continuously, the reaction is carried out for 60min, the crystallization precipitation containing the organic matters is formed by utilizing the organic matter induced nucleation, after the reaction is finished, the crystallization precipitation containing the organic matters is separated by adopting centrifugal filtration liquid-solid separation, and then 945mL zinc sulfate solution with the organic matters removed is obtained.
The detection result shows that the total organic carbon content in the zinc sulfate solution for removing the organic matters is 21.9mg/L, and the removal rate of the organic matters is 41.2 percent.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (5)
1. A method for removing organic matters in a zinc hydrometallurgy solution is characterized by comprising the following steps: stirring the wet-process zinc smelting solution containing the organic matters, gradually cooling to-20-10 ℃, reacting for 10-60 min, forming crystal precipitates containing the organic matters by utilizing the induced nucleation effect of the organic matters, and after the reaction is finished, carrying out solid-liquid separation on the crystal precipitates containing the organic matters by adopting centrifugal filtration to obtain a zinc sulfate solution without the organic matters;
the specific process of gradually cooling is as follows: the temperature is reduced to 25-30 ℃ at a cooling speed of 1-2 ℃/min at the beginning, and then the temperature is reduced to-20-10 ℃ at a cooling speed of 2-5 ℃/min.
2. The method for removing organic matters from a zinc hydrometallurgy solution according to claim 1, wherein: the organic matter-containing zinc hydrometallurgy solution is produced by zinc hydrometallurgy, wherein the concentration of zinc is 40-155 g/L, and the concentration of sulfuric acid in the solution is 0.01-180 g/L.
3. The method for removing organic matters from a zinc hydrometallurgy solution according to claim 1, wherein: the organic matters in the wet zinc smelting solution containing the organic matters are calculated by total organic carbon, and the total organic carbon is more than 35 mg/L.
4. The method for removing organic matters from a zinc hydrometallurgy solution according to claim 1, wherein: the temperature of the wet-process zinc smelting solution containing the organic matters is 35-65 ℃.
5. The method for removing organic matters from a zinc hydrometallurgy solution according to claim 1, wherein: the stirring speed is 10-120 r/min.
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| CN112030003B (en) * | 2020-03-27 | 2021-09-07 | 昆明理工大学 | Method for simultaneously removing multiple impurity ions in wet-process zinc smelting waste electrolyte |
| CN111996390A (en) * | 2020-08-12 | 2020-11-27 | 云南驰宏锌锗股份有限公司 | Method for removing fine particles from zinc sulfate solution |
| CN113667833A (en) * | 2021-08-20 | 2021-11-19 | 云南金鼎锌业有限公司 | Purification and cadmium removal method for zinc hydrometallurgy |
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