CN115652096A - Recycling method of zinc smelting cathode aluminum plate brush plate aluminum powder slag - Google Patents
Recycling method of zinc smelting cathode aluminum plate brush plate aluminum powder slag Download PDFInfo
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- CN115652096A CN115652096A CN202211415845.8A CN202211415845A CN115652096A CN 115652096 A CN115652096 A CN 115652096A CN 202211415845 A CN202211415845 A CN 202211415845A CN 115652096 A CN115652096 A CN 115652096A
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Abstract
The invention belongs to the technical field of nonferrous metallurgy processes, and particularly relates to a method for recycling aluminum powder slag of a zinc smelting cathode aluminum plate brush plate, which comprises the following steps: adding aluminum powder slag of a brush plate of a zinc smelting cathode aluminum plate into zinc electrolysis waste liquid to form mixed liquid; adding the mixed solution into a zinc smelting neutral leaching procedure for neutral leaching; forming complex precipitate along with the increase of PH value in the neutral leaching process, and performing acid leaching along with the middle leaching bottom flow; adding heavy calcium powder to adjust the pH value of acid leaching underflow in a flotation process, placing acid leaching slag in a multi-hearth furnace, introducing oxygen and coke particles, and roasting and removing a fluorine-containing complex by a pyrogenic process. The method not only reduces the risk of solid waste stockpiling, but also recovers the zinc in the aluminum powder slag, reduces the loss of the zinc, makes valuable use of the characteristics of aluminum and aluminum oxide in the aluminum powder slag, utilizes the complexing mechanism of removing fluorine ions by aluminum salt, reduces the content of the fluorine ions, and solves the adverse effects that the fluorine ions of a system are increased and the zinc skin of the electrolytic cathode of zinc smelting is difficult to strip.
Description
Technical Field
The invention relates to the technical field of nonferrous metallurgy processes, in particular to a recycling method of aluminum powder slag of a zinc smelting cathode aluminum plate brush plate.
Background
The annual output of aluminum powder slag of a brushing plate of a zinc smelting cathode aluminum plate of a conventional zinc hydrometallurgy system is about 3t, and the aluminum powder slag has high zinc and aluminum contents and is often accompanied with partial acid-containing liquid in the brushing plate process, so that spontaneous combustion is often generated in the process of generating heat in the oxidation process of zinc and aluminum, the method belongs to solid waste stacking, not only causes environmental protection accidents, but also increases the solid waste stacking quantity, and in order to avoid the environmental protection accidents, the invention needs to provide a recycling method of the aluminum powder slag of the brushing plate of the zinc smelting cathode aluminum plate.
Disclosure of Invention
In order to solve the problem that the solid waste and stockpiling of the aluminum powder slag of the brushing plate of the cathode aluminum plate cannot be reduced in the prior art, the invention provides a recycling method of the aluminum powder slag of the brushing plate of the cathode aluminum plate for zinc smelting.
The invention adopts the following technical scheme:
a recycling method of aluminum powder slag of a zinc smelting cathode aluminum plate brush plate is characterized by comprising the following steps:
step 1: adding cathode aluminum plate brush plate aluminum powder slag into zinc smelting waste electrolyte to form mixed solution; the adding amount of the aluminum powder slag is (20-40) kg/m 3 Zinc smelting waste electrolyte;
step 2: adding the mixed solution obtained in the step 1 into a zinc smelting neutral leaching procedure for neutral leaching; the zinc smelting neutral leaching process comprises the following steps: zinc concentrate calcine (zinc smelting raw material) and an oxidant are used as raw materials, low-pressure air is introduced for neutral leaching, and the final PH value is 4.8-5.2; the oxidant is used for oxidizing ferrous ions and promoting the simple substance of the aluminum powder to be dissolved in an acid environment, the simple substance aluminum is used as a reducing agent, the pyrolusite is used as an oxidant and is used for promoting the simple substance aluminum to be quickly dissolved, and qualified liquid is provided for the next procedure;
after neutral leaching is finished, adding 0.1-0.3% concentration flocculating agent (the concentration refers to the ratio of the weight of the added flocculating agent to the volume of liquid) for adsorbing cationic impurities (arsenic, antimony, germanium and other impurities) in the solution, and then carrying out liquid-solid separation to obtain supernatant in middle leaching and underflow in middle leaching;
the supernatant in the middle leaching is purified in three stages to obtain a new zinc electrolysis solution, and the bottom flow in the middle leaching is mainly an aluminum fluorine complex;
and 3, step 3: taking the middle leaching underflow, adding zinc electrolysis waste liquid, and carrying out acid leaching, wherein the final pH value is 1.5-2.5, and preferably 2.0. Obtaining acid supernatant and acid leaching underflow after acid leaching; returning the acid supernatant to the step 2 for neutral leaching, wherein the purpose of acid leaching is to leach more zinc ions into the acid supernatant and further recover zinc;
and 4, step 4: and (3) taking acid leaching underflow, adding heavy calcium carbonate powder to adjust the pH value to 5.0, then carrying out flotation, and carrying out filter pressing after flotation to form leaching residue. Flotation is to float the silver in the acid leaching underflow to the maximum extent.
Because the pH value of the acid leaching end point is about 2.0, the addition of the medicament in a flotation workshop is not favorable, so that an alkaline auxiliary material is required to be added to adjust the pH value to 5.0; and returning the liquid subjected to flotation and filter pressing to neutral leaching again, and recovering aluminum ions and zinc ions.
And 5: and (4) placing the acid leaching slag obtained in the step (4) in a multi-hearth furnace, introducing oxygen and coke particles, and removing the fluorine-containing complex by pyrogenic roasting.
In the invention, the dissolved aluminum powder slag is added in the neutral leaching process of zinc smelting, and the adding amount of the aluminum powder slag is controlled to be 20-40 kg/m 3 In the whole middle leaching process, fluoride ions and aluminum ions form a complex to precipitate along with the increase of the PH value, then acid leaching is performed to better leach zinc ions in the aluminum powder slag, excessive aluminum ions in acid supernatant after acid leaching are returned to perform neutral leaching and can be continuously used, then acid leaching slag enters a flotation process, the PH value is adjusted, the complex is continuously formed, and thus the fluoride ions enter the leaching slag and enter a multi-hearth furnace to be removed at high temperature.
The leaching process comprises two working procedures of neutral leaching and acidic leaching: neutral leaching is a process of dissolving zinc element in calcine into liquid by using dilute sulfuric acid, simultaneously controlling the pH value of a final tank, and removing impurities such as arsenic, antimony, germanium and the like through hydrolysis of iron; the acid leaching is to leach the zinc element in the neutral leaching residue to the maximum extent under the condition of higher acidity, ensure that the zinc element enters the solution as much as possible, and simultaneously control impurities to enter the liquid.
Further, the content of sulfuric acid in the zinc smelting waste electrolyte is 150-200 g/L, and the content of Zn is 40-65 g/L; the zinc content in the aluminum powder slag is 15-20%, and the balance is aluminum metal simple substance and aluminum oxide.
Furthermore, the oxidant is pyrolusite and air (with enough oxygen), and the particle size of the pyrolusite is 120 meshes. The zinc concentrate calcine contains 55% of zinc, the granularity is +80 meshes and is less than or equal to 5%, and-200 meshes and is more than or equal to 78%.
Further, the content of manganese dioxide in the pyrolusite is more than or equal to 50 percent, and the molar ratio of manganese ions in the added pyrolusite to ferrous ions in the solution is (0.6-0.7): 1.
further, the pressure of the low-pressure wind is 0.4MPa, and the ventilation volume is 10m 3 /h。
Further, the content of the heavy calcium powder is more than or equal to 92 percent.
Further, the temperature in the multi-hearth furnace is 680-720 ℃.
The main principle of the invention is as follows: the zinc and the aluminum in the aluminum powder slag mainly come from the production of the cathode aluminum plate brushing process (namely zinc smelting cathode aluminum plate brushing aluminum powder slag), the zinc and the aluminum powder slag mainly exist in the forms of zinc metal simple substance and zinc oxide as well as aluminum metal simple substance and aluminum oxide, the zinc content is 15% -20%, and the balance is aluminum metal and aluminum oxide basically. The aluminum powder slag is fully dissolved in the acid-containing waste liquid to form zinc sulfate and aluminum sulfate acid-containing liquid, and according to the aluminum-containing adsorbent in the acid solution, aluminum has strong coordination capacity to fluorine, so that the aluminum-containing adsorbent has good selectivity to fluorine in the zinc smelting waste electrolyte, the fluorine removal effect to the zinc smelting waste electrolyte is good, and the action mechanism of removing fluorine ions by aluminum salt is adsorption, ion exchange and complexing sedimentation. (1) Amorphous Al (OH) with a large surface area formed during defluorination of aluminium salts 3 Can generate hydrogen bond adsorption to fluorine, the radius of the fluorine ion is small, the electronegativity is strong, (2)F) - With OH - Has similar radius and same charge, and Al is added into the solution in the process of removing fluorine from aluminum salt 13 O 4 （OH） 14 7+ Isopolycation and amorphous Al (OH) formed after hydrolysis 3 Precipitation of OH therein - And F - An exchange occurs. (3) F - Can be reacted with Al 3+ Form from AlF 2+ To AlF 3- And 6 kinds of complex are complexed and settled to remove fluorine. Therefore, after the aluminum powder slag is added into the zinc smelting waste liquid, the acid-containing liquid of zinc sulfate and aluminum sulfate is formed, and the processDoes not generate arsine gas, is added into the neutral leaching process, and the adding amount of the aluminum powder slag is controlled to be 20-40 kg/m 3 Liquid continuously and stably enters a system to promote the content of fluorine ions in the waste electrolyte of zinc smelting to be gradually reduced, thereby ensuring the normal stripping of electrolytic cathode zinc.
The reaction formula is as follows:
Al 2 O 3 +3H 2 SO 4 =Al 2 (SO 4 ) 3 +3H 2 O
Al 3+ +3H 2 O=Al(OH) 3 +3H +
the invention aims to remove fluoride ions in zinc smelting waste electrolyte by adopting aluminum in aluminum powder slag, and dissolve zinc into the waste electrolyte for recovery. The action mechanisms of removing fluoride ions by aluminum salt are adsorption, ion exchange and complex sedimentation.
Compared with the prior art, the invention has the following technical effects:
the invention provides a recycling method of aluminum powder slag of a zinc smelting cathode aluminum plate brush plate, which is characterized in that the aluminum powder slag is added into zinc smelting acid-containing waste electrolyte, through full dissolution, fluorine-aluminum complex enters acidic leaching slag, the fluorine content of the zinc smelting waste electrolyte is controlled below a normal value of 40mg/L, and the fluorine-aluminum complex in the leaching slag is removed through high-temperature roasting in a multi-hearth furnace.
On the premise of ensuring safety and environmental protection, the aluminum powder slag generated in the process of brushing the cathode aluminum plate by using the zinc smelting is recycled, no additional harmful gas is generated in the whole process, the risk of stockpiling of solid wastes is reduced, the zinc in the aluminum powder slag is recycled, the loss of zinc metal is reduced, the characteristics of aluminum and aluminum oxide in the aluminum powder slag are utilized, the complexing mechanism of removing fluorine ions by using aluminum salt is fully utilized, the aim of removing fluorine in a system is fulfilled, the content of the fluorine ions in the system is reduced, and the adverse effect caused by difficult stripping of zinc skins of the electrolytic cathode in the zinc smelting when the fluorine ions in the system are increased is solved. The invention solves the spontaneous combustion risk of solid waste stockpiling and the adverse effect of high content of fluorinion on the system.
The method fully realizes the valuable utilization of the aluminum powder slag, recovers the zinc metal of the aluminum powder slag, reduces the content of the fluorine ions in the zinc electrolysis waste liquid by utilizing the characteristics of the aluminum metal in the aluminum powder slag, and avoids the adverse effect of high-content fluorine ions on the system.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is further described with reference to the following drawings and detailed description, but the invention is not limited thereto. In the following examples, the particle size of the pyrolusite is 120 meshes, the manganese dioxide content in the pyrolusite is more than or equal to 50%, and the Zn content in the zinc smelting waste electrolyte (also called zinc electrolysis waste liquid) is 40-65 g/L, H 2 SO 4 The content is 150-200 g/L.
The invention provides a method for recycling aluminum powder slag of a zinc smelting cathode aluminum plate brush plate, which comprises the following steps: adding aluminum powder slag of a brush plate of a zinc smelting cathode aluminum plate into zinc electrolysis waste liquid; after fully dissolved under certain stirring intensity, conveying the mixture into a neutral leaching oxidation tank; along with the increase of PH value in the neutral leaching process, aluminum fluoride complex precipitate is formed, and acid leaching is carried out along with the middle leaching bottom flow; in the acid leaching underflow, heavy calcium carbonate powder is added to adjust the pH value in the flotation process, the acid leaching residue is placed in a rotary kiln, oxygen and coke particles are introduced, fluorine forms gas volatilization open circuit, and aluminum enters water quenching residue. On the premise of ensuring safety and environmental protection, the aluminum powder slag generated in the process of smelting the cathode aluminum plate brushing plate by using the zinc is recycled, so that the stockpiling of solid wastes is reduced, the zinc in the aluminum powder slag is recycled, and the characteristics of aluminum and aluminum oxide in the aluminum powder slag are utilized to achieve the aim of removing the fluorine in the system. The risk of solid waste stockpiling and the adverse effect of fluorine ions on the system are solved. By adopting the method, the risk of solid waste stockpiling is reduced, no additional harmful gas is generated in the whole invention process, the characteristics of aluminum metal and aluminum oxide in the aluminum powder slag are utilized effectively, the content of fluorine ions in the system is reduced, and the adverse effect of high content of the fluorine ions on the system is avoided.
Example 1
When the fluorine content in the zinc smelting waste electrolyte (hereinafter referred to as waste liquid) reaches 45mg/L, adding aluminum powder slag into the waste liquid, wherein the adding amount of the aluminum powder slag is 20kg/m in the embodiment 3 The waste liquid ensures that the aluminum powder slag is fully dissolved, and the waste liquid continuously and stably enters a system to ensure that enough aluminum salt exists in the liquid. Adding the mixed solution into a zinc smelting neutral leaching procedure for neutral leaching; the zinc smelting neutral leaching process comprises the following steps: taking zinc concentrate calcine (zinc smelting raw material) and pyrolusite as raw materials, introducing low-pressure air, and performing neutral leaching, wherein the final pH value is 4.8-5.2; the pressure of the low-pressure air is 0.4MPa, and the ventilation volume is 10m 3 H; after neutral leaching, adding 0.1-0.3% concentration flocculant polyacrylamide for adsorbing cationic impurity in the solution, settling in a thickener to separate liquid from solid, purifying the supernatant in three stages to obtain new electrolytic solution, and recovering zinc from the aluminum powder slag. Taking the middle leaching underflow (mainly aluminum fluorine complex), adding zinc electrolysis waste liquid, and performing acid leaching, wherein the final pH value is 1.5-2.5; returning the acid supernatant to the neutral leaching process, introducing the acid leaching underflow into a thickener of a silver recovery process, adding heavy calcium powder into a raw ore tank (i.e. a reaction tank in which the heavy calcium powder is added in the silver flotation process), gradually adjusting the pH value to be more than 5.0, filtering the silver flotation tailings dense underflow on a diaphragm automatic box-type filter press, and squeezing to reduce the water content in the acidic leaching residues. Taking the acid leaching slag in the acid leaching underflow, placing the acid leaching slag in a multi-hearth furnace, wherein the temperature of the multi-hearth furnace is 680-720 ℃, introducing oxygen and coke particles, and removing the fluorine-containing complex by roasting with a fire method. The fluorine content of the new electrolytic liquid sample assay liquid is 29.25mg/l, and the electrolytic cathode zinc skin is not difficult to strip.
Example 2
When the fluorine content in the zinc smelting waste electrolyte reaches 55mg/l, adding 30 kg/m of aluminum powder slag into the waste liquid 3 Liquid ensures that the aluminum powder slag is fully dissolved, and the waste liquid continuously and stably enters a system to ensure that enough aluminum salt is in the liquid. Adding the mixed solution into a zinc smelting neutral leaching procedure for neutral leaching; the zinc smelting neutral leaching process comprises the following steps: taking zinc concentrate calcine (zinc smelting raw material) and pyrolusite as raw materials, introducing low-pressure air, performing neutral leaching, wherein the final pH value is 4.8-5.2, the pressure of the low-pressure air is 0.4MPa, and the ventilation volume is 10m 3 H; adding 0.1-0.3% concentration flocculant polyacrylic ester after neutral leachingAmine is used for adsorbing cationic impurities in the solution and is settled to a thickener to achieve the effect of liquid-solid separation; and then the middle supernatant is purified by three sections to obtain new electrolytic solution, and zinc in the aluminum powder slag enters the middle supernatant to be recovered. Taking the middle leaching bottom flow, adding zinc electrolysis waste liquid, and performing acid leaching, wherein the end point pH value is 1.5-2.5; returning the acid supernatant to the neutral leaching process, feeding the acid leaching underflow into a thickener of a silver recovery section, passing through a raw ore tank, adding heavy calcium powder, gradually adjusting the pH value to be more than 5.0, filtering the silver flotation tailings dense underflow on a diaphragm automatic chamber filter press, and squeezing to reduce the water content in the acid leaching slag. Taking the acid leaching slag in the acid leaching underflow, placing the acid leaching slag in a multi-hearth furnace, wherein the temperature of the multi-hearth furnace is 680-720 ℃, introducing oxygen and coke particles, and removing the fluorine-containing complex by roasting with a fire method. The fluorine content of the new electrolytic liquid sample assay liquid is 35mg/l, and the electrolytic cathode zinc skin is not difficult to peel.
Example 3
When the fluorine content of the fluorine-containing solution for wet zinc electrolysis reaches 65mg/l, the aluminum powder slag is added into the waste liquid, 40 kg/m is added in the embodiment 3 Liquid ensures that the aluminum powder slag is fully dissolved, and the waste liquid continuously and stably enters a system to ensure that enough aluminum salt is in the liquid. Adding the mixed solution into a zinc smelting neutral leaching procedure for neutral leaching; the zinc smelting neutral leaching process comprises the following steps: taking zinc concentrate calcine (zinc smelting raw material) and pyrolusite as raw materials, introducing low-pressure air, performing neutral leaching, wherein the final pH value is 4.8-5.2, the pressure of the low-pressure air is 0.4Map, and the ventilation volume is 10m 3 H; after neutral leaching, adding 0.1-0.3% concentration flocculant polyacrylamide for adsorbing cationic impurity in the solution, and settling to a thickener to realize liquid-solid separation; and then the middle supernatant is purified by three sections to obtain new electrolytic solution, and zinc in the aluminum powder slag enters the middle supernatant to be recovered. Taking the middle leaching bottom flow, adding zinc electrolysis waste liquid, and performing acid leaching, wherein the end point pH value is 1.5-2.5; returning the acid supernatant to the neutral leaching process, introducing the acid leaching underflow into a thickener of a silver recovery section, passing through a raw ore tank, adding heavy calcium powder, gradually adjusting the pH value to be above 5.0, filtering the silver flotation tailings dense underflow on a diaphragm automatic chamber filter press, and squeezing to reduce the acidityWater in the leached residue. Taking the acid leaching slag in the acid leaching underflow, placing the acid leaching slag in a multi-hearth furnace, wherein the temperature of the multi-hearth furnace is 680-720 ℃, introducing oxygen and coke particles, and removing the fluorine-containing complex by roasting with a fire method. The fluorine content of the new electrolytic liquid sample test liquid is 32.5mg/l, and the electrolytic cathode zinc skin is not difficult to peel.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are merely illustrative and not restrictive, and it should be understood that other embodiments may be easily implemented by those skilled in the art by means of replacement or modification according to the technical contents disclosed in the specification, and therefore, all changes and modifications that come within the spirit and technical conditions of the present invention should be included in the claims of the present invention.
Claims (9)
1. A recycling method of aluminum powder slag of a zinc smelting cathode aluminum plate brush plate is characterized by comprising the following steps:
step 1: adding cathode aluminum plate brush plate aluminum powder slag into zinc smelting waste electrolyte to form mixed solution;
step 2: adding the mixed liquor obtained in the step 1 into a zinc smelting neutral leaching process for neutral leaching; adding a flocculating agent after the neutral leaching is finished to obtain a supernatant in the middle leaching and a bottom flow in the middle leaching;
and step 3: taking the middle leaching bottom flow, adding zinc electrolysis waste liquid, carrying out acid leaching, obtaining acid supernatant and acid leaching bottom flow after acid leaching, and returning the acid supernatant to the step 2 for neutral leaching;
and 4, step 4: taking acid leaching underflow, adding heavy calcium powder to adjust the pH value to 5.0, then carrying out flotation, and carrying out filter pressing after flotation to form leaching residue;
and 5: and (4) placing the leaching residue obtained in the step (4) in a multi-hearth furnace, introducing oxygen and coke particles, and removing the fluorine-containing complex by pyrogenic roasting.
2. The method for recycling the aluminum powder slag of the zinc smelting cathode aluminum plate brush plate according to claim 1, wherein the supernatant of the immersion medium obtained in the step 2 is subjected to three-stage purification to obtain a new zinc electrolysis solution.
3. The recycling method of aluminum powder slag of a zinc smelting cathode aluminum plate brush plate according to claim 1, characterized in that the content of sulfuric acid in the zinc smelting waste electrolyte is 150-200 g/L, zn is 40-65 g/L; the zinc content in the aluminum powder slag is 15-20%, and the balance is aluminum metal simple substance and aluminum oxide.
4. The recycling method of aluminum powder slag of zinc smelting cathode aluminum plate brushing plates according to claim 1, characterized in that the amount of the aluminum powder slag added per cubic meter of the zinc smelting waste electrolyte is 20-40 kg.
5. The method for recycling the aluminum powder slag of the zinc smelting cathode aluminum plate brush plate according to claim 1, wherein the pH value of the neutral leaching end point is 4.8-5.2.
6. The method for recycling the aluminum powder slag of the zinc smelting cathode aluminum plate brush plate according to claim 1, wherein the pH value of the acid leaching end point is 1.5-2.5.
7. The method for recycling the aluminum powder slag of the zinc smelting cathode aluminum plate brush as recited in claim 1, wherein the flocculant is anionic polyacrylamide.
8. The method for recycling the aluminum powder slag of the zinc smelting cathode aluminum plate brush plate according to claim 1, wherein the content of the heavy calcium powder is more than or equal to 92 percent.
9. The method for recycling the aluminum powder slag of the zinc smelting cathode aluminum plate brush plate according to claim 1, wherein the temperature of the multi-hearth furnace is 680-720 ℃.
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| CN202211415845.8A CN115652096A (en) | 2022-11-11 | 2022-11-11 | Recycling method of zinc smelting cathode aluminum plate brush plate aluminum powder slag |
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| CN202211415845.8A CN115652096A (en) | 2022-11-11 | 2022-11-11 | Recycling method of zinc smelting cathode aluminum plate brush plate aluminum powder slag |
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