CN110295290B - Method for leaching zinc by acid leaching slag and lead slag in one-kettle three-stage oxygen pressure manner - Google Patents
Method for leaching zinc by acid leaching slag and lead slag in one-kettle three-stage oxygen pressure manner Download PDFInfo
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- C22B11/00—Obtaining noble metals
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- C22B11/021—Recovery of noble metals from waste materials
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- C22B13/00—Obtaining lead
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- C22B13/025—Recovery from waste materials
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- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
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- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C22B7/007—Wet processes by acid leaching
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Abstract
The invention relates to a method for leaching zinc by acid leaching slag and lead slag through one-kettle three-stage oxygen pressure, which belongs to the technical field of wet metallurgy. The method provides a new idea for combined treatment of lead-zinc smelting slag materials, the iron content of the obtained oxygen pressing liquid is less than or equal to 500mg/L, iron does not need to be removed independently, and the obtained oxygen pressing liquid can be directly merged into a main system zinc leaching process after germanium and indium are recovered; the zinc content of the oxygen pressing slag is less than or equal to 2 percent, and more than 90 percent of the iron slag is merged into a crude lead pyrogenic process system along with the oxygen pressing slag to be used as a smelting flux, the lead and the silver are recovered, and finally, the cement is produced in a water quenching slag mode, so that the harmless treatment and utilization of the zinc smelting wet-process iron slag are realized.
Description
Technical Field
The invention belongs to the technical field of wet metallurgy, and particularly relates to a method for leaching zinc by acid leaching slag and lead slag in a one-kettle three-stage oxygen pressure manner.
Background
The existing treatment modes of acid leaching slag generated by zinc traditional wet smelting include a pyrogenic method and a wet method, wherein the pyrogenic method mainly adopts a fuming furnace or a rotary kiln and the like to perform fuming enrichment at present, so that the defects of long flow, high cost and the like exist, but smelting waste slag enters the cement industry and can be well harmlessly treated and utilized; the wet process mainly comprises reduction leaching and high-acid leaching, and compared with the pyrogenic process, the process is shorter, the cost is reduced, but the gypsum slag and the iron slag produced in a recycling way are not harmless and applied at present, only can be treated in a stockpiling way, and can cause unpredictable pollution to the environment. Aiming at the defects of the acid leaching residue wet treatment process, technical workers carry out technical improvement and develop some new processes. For example, the invention adopts a normal-pressure dilute acid leaching process to effectively reduce the zinc content in the slag, thereby greatly improving the zinc recovery rate and reducing the pollution to the environment, but the invention adopts a normal-pressure oxidation leaching process, has lower reaction efficiency (more than 3 h), does not reasonably treat the generated iron slag and does not realize the harmless treatment of slag materials. ② the Chinese patent application (201510334478.2) discloses a method for separating valuable metals from wet zinc smelting waste residue, the invention adopts roasting-pressure leaching mode to treat acid leaching residue, the roasting temperature is 600-720 ℃, so that 30% of zinc is volatilized and dispersed into smoke dust, the initial acid of pressure leaching is lower, the mechanism is unknown, and the leaching rate of zinc is lower (85%).
The zinc oxide smoke dust leaching slag (lead slag) is treated by a wet treatment process which comprises normal pressure leaching and pressure leaching, the specific process varies according to different materials, but the research on the aspect of producing the zinc oxide smoke dust leaching slag by a full-cooling fuming process is relatively fresh, and compared with the conventional lead slag, the zinc oxide smoke dust leaching slag has higher ZnS content and is difficult to leach by normal pressure leaching. ③ the patent with the Chinese patent application number of (201610049725.9) discloses a recovery process of zinc in acid leaching slag (lead slag), the invention adopts a closed cycle mode to return the byproduct colloidal ferric hydroxide (iron slag) to leaching and recycling, thus avoiding environmental pollution, but the process has no open circuit part of Fe, which can lead to the enrichment of Fe element in the system and can not operate effectively and continuously. The invention adopts a middle leaching-acid leaching-oxygen leaching process to treat the secondary zinc oxide smoke dust, the process is long and tedious, and the zinc sulfide in the smoke dust can not be fully leached.
The iron removal of the leachate or the oxygen hydraulic fluid is mainly divided into neutralization iron removal, alum precipitation iron removal, goethite iron removal and hematite iron removal, and the generated iron slag is stockpiled as solid waste, so that the harmless and recycling treatment is in bottleneck. The invention adopts the steps that high-iron zinc sulfide concentrate and oxidized ore are put into a kettle together according to the ratio of 23:1, the pH value of a control end point is 0.15-0.2mol/L, the reacted oxygen pressure liquid is adjusted to the pH value of 5.0-5.2 to purify and precipitate iron, the process adopts twice iron precipitation, the entrainment loss of zinc is increased, the common slag zinc is not distributed, and the harmless disposal of iron slag has no clear direction; the invention improves on the basis of the fifth step, controls the end point pH value in the kettle to be 5.2-5.5, thus leading a large amount of leached zinc to be hydrolyzed and precipitated into slag, also having no public distribution of zinc in the slag, having no definite direction for harmless treatment of iron slag and having no obvious progress.
Disclosure of Invention
In order to overcome the problems in the background art, the invention provides a method for leaching zinc by matching acid leaching slag with lead slag and three-stage oxygen pressure in one kettle, the method has three functions in one kettle, the flow is short, the operation is simple and convenient, the obtained oxygen pressure liquid does not need to be deironized independently, and meanwhile, the harmless disposal and utilization of iron and sulfur in iron slag are realized.
In order to realize the purpose, the invention is realized by the following technical scheme:
the method for leaching zinc from acid leaching slag by matching with lead slag through one-kettle three-section oxygen pressure leaching is characterized in that the material properties of the acid leaching slag and the lead slag are utilized, a one-kettle three-section high-efficiency treatment process is adopted, short-flow leaching is carried out on zinc in raw materials, and hot acid leaching of the acid leaching slag, oxidation leaching of the lead slag and vanadium precipitation iron removal are continuously realized in a kettle in a segmented manner, and the method specifically comprises the following steps: 1) carrying out acid leaching residue leaching reaction in an oxygen pressure kettle front chamber; 2) carrying out oxidation leaching and neutralization reaction of lead slag in an oxygen autoclave in a room; 3) and carrying out lead slag iron precipitation reaction in a rear chamber of the oxygen autoclave.
Further, in the step 1), directly mixing acid leaching residues and zinc electrolysis waste liquid, pumping into a front chamber of the oxygen pressure kettle, controlling the temperature to be 100 ℃ and 120 ℃, introducing no oxygen into the front chamber, leaching for 1-2h, and then feeding ore pulp into a middle chamber of the oxygen pressure kettle.
Further, in the step 2), pulping the lead slag and the process water, pumping into a middle chamber of an oxygen pressure kettle, controlling the temperature to be less than or equal to 110 ℃, controlling the oxygen concentration to be 90%, leaching for 0.5-1h, and then feeding the ore pulp into a rear chamber of the oxygen pressure kettle.
Further, the adopted lead slag is generated by leaching full-cold-material fuming zinc hypoxide smoke dust with sulfuric acid, the zinc content of the lead slag is 12% -20%, wherein the Zn accounts for more than 50% of the total Zn in the ZnS.
Further, the proportion of the acid leaching slag and the lead slag in the steps 1) and 2) is 0.5-2.5.
Further, in the step 3), the mixed ore pulp enters a rear chamber of an oxygen pressure kettle, alum precipitation and iron removal are carried out, the temperature is controlled to be 90-110 ℃, the oxygen concentration is 90%, after reaction is carried out for 0.25-0.5h, the final acid is controlled to be 5-20g/L, and the ore pulp is discharged from the kettle.
Further, the ore pulp obtained in the step 3) is subjected to solid-liquid separation to obtain oxygen pressing liquid and oxygen pressing slag.
Furthermore, the zinc content of the obtained oxygen pressing slag is less than or equal to 2 percent, and the iron content of the oxygen pressing liquid is less than or equal to 500 mg/L.
Furthermore, the oxygen pressure liquid can enter a zinc system for recycling without removing iron, the iron slag is merged into the oxygen pressure slag to directly enter a crude lead smelting system, the oxygen pressure slag serves as a slagging solvent for recycling, the iron slag can not be generated independently, and the harmless treatment and utilization of iron and sulfur in the iron slag are realized.
Further, the pressure in the oxygen autoclave is 0.6-0.8 MPa.
The invention has the beneficial effects that:
the method fully utilizes the material properties of the acid leaching slag and the lead slag, adopts a one-kettle three-section efficient treatment process to leach zinc in the raw materials in a short flow, and continuously realizes acid leaching slag leaching, lead slag oxidation leaching and alum precipitation iron removal in a kettle in sections. The method provides a new idea for combined treatment of lead-zinc smelting slag materials, the iron content of the obtained oxygen pressing liquid is less than or equal to 500mg/L, iron does not need to be removed independently, and the obtained oxygen pressing liquid can be directly merged into a main system zinc leaching process after germanium and indium are recovered; the zinc content of the oxygen pressing slag is less than or equal to 2 percent, and more than 90 percent of the iron slag is merged into a crude lead pyrogenic process system along with the oxygen pressing slag to be used as a smelting flux, the lead and the silver are recovered, and finally, the cement is produced in a water quenching slag mode, so that the harmless treatment and utilization of the zinc smelting wet-process iron slag are realized.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention will be described in detail below to facilitate understanding of the skilled person.
The method fully utilizes the material properties of the acid leaching slag and the lead slag, adopts a one-kettle three-section efficient treatment process to leach zinc in the raw materials in a short flow, and continuously realizes acid leaching slag leaching, lead slag oxidation leaching and alum precipitation iron removal in a kettle in sections. The method specifically comprises the following steps:
1) carrying out acid leaching residue leaching reaction in an oxygen pressure kettle front chamber;
2) carrying out oxidation leaching and neutralization reaction of lead slag in an oxygen autoclave in a room;
3) and carrying out lead slag iron precipitation reaction in a rear chamber of the oxygen autoclave.
More specific embodiments are:
step 1) directly mixing acid leaching residues (without ball milling) and zinc electrolysis waste liquid, pumping into an oxygen pressure kettle front chamber, controlling the temperature to be 100-120 ℃, introducing no oxygen, and leaching for 1-2h, wherein ore pulp enters an oxygen pressure kettle middle chamber. The zinc in the acid leaching residue exists mainly in the form of zinc ferrite, and the zinc ferrite is dissolved under the conditions of high acid and high temperature, such as direct size mixing by using zinc electrolysis waste liquid, temperature of 100-:
ZnO.Fe2O3+3H2SO4＝ZnSO4+Fe2(SO4)3+3H2O (1)
and 2) pulping lead slag (without ball milling) generated by leaching the fully-cooled fuming secondary zinc oxide smoke dust with sulfuric acid and process water, pumping the pulp into a middle chamber of an oxygen pressure kettle, controlling the temperature to be less than or equal to 110 ℃, controlling the oxygen concentration to be 90 percent and the pressure to be 0.6-0.8MPa, and after leaching for 0.5-1h, feeding ore pulp into a rear chamber of the oxygen pressure kettle. In the middle chamber of the reaction kettle, except that zinc sulfide in the lead slag reacts with ferric sulfate generated by the reaction formula (1), iron ions also transmit oxygen to promote and accelerate the dissolution of the zinc sulfide, and the reaction formula is as follows:
Fe2(SO4)3+ZnS＝2FeSO4+ZnSO4+S (2)
2FeSO4+1/2O2+H2SO4＝Fe2(SO4)3+H2O (3)
and 3) feeding the mixed ore pulp into a rear chamber of an oxygen pressure kettle, precipitating alum and removing iron, controlling the temperature to be 90-110 ℃, the oxygen concentration to be 90% and the pressure to be 0.6-0.8MPa, reacting for 0.25-0.5h, controlling the final acid to be 5-20g/L, and discharging the ore pulp out of the kettle. With the reduction of the acidity of the ore pulp, ferric ions in the ore pulp and lead sulfate in the lead slag generate lead jarosite precipitate, so that iron is precipitated into the slag. The reaction formula is as follows:
Fe2(SO4)3+PbSO4+H2O＝PbFe6(SO4)4(OH)12↓+6H2SO4 (4)
and 3) performing solid-liquid separation on the ore pulp obtained in the step 3) to obtain oxygen pressing liquid and oxygen pressing slag, wherein the oxygen pressing liquid can enter a zinc system for recycling without removing iron, and the oxygen pressing slag directly enters a crude lead smelting system to serve as a slagging solvent for recycling, so that iron slag cannot be generated independently.
The invention is further illustrated by the following examples in conjunction with a schematic process flow diagram (FIG. 1) and the major components of the materials and products (Table 1).
TABLE 1 main Components of acid-leached slag and lead slag
| Material(s) | Pb | Zn | Ge | As | Fe | S |
| Acid leaching slag | 5.30 | 13.79 | 0.0229 | 0.23 | 22.42 | 9.08 |
| Lead slag | 22.53 | 25.10 | 0.0394 | 0.11 | 1.53 | 18.98 |
Example 1
The matching ratio of the acid leaching slag and the lead slag is 1:1, the acid leaching slag is directly pulped by waste liquid, the solid-to-solid ratio of the pulped liquid is 5, the pulped liquid is directly pumped into a front chamber of a pressure kettle through a diaphragm, the stirring is controlled at 500rpm, the temperature is 105 ℃, oxygen is not introduced, the pressure is 0.6MPa, and after leaching is carried out for 1h, ore pulp flows to a middle chamber; pulping the lead slag and the process water, controlling the solid-to-liquid ratio of the pulping liquid to be 3, reacting in a middle chamber of a pressure kettle, controlling the stirring speed to be 500rpm, the temperature to be 110 ℃, the oxygen concentration to be 90 percent and the pressure to be 0.6MPa, leaching for 0.5h, and then feeding the mixed ore pulp into a rear chamber of the oxygen pressure kettle; stirring at 500rpm, controlling the temperature at 110 ℃, the oxygen concentration at 90% and the pressure at 0.6MPa, reacting for 0.25h, controlling the final acid at 18.14g/L, and discharging the solution from the kettle; the obtained oxygen hydraulic fluid is subjected to solid-liquid separation to obtain oxygen hydraulic fluid and oxygen hydraulic slag, wherein zinc in the oxygen hydraulic slag is 1.9%, iron in the oxygen hydraulic fluid is 400mg/L, the oxygen hydraulic fluid can enter a zinc system for recycling without removing iron, and the oxygen hydraulic slag directly enters a crude lead smelting system to serve as a slagging solvent for recycling. The oxygen hydraulic fluid and the iron slag composition are shown in Table 2.
TABLE 2 main Components of oxygen hydraulic fluid and oxygen hydraulic slag
Example 2
The matching ratio of the acid leaching slag and the lead slag is 1:2, the acid leaching slag is directly pulped by waste liquid, the solid-to-solid ratio of the pulped liquid is 5, the pulped liquid is directly pumped into a front chamber of a pressure kettle through a diaphragm, the stirring is controlled at 500rpm, the temperature is 120 ℃, oxygen is not introduced, the pressure is 0.8MPa, and after leaching is carried out for 1h, ore pulp flows to a middle chamber; pulping the lead slag and the process water, controlling the solid-to-liquid ratio of the pulping liquid to be 3, reacting in a middle chamber of a pressure kettle, controlling the stirring speed to be 500rpm, the temperature to be 110 ℃, the oxygen concentration to be 90 percent and the pressure to be 0.8MPa, leaching for 0.5h, and then feeding the mixed ore pulp into a rear chamber of the oxygen pressure kettle; stirring at 500rpm, controlling the temperature at 95 ℃, the oxygen concentration at 90% and the pressure at 0.8MPa, reacting for 0.25h, controlling the final acid at 6.42g/L, and discharging the solution from the kettle; the obtained oxygen hydraulic fluid is subjected to solid-liquid separation to obtain oxygen hydraulic fluid and oxygen hydraulic slag, wherein zinc in the oxygen hydraulic slag is 1.8%, iron in the oxygen hydraulic fluid is 410mg/L, the oxygen hydraulic fluid can enter a zinc system for recycling without removing iron, and the oxygen hydraulic slag directly enters a crude lead smelting system to serve as a slagging solvent for recycling. The oxygen hydraulic fluid and the iron slag composition are shown in Table 3.
TABLE 3 main Components of oxygen hydraulic fluid and oxygen hydraulic slag
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (5)
1. A method for leaching zinc by acid leaching slag and lead slag in a one-kettle three-stage oxygen pressure is characterized by comprising the following steps: the method comprises the following steps of performing short-flow leaching on zinc in a raw material by utilizing the material properties of acid leaching slag and lead slag and adopting a one-kettle three-section efficient treatment process, and continuously performing hot acid leaching of the acid leaching slag, oxidation leaching of the lead slag and alum precipitation iron removal in a one-kettle section by section, wherein the pressure in an oxygen pressure kettle is 0.6-0.8MPa, and the method specifically comprises the following steps:
carrying out acid leaching residue leaching reaction in an oxygen pressure kettle front chamber, wherein zinc in the acid leaching residue mainly exists in a zinc ferrite form; directly mixing acid leaching residue without ball milling with zinc electrolysis waste liquid, pumping into an oxygen pressure kettle front chamber, controlling the temperature at 100 ℃ and 120 ℃, introducing no oxygen into the front chamber, leaching for 1-2h, and then feeding ore pulp into an oxygen pressure kettle middle chamber;
carrying out oxidation leaching and neutralization reaction on lead slag in an oxygen autoclave indoors, wherein the lead slag is generated by leaching smoke sub-zinc oxide smoke dust of a full-cold material by sulfuric acid, and the lead slag contains zinc sulfide and lead sulfate; pulping lead slag without ball milling with process water, pumping into an oxygen pressure kettle middle chamber, controlling the temperature to be less than or equal to 110 ℃, controlling the oxygen concentration to be 90%, leaching for 0.5-1h, and then feeding ore pulp into an oxygen pressure kettle rear chamber;
3) carrying out lead slag iron precipitation reaction in a rear chamber of the oxygen autoclave, adding mixed ore pulp into the rear chamber of the oxygen autoclave, precipitating alum and removing iron, controlling the temperature to be 90-110 ℃, the oxygen concentration to be 90%, reacting for 0.25-0.5h, controlling the final acid to be 5-20g/L, and discharging the ore pulp out of the autoclave.
2. The method for leaching zinc by the acid leaching slag and the lead slag in a kettle through three-stage oxygen pressure according to the claim 1, which is characterized in that: the proportion of the acid leaching slag in the step 1) and the lead slag in the step 2) is 0.5-2.5.
3. The method for leaching zinc by the acid leaching slag and the lead slag in a kettle through three-stage oxygen pressure according to the claim 1, which is characterized in that: and 3) performing solid-liquid separation on the ore pulp obtained in the step 3) to obtain oxygen pressing liquid and oxygen pressing slag.
4. The method for leaching zinc by the acid leaching slag and the lead slag in a kettle through three-stage oxygen pressure according to the claim 3, which is characterized in that: the zinc content of the obtained oxygen pressing slag is less than or equal to 2 percent, and the iron content of the oxygen pressing liquid is less than or equal to 500 mg/L.
5. The method for leaching zinc by the acid leaching slag and the lead slag in a kettle through three-stage oxygen pressure according to the claim 4, which is characterized in that: the oxygen pressing liquid can enter a zinc system for recycling without removing iron, the oxygen pressing slag directly enters a crude lead smelting system and serves as a slagging solvent for recycling, iron slag cannot be generated independently, and harmless treatment and utilization of iron and sulfur in the iron slag are realized.
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| CN113832346B (en) * | 2021-09-16 | 2023-07-21 | 云南驰宏资源综合利用有限公司 | Method for efficiently and simply treating germanium-containing zinc leaching residues |
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| CN102560087B (en) * | 2012-03-23 | 2013-06-12 | 广西冶金研究院 | Method for extracting indium and zinc from high-iron indium-containing zinc calcine and preparing iron oxide |
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