CN114427035B - Synergistic extraction and harmless treatment method for valuable components of zinc smelting high-sulfur slag and application thereof - Google Patents
Synergistic extraction and harmless treatment method for valuable components of zinc smelting high-sulfur slag and application thereof Download PDFInfo
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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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- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
- C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
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Abstract
The invention discloses a method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag and application thereof, which comprises the following steps: crushing, sieving and alkaline extracting, wherein high-purity ammonia gas is introduced into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and the concentration of ammonium ions in the impregnating solvent is controlled to be 5-10mol/L and the concentration of ammonia gas is controlled to be 2-5mol/L; adding the high-sulfur slag into the impregnating solvent, slowly stirring at 5-10 ℃ for 6-12 hours, heating and stirring, overflowing ammonia gas in the heating and stirring process, stirring until no ammonia gas overflows, and standing for 3-6 hours to obtain filtrate and filter residues; adjusting the pH value of the solution to be neutral, continuously clouding the solution until the turbidity is not increased in the process of adding dilute sulfuric acid, and carrying out pressure filtration, acid extraction and the like. By adopting the technical scheme disclosed by the invention, the extraction efficiency is high by two times of reversed phase extraction, and the generated waste is convenient for harmless and environment-friendly treatment in the extraction process.
Description
Technical Field
The invention relates to the field of smelting, in particular to a method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag.
Background
Smelting is a refining technology, which is to extract metals from ores by roasting, smelting, electrolysis, chemical agent and other methods; reducing impurities contained in the metal or increasing certain components in the metal to smelt the metal into the required metal.
In the smelting process, a large amount of slag such as zinc smelting process is necessarily generated, and a large amount of high-sulfur slag is generated, wherein the high-sulfur slag contains a large amount of valuable metals which cannot be smelted, so that the high-sulfur slag is directly discarded to cause resource waste and is easy to generate a large amount of solid garbage pollution.
Therefore, in order to recycle valuable metals in slag, there are many reports on a technique for recycling valuable metals in slag, such as chinese patent application No.: CN200910303503.5 discloses a method for extracting valuable metals from electronic waste, which comprises the steps of crushing, ammoxidation leaching, organic component separation, leaching liquid purification and electrodeposition, and finally obtaining organic particles, gold/silver/palladium powder and cathode copper products respectively. The invention adopts an ammonia oxidation system to selectively leach the high-sulfur slag in zinc smelting, then utilizes the characteristic that the sulfur simple substance has good floatability, the organic component has smaller density and floats on the surface layer of the leaching liquid to separate the organic particles, and valuable metals Au, ag, pd, cu, ni, cd, zn and Pb enter the solution; then, the leaching solution is subjected to displacement extraction to obtain precious metals Au, ag and Pd; finally, electrodepositing copper is obtained by adopting an electrodepositing method, and after electrolyte is enriched, metals such as nickel, lead, zinc and cadmium are opened. The invention has the outstanding advantages of strong raw material adaptability, high metal recovery rate and small environmental pollution, and can achieve the unification of environmental benefit and economic benefit.
The technical proposal can extract valuable metals, but cannot recycle the valuable metals in the high-sulfur slag in zinc smelting.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag.
The invention solves the technical problems through the following technical scheme:
a method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag comprises the following steps:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be 1-5mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 5-10mol/L and the concentration of ammonia gas to be 2-5mol/L;
slowly stirring at 5-10deg.C for 6-12 hr, heating and stirring, overflowing ammonia gas during heating and stirring, stirring until no ammonia gas overflows, and standing for 3-6 hr to obtain filtrate and residue;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, turning on a stirring motor, slowly stirring, slowly dripping dilute sulfuric acid into the seasoning tank during stirring to adjust the pH of the solution to be neutral, and continuously clouding the solution until the turbidity is not increased during adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 4-6 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution to adjust the pH of the solution to be 1-2, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH of the detection solution is 7.0-7.5, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
(7) After the ammonia gas is introduced, standing and press filtering are carried out, and the obtained filter residue is acid extracted valuable metal.
Preferably, in the step (2), the concentration of ammonium ions is controlled to be 5mol/L.
Preferably, the ammonia concentration in the step (2) is controlled to be 2mol/L.
Preferably, after the impregnating solvent is added in the step (2), the solution is slowly stirred at 8 ℃ for 8 hours, and the stirring speed is controlled to be 40r/min.
Preferably, the concentration of the dilute sulfuric acid regulating solution in the step (3) is 0.5mol/L.
Preferably, the turbid liquid in the step (4) is subjected to pressure filtration after being kept stand for 5 hours.
Preferably, the slurry in the step (6) is added with a dilute sulfuric acid solution to adjust the pH of the solution to be 1.5, and then the solution is subjected to pressure filtration, and saturated ammonia gas is introduced into the filtrate until the pH of the detection solution is 7.2.
Preferably, the concentration of the dilute sulfuric acid solution in the step (6) is 0.5mol/L.
The invention also discloses application of the zinc smelting high-sulfur slag valuable component synergistic extraction and harmless treatment method in valuable metal recovery.
Compared with the prior art, the invention has the following advantages:
the invention discloses a method for synergic extraction and harmless treatment of valuable components in zinc smelting high-sulfur slag, which adopts alkali extraction and acid extraction in the technical scheme disclosed by the invention, and adopts twice reversed phase extraction, so that the extraction efficiency is high, and in the extraction process, the extraction agent which is weak in pollution and convenient to treat, such as ammonia gas, is adopted, so that valuable metals in slag can be fully extracted, and the waste generated by extraction is convenient for harmless and environment-friendly treatment, therefore, the environment-friendly treatment cost is low.
Drawings
FIG. 1 is a graph showing statistics of extraction yield in comparative example of the present invention.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Example 1
A method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag comprises the following steps:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be between 1mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 5mol/L and the concentration of ammonia gas to be 2mol/L;
slowly stirring at 5 ℃ after adding the impregnating solvent, heating and stirring for 6 hours, overflowing ammonia gas in the heating and stirring process, and standing for 3 hours after stirring until no ammonia gas overflows, thereby obtaining filtrate and filter residues;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, turning on a stirring motor, slowly stirring, slowly dripping dilute sulfuric acid (the concentration of the dilute sulfuric acid solution is 0.5 mol/L) into the seasoning tank in the stirring process, and regulating the pH of the solution to be neutral, wherein the solution is continuously turbid until the turbidity is not increased in the process of adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 6 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution (the concentration of the dilute sulfuric acid solution is 0.5 mol/L) to adjust the pH of the solution to 2, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH of the detection solution is 7.5, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
(7) After the ammonia gas is introduced, standing and press filtering are carried out, and the obtained filter residue is acid extracted valuable metal.
Example 2
A method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag comprises the following steps:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be 1-5mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 10mol/L and the concentration of ammonia gas to be 5mol/L;
slowly stirring at 10 ℃ after adding the impregnating solvent, heating and stirring for 2 hours, overflowing ammonia gas in the heating and stirring process, and standing for 6 hours after stirring until no ammonia gas overflows, thereby obtaining filtrate and filter residues;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, opening a stirring motor, slowly stirring, controlling the stirring speed to be 40r/min, slowly dripping dilute sulfuric acid into the seasoning tank to adjust the pH of the solution to be neutral in the stirring process, and continuously clouding the solution until the turbidity is no longer increased in the process of adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 4 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution to adjust the pH value of the solution to be 1, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH value of the detection solution is 7.0, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
the concentration of the dilute sulfuric acid regulating solution is 0.5mol/L.
Example 3
A method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag comprises the following steps:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be 3.5mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 8mol/L and the concentration of ammonia gas to be 3mol/L;
slowly stirring at 7 ℃ after adding the impregnating solvent, heating and stirring for 8 hours, overflowing ammonia gas in the heating and stirring process, and standing for 5 hours after stirring until no ammonia gas overflows, so as to obtain filtrate and filter residues;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, opening a stirring motor, slowly stirring, controlling the stirring speed to be 40r/min, slowly dripping dilute sulfuric acid into the seasoning tank to adjust the pH of the solution to be neutral in the stirring process, and continuously clouding the solution until the turbidity is no longer increased in the process of adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 5 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution to adjust the pH value of the solution to be 1.5, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH value of the detection solution is 7.2, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
the concentration of the dilute sulfuric acid regulating solution is 0.5mol/L.
Example 4
A method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag comprises the following steps:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be 1.5mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 9mol/L and the concentration of ammonia gas to be 5mol/L;
slowly stirring at 9 ℃ after adding the impregnating solvent, heating and stirring for 11 hours, overflowing ammonia gas in the heating and stirring process, and standing for 5.5 hours after stirring until no ammonia gas overflows, thereby obtaining filtrate and filter residues;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, opening a stirring motor, slowly stirring, controlling the stirring speed to be 40r/min, slowly dripping dilute sulfuric acid into the seasoning tank to adjust the pH of the solution to be neutral in the stirring process, and continuously clouding the solution until the turbidity is no longer increased in the process of adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 5 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution to adjust the pH value of the solution to be 1.8, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH value of the detection solution is 7.5, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
the concentration of the dilute sulfuric acid solution was 0.5mol/L.
Example 5
A method for cooperatively extracting and harmlessly disposing valuable components of zinc smelting high-sulfur slag comprises the following steps:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be 1-5mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 6mol/L and the concentration of ammonia gas to be 3mol/L;
slowly stirring at 8 ℃ after adding the impregnating solvent, heating and stirring for 7 hours, overflowing ammonia gas in the heating and stirring process, and standing for 4.5 hours after stirring until no ammonia gas overflows, thereby obtaining filtrate and filter residues;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, opening a stirring motor, slowly stirring, controlling the stirring speed to be 40r/min, slowly dripping dilute sulfuric acid into the seasoning tank to adjust the pH of the solution to be neutral in the stirring process, and continuously clouding the solution until the turbidity is no longer increased in the process of adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 5 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution to adjust the pH value of the solution to be 1.5, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH value of the detection solution is 7.2, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
(7) After the ammonia gas is introduced, standing and press filtering are carried out, and the obtained filter residue is acid extracted valuable metal.
The concentration of the dilute sulfuric acid solution was 0.5mol/L.
Comparative examples
Performance test:
according to the methods disclosed in inventive examples 1 to 5, valuable metals are extracted from slag, and the extraction rate is calculated by: the mass of the extracted (acid extracted valuable metal and alkali extracted valuable metal)/the mass of the crushed slag to be extracted is x100 percent, and the calculation result is shown in figure 1.
As can be seen from fig. 1: the method disclosed by the invention has the advantages of high extraction efficiency, stable extraction process, capability of fully extracting valuable metals in slag and improvement of resource reuse efficiency.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The method for cooperatively extracting and harmlessly disposing valuable components of the zinc smelting high-sulfur slag is characterized by comprising the following steps of:
(1) Crushing and sieving zinc smelting high-sulfur slag, and controlling the grain size of slag obtained by sieving to be 1-5mm to obtain slag to be extracted;
(2) Adding the slag to be extracted in the step (1) into a charging barrel, and adding a pre-prepared impregnating solvent;
the preparation method of the impregnating solvent comprises the following steps:
introducing high-purity ammonia gas into an ammonium chloride aqueous solution at normal temperature until the high-purity ammonia gas is saturated to obtain an impregnating solvent, and controlling the concentration of ammonium ions in the impregnating solvent to be 5-10mol/L and the concentration of ammonia gas to be 2-5mol/L;
slowly stirring at 5-10deg.C for 6-12 hr, heating and stirring, overflowing ammonia gas during heating and stirring, stirring until no ammonia gas overflows, and standing for 3-6 hr to obtain filtrate and residue;
(3) Adding the filtrate obtained in the step (2) into a seasoning tank, turning on a stirring motor, slowly stirring, slowly dripping dilute sulfuric acid into the seasoning tank during stirring to adjust the pH of the solution to be neutral, and continuously clouding the solution until the turbidity is not increased during adding the dilute sulfuric acid;
(4) Standing the turbid liquid in the step (3) for 4-6 hours, and performing filter pressing to obtain filter residues which are alkali-extracted valuable metals;
(5) Adding the filtrate obtained after the filter pressing in the step (4) into the filter residue in the step (2), and mixing and stirring to form slurry;
(6) Adding the slurry obtained in the step (5) into a dilute sulfuric acid solution to adjust the pH value of the solution to be 1-2, performing filter pressing, introducing saturated ammonia gas into the filtrate until the pH value of the detection solution is 7.0-7.5, continuously clouding the solution in the process of introducing the ammonia gas, and continuously stirring the solution in the process of introducing the ammonia gas;
(7) After the ammonia gas is introduced, standing and press filtering are carried out, and the obtained filter residue is acid extracted valuable metal.
2. The method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag according to claim 1, wherein the concentration of ammonium ions in the step (2) is controlled to be 5mol/L.
3. The method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag according to claim 2, wherein the ammonia concentration in step (2) is controlled to be 2mol/L.
4. The method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag according to claim 3, wherein the step (2) is characterized in that after the impregnating solvent is added, stirring is slowly carried out at 8 ℃ for 8 hours, and the stirring speed is controlled to be 40r/min.
5. The method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag according to claim 1, wherein the concentration of dilute sulfuric acid in step (3) is 0.5mol/L.
6. The method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag according to claim 1, wherein the turbid liquid in the step (4) is subjected to pressure filtration after being kept stand for 5 hours.
7. The method for synergic extraction and harmless treatment of valuable components of zinc smelting high-sulfur slag according to claim 1, wherein the slurry in step (6) is added with dilute sulfuric acid solution to adjust the pH of the solution to 1.5, and then is subjected to filter pressing, and saturated ammonia gas is introduced into the filtrate until the pH of the detection solution is 7.2.
8. The method for synergistic extraction and innocuous treatment of valuable components in zinc smelting high sulfur slag according to claim 7, wherein the concentration of the dilute sulfuric acid solution in the step (6) is 0.5mol/L.
9. Use of the zinc smelting high-sulfur slag valuable component synergistic extraction and harmless treatment method according to any one of claims 1-8 in valuable metal recovery.
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| CN102719675B (en) * | 2012-06-18 | 2014-08-06 | 山东国大黄金股份有限公司 | Method for comprehensively recovering zinc, lead and silver from waste residues generated in zinc smelting |
| JP6327943B2 (en) * | 2014-05-20 | 2018-05-23 | 太平洋セメント株式会社 | Method for recovering valuable metals in waste |
| CN106086439A (en) * | 2016-08-04 | 2016-11-09 | 西北矿冶研究院 | Method for recovering zinc and cobalt from zinc smelting slag |
| CN106399707A (en) * | 2016-11-07 | 2017-02-15 | 南昌专腾科技有限公司 | Comprehensive recovery method and system for zinc and silver in zinc smelting waste slag |
| CN109402411B (en) * | 2018-11-05 | 2022-11-15 | 北京清新环境技术股份有限公司 | Method for comprehensively recovering valuable metals from zinc smelting slag |
| CN113969354A (en) * | 2021-10-09 | 2022-01-25 | 六盘水中联工贸实业有限公司 | Method for recovering indium and zinc from zinc smelting soot |
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| CN113355527A (en) * | 2021-05-11 | 2021-09-07 | 江西铜业技术研究院有限公司 | Treatment method of high-sulfur smelting slag |
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