Separation and Recovery of Trace Silver from Sintering Filtrated Dust of Ferrous Metallurgy via Complexation Leaching
Abstract
:1. Introduction
2. Results and Discussion
2.1. Composition of SFD
2.2. Particle Size Analysis of SFD
2.3. Removal of Potassium from SFD
2.4. Na2S2O3-CuCl Leaching of SFD
2.5. Removal of Copper and Lead from the Leaching Solution
2.6. Separation and Recovery of Silver from Purified Liquids
3. Analysis of the Reaction Mechanism in the Recovery Process
3.1. Kinetics of Sodium Thiosulfate Extraction
3.2. Mechanism of the Removal of Copper and Lead Impurities from the Leaching Solution
4. Materials and Methods
4.1. Main Instruments and Reagents
4.2. Experimental Methods
4.2.1. Chemical Composition and Physical Analysis of SFD
- (1)
- Physical phase analysis. The physical phases of the experimental raw materials, i.e., iron and steel metallurgical sintering ash, sintering ash after washing, filter residue after leaching, intermediate products, and final products, were detected and analyzed via a D/max 2550 X-ray diffractometer produced by the Nippon Mechanics Company. The test conditions were as follows: rotating anode, 18 kW; phototube voltage, 40 kV; phototube current, 300 mA; scanning angle range, 5–90°; step size, 0.02°; and scanning speed, 14°/min. The X-ray diffraction (XRD) patterns were analyzed via Jade5.0 software.
- (2)
- Elemental analysis. A total of 0.1000 g of SFD was accurately weighed, completely covered with 2 g of sodium hydroxide, and calcined in a nickel crucible at 700 °C for 2 h. Then, the solid in the crucible was dissolved with 4 mol/L hydrochloric acid and filtered, and the solution was fixed to 100 mL. The solution was diluted several times and analyzed by an atomic absorption spectrometer to determine the content of each major valent metal in the SFD.
- (3)
- Particle size analysis. Using anhydrous ethanol as the dispersing medium and nitrogen as the carrier, the SFD after washing, drying, and sieving was subjected to particle size analysis via a Mastersizer 2000 laser particle size analyzer.
- (4)
- Structural analysis. A Nicolet 6700 Fourier transform infrared spectrometer was used to detect and analyze the structure of the experimental raw materials, i.e., iron and steel metallurgical sintering ash, sintering ash after washing, filtrate residue after leaching, intermediate products, and final products. The instrument test conditions were as follows: resolution, 4 cm−1; sample prepared by a KBr press sheet; scanning, four times; and scanning range, 4000–400 cm−1.
4.2.2. Complexing Agent Selection
4.2.3. Experimental Method of Complexation Leaching via the Sodium Thiosulfate Method
5. Conclusions
- (1)
- The leaching effects of different complexing agents and complexing auxiliaries on each metal element in sintered ash were compared through experiments, the possible reasons for the large difference in the silver leaching rates caused by different methods were analyzed and explored, and the Na2S2O3-CuCl leaching system was finally determined.
- (2)
- Through one-factor experimental exploration and optimization of the Na2S2O3-CuCl co-complexation method, the recommended leaching conditions were obtained as follows: a reaction time of 120 min, a reaction temperature of 60 °C, an L/S of 6:1, a Na2S2O3 concentration of 45 g/L, and a CuCl dosage of 5.0 mol/L. The silver leaching rate under these conditions reached 84.3%, and the main impurity in the sintered ash was copper metal. The leaching rate of lead from the sintered ash was less than 5%, and iron was not leached, resulting in selective leaching of silver.
- (3)
- The optimum conditions for the removal of impurity ions were determined to be as follows: a reaction time of 1 min and a 30% H2O2 dosage of 1.5 mL/100 mL of solution. Under these conditions, the conversion rate of the impurity ion lead reached 100%, the copper conversion rate reached 95%, and the silver loss rate was within 4%. The optimum recovery conditions were as follows: a reaction time of 20 min and a 30% H2O2 dosage of 0.6 mL/50 mL of solution. Under these conditions, silver at a low concentration could be completely converted, and the conversion rate of the remaining copper in the solution was less than 5%. The product obtained by filtration was silver sulfide, the purity of which was determined by titration to be approximately 97%.
- (4)
- The leaching kinetics of the Na2S2O3-CuCl system and the mechanism of the removal of copper and lead impurities from the leaching solution were investigated. The removal process was divided into three steps: first, the generation of hydroxyl radicals from H2O2 catalyzed by cuprous thiosulfate; second, the reaction of hydroxyl radicals with hydrogen peroxide to generate superoxide radicals; and third, the combination of superoxide radicals with cuprous thiosulfate to generate insoluble intermediates of ternary metal ion–peroxo structure–ligand complexes.
- (5)
- The process is easy to perform, is environmentally friendly, and significantly improves the silver recovery efficiency, providing a new technological pathway for the recovery of silver from industrial wastes, which is highly important for realizing the sustainable use of resources.
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Element | K | Sodium Carbonate (Chemistry) | Fe | Pb | Cu | Ag |
---|---|---|---|---|---|---|
Raw ash content (%) | 18.11 | 3.2 | 16.33 | 1.78 | 0.29 | 160 (g/t) |
Washed ash content (%) | 1.3 | 0.6 | 65.3 | 7.1 | 1.2 | 500 (g/t) |
Median Diameter (μm) d(0.5) | Volume Average Particle Size (μm) D[4,3] | Surface Area Average Particle Size (μm) D[3,2] | Specific Surface Area (m2/g) |
---|---|---|---|
51.1 | 61.1 | 9.7 | 0.6 |
Temperature (°C) | Reaction Time (min) | Efficiency Constant k1 | R2 |
---|---|---|---|
30 | 30–130 | 1.73 × 10−5 | 0.9624 |
40 | 30–130 | 1.48 × 10−5 | 0.8593 |
50 | 30–130 | 2.23 × 10−5 | 0.8912 |
Temperature (°C) | Reaction Time (min) | Efficiency Constant k2 | R2 |
---|---|---|---|
30 | 30–130 | 4.13 × 10−5 | 0.9650 |
40 | 30–130 | 5.19 × 10−5 | 0.8993 |
50 | 30–130 | 9.45 × 10−5 | 0.9189 |
Apparatus | Specification | Manufacturer |
---|---|---|
Atomic Absorption Spectrometer | ZA3000 | Hitachi High-tech Co., Ltd., Tokyo, Japan |
Rotary Evaporator | RE-2000A | Shanghai Yarong Co., Ltd., Shanghai, China |
Circulating water vacuum pump | SHB-Ⅲ | Zhengzhou Chengke Industry and Trade Co., Ltd., Zhengzhou, China |
X-ray diffraction (XRD) | D/max 2550 | Rigaku Co., Ltd., Tokyo, Japan |
Inductively Coupled Plasma Optical Emission Spectrometers (ICP-OES) | Optima 3000 | Perkin-Elmer Co., Ltd., Waltham, MA, USA |
Laser Particle Sizer | Mastersizer 2000 | Malvern Instruments Co., Ltd., Malvern, UK. |
Electric Blast Dryer | 101–2AB | Tianjin Teste Instruments Co., Ltd., Tianjin, China |
Infrared spectrometer | Nicolet 6700 | Thermo Nicolet Co., Ltd., Madison, WI, USA |
Reagent | Specification | Manufacturer |
---|---|---|
Sodium dodecylbenzene sulfonate | AR | Sinopharm Chemical Reagent Co., Ltd., Shanghai, China |
Sodium hyposulfide | AR | Hunan Huihong Reagent Co., Ltd., Changsha, China |
Sodium sulfurous acid | AR | Hunan Huihong Reagent Co., Ltd., Changsha, China |
Cuprous chloride | AR | Shanghai Maclean Reagent Co., Ltd., Shanghai, China |
Ammonia | AR | Sinopharm Chemical Reagent Co., Ltd., Shanghai, China |
30% Hydrogen peroxide | AR | Hunan Huihong Reagent Co., Ltd., Changsha, China |
Silver nitefficiency | AR | Guangzhou Jinzhujiang Chemical Co., Ltd., Guangzhou, China |
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Qiao, Z.; Yang, Y.; Zhang, T.; Chen, W. Separation and Recovery of Trace Silver from Sintering Filtrated Dust of Ferrous Metallurgy via Complexation Leaching. Molecules 2025, 30, 1339. https://doi.org/10.3390/molecules30061339
Qiao Z, Yang Y, Zhang T, Chen W. Separation and Recovery of Trace Silver from Sintering Filtrated Dust of Ferrous Metallurgy via Complexation Leaching. Molecules. 2025; 30(6):1339. https://doi.org/10.3390/molecules30061339
Chicago/Turabian StyleQiao, Zhiqiang, Yunquan Yang, Tian Zhang, and Weishun Chen. 2025. "Separation and Recovery of Trace Silver from Sintering Filtrated Dust of Ferrous Metallurgy via Complexation Leaching" Molecules 30, no. 6: 1339. https://doi.org/10.3390/molecules30061339
APA StyleQiao, Z., Yang, Y., Zhang, T., & Chen, W. (2025). Separation and Recovery of Trace Silver from Sintering Filtrated Dust of Ferrous Metallurgy via Complexation Leaching. Molecules, 30(6), 1339. https://doi.org/10.3390/molecules30061339