Valorization Potential of Polish Laterite Leaching Residues through Alkali Activation
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Alkali Activation
2.3. Characterization Method Techniques
3. Results and Discussion
3.1. Reactivity of Raw Materials in Alkaline Media
3.2. Effect of H2O/Na2O Molar Ratio in the Activating Solution and Ageing Period
3.3. Effect of Curing Temperature and Selected Molar Ratios
3.4. Physical Properties of AAMs
3.5. Structural Integrity of PLR50MK50 AAΜs
3.6. Comparison with a Previous Study
- -
- The SiO2 and Al2O3 content of the GLR were significantly higher (30.8 wt% SiO2 and 2.3 wt% Al2O3), compared to the respective values of the PLR, namely 23.3 and 1.2 wt%.
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- The Si and Al concentrations after the leaching of each residue with NaOH solution were 20.1 and 2.4 mg L−1, respectively, for the GLR (when 8 M NaOH solution was used), compared to 59.1 and 0.5 mg L−1, respectively, for the PLR (when 10 M NaOH solution was used); this indicated a deficiency of Al species in the solution in the second case, which was not favorable for the development of aluminosilicate bonds.
- -
- The molar ratio (SiO2 + Al2O3)/Na2O was more favorable in the reactive phase of the GLR.
- -
- The PLR had a high content of sulfates (30.6 wt%), which were shown as SO3 in Table 2 and confirmed by the presence of gypsum (Figure 3). Such sulfate compounds may have caused internal expansion during curing, ageing, and solidification [70]. The presence of gypsum in the precursors and its effect during alkali activation has been investigated in earlier studies, and the results varied. For example, Cong et al. [71] stated that silica fume could be used for the improvement of fly ash/slag-based geopolymers activated with calcium carbide residue and gypsum. On the other hand, exposure of specimens to 5% MgSO4 resulted in the formation of gypsum and ettringite, which caused surface spalling, cracking and the deterioration of the structural integrity of one-part geopolymers [72]. In another study, prior to efficient valorization of sulfidic mine waste for the production of construction materials, the extraction of hazardous contaminants and the removal of sulfur using flotation or bioleaching was carried out [73].
- -
- The content of the CaO in the PLR was much higher (17.9 wt%) compared to the respective one of the GLR (3.7 wt%), and this may have created implications during alkali activation. The role of CaO/Fe2O3 molar ratios needs to be further elucidated. So far, the few studies which were carried out to elucidate this ratio indicate that low CaO/FexOy molar ratios enhance the early kinetics and compressive strength of the produced specimens; in the present study, the CaO/Fe2O3 molar ratio was 1.99, which was four times higher than the ratio recorded in the previous study, at 0.48. [37,74,75].
- -
- The L/S ratio in GLR was smaller and thus more suitable for the production of specimens with higher compressive strengths. This ratio varied for different materials, but played an important role in assessing the viscosity and flowability of the paste. In several cases, low L/S ratios resulted in the production of AAMs with more compact microstructures and beneficial properties [61,76].
3.7. Characterization of Selected AAMs
3.7.1. Mineralogical Analysis
3.7.2. FTIR Analysis
3.7.3. SEM Analysis
3.8. Toxicity Assessment
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Particle Size (μm) | d90 (μm) | d50 (μm) | Specific Surface Area (m2/g) |
---|---|---|---|
PLR | 13.0 | 2.3 | 65.3 |
MK | 25.5 | 8.8 | 2.4 |
Oxide (%) | PLR | MK |
---|---|---|
Na2O | 8.1 | 1.3 |
Fe2O3 | 9.0 | 0.6 |
SiO2 | 23.3 | 52.5 |
Al2O3 | 1.2 | 38.6 |
Cr2O3 | 0.4 | 0.02 |
MgO | 5.9 | 0.3 |
NiO | 0.4 | - |
K2O | 0.01 | 2.4 |
TiO2 | 0.01 | 0.4 |
CoO | 0.02 | <0.00097 |
MnO | 0.1 | 0.01 |
CaO | 17.9 | 0.1 |
P2O5 | 0.2 | 0.5 |
SO3 | 30.6 | 0.1 |
ZnO | - | <0.00003 |
LOI * | 2.9 | 3.3 |
SUM | 100.0 | 100.1 |
AAMs Code | Solids (wt%) | NaOH (mol L−1) | NaOH (wt%) | H2O (wt%) | Na2SiO3 (wt%) | L/S Ratio * | H2O/Na2O ** | SiO2/Na2O ** | |
---|---|---|---|---|---|---|---|---|---|
PLR | MK | ||||||||
PLR50MK50_1 | 25.1 | 25.1 | 6 | 4.9 | 20.0 | 24.9 | 0.81 | 21.4 | 1 |
PLR50MK50_2 | 26.4 | 26.4 | 8 | 5.9 | 18.2 | 23.1 | 0.70 | 17.3 | 1 |
PLR50MK50_3 | 27.1 | 27.1 | 10 | 7.0 | 15.9 | 22.9 | 0.63 | 14.6 | 1 |
PLR70MK30_1 | 34.7 | 14.8 | 6 | 5.0 | 20.3 | 25.2 | 0.83 | 21.4 | 1 |
PLR70MK30_2 | 34.8 | 14.9 | 8 | 6.4 | 18.7 | 25.2 | 0.78 | 17.3 | 1 |
PLR70MK30_3 | 35.7 | 15.3 | 10 | 7.5 | 17.0 | 24.5 | 0.71 | 14.6 | 1 |
Raw Material | Si (mg L−1) | Al (mg L−1) | Si/Al |
---|---|---|---|
PLR | 59.1 | 0.5 | 118.2 |
MK | 61.3 | 43.4 | 1.4 |
AAMs Code | Compressive Strength (MPa) | NaOH (M) | SiO2/Al2O3 | (SiO2 + Al2O3)/Na2O |
---|---|---|---|---|
PLR50MK50 | 25.9 | 10 | 4.1 | 3.6 |
PLR70MK30 | 17.6 | 6.0 | 2.6 |
AAMs Code | Compressive Strength (MPa) | Porosity (%) | Water Absorption (%) | Apparent Density (g cm−3) |
---|---|---|---|---|
PLR50MK50 | 25.9 | 7.0 | 4.2 | 1.7 |
PLR70MK30 | 17.6 | 7.3 | 4.5 | 1.6 |
Durability Test | Period | Compressive Strength (MPa) | Weight Loss (%) | Shrinkage (%) |
---|---|---|---|---|
Control AAMs 1 | - | 25.9 | - | - |
Firing at 200 °C | 2 h | 20.4 | 0.4 | 3.5 |
Firing at 500 °C | 2 h | 5.9 | 4.7 | 6.9 |
Immersion in H2O | 7 days | 21.8 | 0.2 | 3.1 |
Immersion in 1M HCl | 7 days | 12.0 | 0.9 | 4.7 |
Raw Materials | Greek Laterite Leaching Residues (GLR) | Polish Laterite Leaching Residues (PLR) | |
---|---|---|---|
Chemical composition (wt%) | SiO2 | 30.8 | 23.3 |
Al2O3 | 2.3 | 1.2 | |
CaO | 3.7 | 17.9 | |
SO3 | 6.12 | 30.6 | |
Fe2O3 | 50.9 | 9.0 | |
Reactivity (mg L−1) | Si | 20.1 | 59.1 |
Al | 2.4 | 0.5 | |
AAMs | GLR90MK10 | PLR50MK50 | |
Molar ratio in the activating solution | H2O/Na2O | 17.4 | 14.6 |
SiO2/Na2O | 1 | 1 | |
Molar ratio in the reactive paste | (SiO2 + Al2O3)/Na2O | 9.3 | 5.1 |
Fe2O3/CaO | 4.8 | 0.2 | |
Curing Conditions | 80 °C, 24 h, 7 days | 40 °C, 24 h, 7 days | |
L/S ratio | 0.3 | 0.6 | |
Porosity (%) | 21.3 | 7.0 | |
Water Absorption (%) | 5.1 | 4.2 | |
Density (g cm−3) | 2.3 | 1.7 | |
Compressive strength (MPa) | 41 | 26 | |
References | [37] | This study |
Elements | Raw Material | AAMs | Limit Values * | ||
---|---|---|---|---|---|
Leaching Residues (PLR) | PLR50MK50 | For Wastes Accepted at Landfills for Inert Wastes | For Non Hazardous Wastes | For Wastes Accepted at Landfills for Hazardous Wastes | |
mg kg−1 | |||||
Al | 5.4 | 15.7 | - | - | - |
Cr | 0.3 | 0.3 | 0.5 | 10 | 50 |
Mn | 98.2 | 0.2 | - | - | - |
Fe | 7.3 | 29.8 | - | - | - |
Ni | 449.4 | 0.6 | 0.4 | 10 | 40 |
Cu | 0.3 | 0.06 | 2 | 50 | 100 |
Zn | 3.9 | 0.4 | 4 | 50 | 200 |
As | <DL | 0.06 | 0.5 | 2 | 25 |
Mo | 0.7 | 0.05 | 0.5 | 10 | 30 |
Cd | 0.4 | 0.04 | 1 | 5 | |
Pb | 0.6 | 0.01 | 0.5 | 10 | 50 |
SO42− | 800 | 80 | 1000 | 20,000 | 50,000 |
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Karmali, V.; Petrakis, E.; Bartzas, G.; Komnitsas, K. Valorization Potential of Polish Laterite Leaching Residues through Alkali Activation. Minerals 2022, 12, 1466. https://doi.org/10.3390/min12111466
Karmali V, Petrakis E, Bartzas G, Komnitsas K. Valorization Potential of Polish Laterite Leaching Residues through Alkali Activation. Minerals. 2022; 12(11):1466. https://doi.org/10.3390/min12111466
Chicago/Turabian StyleKarmali, Vasiliki, Evangelos Petrakis, Georgios Bartzas, and Konstantinos Komnitsas. 2022. "Valorization Potential of Polish Laterite Leaching Residues through Alkali Activation" Minerals 12, no. 11: 1466. https://doi.org/10.3390/min12111466