Characterization of Waste Sludge Pigment from Production of ZnCl2
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Sample Preparation
2.3. Characterization Techniques
- Chemical composition of raw materials was determined using energy dispersive fluorescence spectrometer SPECTRO XEPO (SPECTRO Analytical Instruments GmbH, Kleve, Germany), equipped with 50 Watt Pd X-ray tube.
- The phase composition of samples was characterized using a Bruker D8 Advance X-ray powder diffractometer (Bruker AXS GmbH, Karlsruhe, Germany). The diffraction patterns in the range of 5° to 70° 2θ were recorded under CoKα (λ = 1.78897 Å, U = 35 kV, I = 25 mA) irradiation with scanning rate 2°/min using fast position-sensitive detector VÅNTEC1.
- The morphology of the particles was characterized using the scanning electron microscope (SEM) QUANTA 450 FEG, (FEI, Hillsboro, OR, USA); the images were collected using a secondary electron detector.
- The particle size distribution (PSD) was analyzed using Mastersizer (Malvern Panalytical Ltd., Malvern, UK). Measurements were performed in an aquatic environment, and ultrasound was used for homogenization of the suspension.
- The characterization of the thermal behavior was performed on TG/DTAanalyzer STA504 (TA Instruments, New Castle, Delaware, USA). The sample of scale placed in alumina crucible was analyzed in a temperature range from 21 to 1100 °C in the dynamic atmosphere of N2 (5 L⋅h−1), and the heating rate was 10 K·min−1.
- The reflectance spectra of the final glazes in the spectral range 400–700 nm were obtained using MiniScan EZ0828 spectrometer (HunterLab, Reston, VA, USA), model 45°/0°, small observation area. The color of the glazes was expressed using CIE L*a*b* coordinates calculated for 10° observer and D65 illuminant.
- Specific surface area was determined by BET method-equipment (Quantachrome NovaWin Instrument-Acquisition and Reduction for NOVA instrument, analysis gas nitrogen, Graz, Austria).
- Density of samples was determined by Pycnomatic and Pycnomatic ATC (Helium pycnometer) POROTEC GmbH, Coconut Creek, FL, USA.
3. Results and Discussion
3.1. Chemical Composition
3.2. Phase Composition of Commercial Pigments
3.3. Granulometry of Commercial Pigments
3.4. SEM Analysis of Commercial Pigments
3.5. The Treatment of Waste Fe Sludge
- WFS/0—Waste Fe sludge washed by H2O by 1 L H2O/300 g of WFS,
- WFS/180—Waste Fe sludge washed by H2O by 1 L H2O/300 g of WFS and calcined at 180 °C at the mode of 15 °C/min for 10 h/180 °C, and
- WFS/900—Waste Fe sludge washed by H2O by 1 L H2O/300 g of WFS and calcined at 900 °C at the mode of 15 °C/min for 3 h/900 °C.
3.6. Granulometry of Waste Fe Sludge
3.7. SEM Analysis of Waste Fe Sludge
3.8. Phase Analysis of Waste Fe Sludge
3.9. TG and DTA of Waste Fe Sludge
3.10. Color of Glaze
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Recipe | Samples | Amount of the Materials (wt.%) | ||||||
---|---|---|---|---|---|---|---|---|
Transparent Glaze (TG) | Waste Fe Sludge (WFS) | Standard Pigments (SP) | ||||||
WFS/0 | WFS/180 | WFS/900 | SP1 | SP2 | SP3 | |||
R1 | GP01 | 99 | 1 | |||||
GP02 | 95 | 5 | ||||||
GP03 | 90 | 10 | ||||||
GP04 | 85 | 15 | ||||||
GPX | 90 | 10 | ||||||
GOKP | 90 | 10 | ||||||
R2 | GPF1 | 90 | 10 | |||||
GPF2 | 90 | 10 | ||||||
GPF3 | 90 | 10 |
Amount of Oxides in Raw Materials (wt.%) | ||||||||
---|---|---|---|---|---|---|---|---|
Oxides | Ceramic Slurry (CS) | Waste Fe Sludge(WFS) | Waste Fe Sludge (WFS/0) | Waste Fe Sludge (WFS/180) | Transparent Glaze (TG) | SP3 (Dark Brown) | SP2 (Light Brown) | SP1 (Red) |
Na2O | 1.22 | 5.61 | 4.61 | 5.50 | ||||
MgO | 2.83 | 1.12 | 0.18 | <0.3 | 0.58 | 0.44 | <0.001 | |
Al2O3 | 12.42 | 0.20 | 0.74 | 0.49 | 9.10 | <0.001 | 0.44 | <0.001 |
SiO2 | 69.57 | 80.10 | 0.16 | 0.80 | <0.001 | |||
P2O5 | <0.0012 | 0.06 | 0.16 | <0.01 | 0.022 | 0.073 | <0.001 | |
SO3 | 0.19 | 0.15 | 0.19 | 0.71 | 0.12 | 0.27 | 0.33 | 0.20 |
K2O | 2.08 | 0.88 | <0.001 | <0.001 | <0.001 | |||
CaO | 4.52 | 0.02 | <0.001 | 0.30 | 0.05 | 0.31 | 0.01 | |
TiO2 | 0.56 | <0.001 | 0.13 | 0.67 | 0.59 | 1.311 | ||
MnO | 0.07 | <0.001 | 0.006 | 1.06 | 0.75 | 0.13 | ||
Fe2O3 | 4.09 | 40.92 | 90.09 | 97.56 | 0.22 | 96.97 | 95.22 | 97.807 |
BaO | 0.05 | 0.05 | ||||||
Cl | 22.08 | 2.47 | 0.49 | 0.006 | 0.017 | <0.001 | ||
ZnO | 29.87 | 1.52 | 0.24 | 0.15 | 0.13 | 0.03 | ||
PbO | 0.05 | 0.12 | <0.001 | |||||
V2O5 | <0.001 | 0.03 | <0.001 | |||||
Cr2O3 | 0.14 | <0.001 | 0.12 | <0.001 | ||||
NiO | 0.028 | 0.10 | <0.001 | |||||
CuO | <0.001 | 0.047 | <0.001 |
Samples | CIE Values | ||
---|---|---|---|
L* | a* | b* | |
GPO1 | 82.04 | 6.28 | 17.85 |
GPO2 | 31.48 | 6.97 | 16.57 |
GPO3 | 21.28 | 12.23 | 9.71 |
GPX | 16.98 | 17.69 | 10.93 |
GOKP | 27.95 | 6.36 | 25.84 |
GPF1 | 23.44 | 25.41 | 18.88 |
GPF2 | 20.23 | 21.27 | 15.72 |
GPF3 | 18.29 | 20.27 | 16.45 |
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Ovčačíková, H.; Velička, M.; Maierová, P.; Vlček, J.; Tokarský, J.; Čegan, T. Characterization of Waste Sludge Pigment from Production of ZnCl2. Minerals 2021, 11, 313. https://doi.org/10.3390/min11030313
Ovčačíková H, Velička M, Maierová P, Vlček J, Tokarský J, Čegan T. Characterization of Waste Sludge Pigment from Production of ZnCl2. Minerals. 2021; 11(3):313. https://doi.org/10.3390/min11030313
Chicago/Turabian StyleOvčačíková, Hana, Marek Velička, Petra Maierová, Jozef Vlček, Jonáš Tokarský, and Tomáš Čegan. 2021. "Characterization of Waste Sludge Pigment from Production of ZnCl2" Minerals 11, no. 3: 313. https://doi.org/10.3390/min11030313