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Synthesis of hydroxy-sodalite/cancrinite zeolites from calcite-bearing kaolin for the removal of heavy metal ions in aqueous media

2019, Esaifan, Muayad, Warr, Laurence N., Gratho, Georg, Meyer, Tammo, Schafmeister, Maria-Theresia, Kruth, Angela, Testrich, Holger

A hydroxy-sodalite/cancrinite zeolite composite was synthesized from low-grade calcite-bearing kaolin by hydrothermal alkali-activation method at 160 °C for 6 h. The effect of calcite addition on the formation of the hydroxy-sodalite/cancrinite composite was investigated using artificial mixtures. The chemical composition and crystal morphology of the synthesized zeolite composite were characterized by X-ray powder diffraction, infrared spectroscopy, scanning electron microscopy, and N2 adsorption/desorption analyses. The average specific surface area is around 17–20 m2·g−1, whereas the average pore size lies in the mesoporous range (19–21 nm). The synthesized zeolite composite was used as an adsorbent for the removal of heavy metals in aqueous solutions. Batch experiments were employed to study the influence of adsorbent dosage on heavy metal removal efficiency. Results demonstrate the effective removal of significant quantities of Cu, Pb, Ni, and Zn from aqueous media. A comparative study of synthesized hydroxy-sodalite and hydroxy-sodalite/cancrinite composites revealed the latter was 16–24% more efficient at removing heavy metals from water. The order of metal uptake efficiency for these zeolites was determined to be Pb > Cu > Zn > Ni. These results indicate that zeolite composites synthesized from natural calcite-bearing kaolin materials could represent effective and low-cost adsorbents for heavy metal removal using water treatment devices in regions of water shortage.

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Plasma Spraying of Kaolinite for Preparing Reactive Alumino-Silicate Glass Coatings

2022, Warr, Laurence N., Wolff, Thorben, Testrich, Holger, Grathoff, Georg, Kruth, Angela, Foest, Rüdiger

Thermally treated kaolinite is used to develop a range of alumino-silicate-based precursor materials but its behavior during plasma spraying has not been well-researched. In this study, two types of kaolinite samples were investigated in the form of low defect (KGa-1b) and high defect (KGa-2) varieties. The extreme temperatures of the plasma stream (up to 20 000 K) induced flash melting to produce a highly porous alumino-silicate glass without any crystallization of new Al−Si oxide minerals. The glass is comprised largely of intact or deformed spheres (average diameters 1.14–1.44 μm), which indicates rapid quenching and solidification before impact. The subspherical structures contain up to 40 % closed pore space caused by the rapid escape of water during melting. The low-density, porous alumino-silicate glass coatings with predicted specific surface areas (>0.95 m2/g) and hardnesses >1.8 GPa represent a potentially reactive but physically stable substrate ideal for further chemical functionalization.

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Porosity and distribution of water in perlite from the island of Milos, Greece

2014, Kaufhold, Stephan, Reese, Anke, Schwiebacher, Werner, Dohrmann, Reiner, Grathoff, Georg H., Warr, Laurence N., Halisch, Matthias, Müller, Cornelia, Schwarz-Schampera, Ulrich, Ufer, Kristian

A perlite sample representative of an operating mine in Milos was investigated with respect to the type and spatial distribution of water. A set of different methods was used which finally provided a consistent view on the water at least in this perlite. Infrared spectroscopy showed the presence of different water species (molecular water and hydroxyl groups / strongly bound water). The presence of more than 0.5 mass% smectite, however, could be excluded considering the cation exchange capacity results. The dehydration measured by thermal analysis occurred over a wide range of temperatures hence confirming the infrared spectroscopical results. Both methods point to the existence of a continuous spectrum of water binding energies. The spatial distribution of water and/or pores was investigated using different methods (CT: computer tomography, FIB: scanning electron microscopy including focused ion beam technology, IRM: infrared microscopy). Computer tomography (CT) showed large macropores (20 – 100 μm) and additionally revealed a mottled microstructure of the silicate matrix with low density areas up to a few μm in diameter. Scanning electron microscopy (FIB) confirmed the presence of μm sized pores and IRM showed the filling of these pores with water. In summary, two types of pores were found. Airfilled 20 – 100 μm pores and μm-sized pores disseminated in the glass matrix containing at least some water. Porosity measurements indicate a total porosity of 26 Vol%, 11 Vol% corresponding to the μm-sized pores. It remains unsolved wether the water in the μm-sized pores entered after or throughout perlite formation. However, the pores are sealed and no indications of cracks were found which indicated a primary source of the water, i.e. water was probably entrapped by quenching of the lava. The water in these pores may be the main reason for the thermal expandability which results in the extraordinarily porous expanded perlite building materials.