Thermogravimetric analysis of layered double hydroxides intercalated with sulfate and alkaline cations [M62+Al3(OH)18][A+(SO4)2] 12H2O (M2+ = Mn, Mg, Zn; A+ = Li, Na, K)

The synthesized phases with chemical composition M 6 2 + Al 3 OH 18 A + SO 4 2 12 H 2 O (M 2+  = Mn, Mg, Zn; A +  = Li, Na or K) were evaluated in relation to their thermal behavior by thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). In th...

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Bibliographic Details
Published in:Journal of thermal analysis and calorimetry 2020, Vol.140 (4), p.1715-1723
Main Authors: Sotiles, Anne Raquel, Gomez, Neffer Arvey Gomez, Wypych, Fernando
Format: Article
Language:English
Subjects:
Amorphous materials
Analytical Chemistry
Chemical composition
Chemical synthesis
Chemistry
Chemistry and Materials Science
Dehydration
Fourier transforms
Heat treatment
Hydroxides
Infrared analysis
Infrared spectroscopy
Inorganic Chemistry
Magnesium
Manganese
Measurement Science and Instrumentation
Phases
Physical Chemistry
Polymer Sciences
Sodium
Spinel
Thermodynamic properties
Thermogravimetric analysis
X-ray diffraction
Zinc
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Summary:The synthesized phases with chemical composition M 6 2 + Al 3 OH 18 A + SO 4 2 12 H 2 O (M 2+  = Mn, Mg, Zn; A +  = Li, Na or K) were evaluated in relation to their thermal behavior by thermogravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). In the shigaite (M 2+  = Mn), natroglaucocerinite (M 2+  = Zn) and motukoreaite (M 2+  = Mg) phases, the TGA measurements indicated that all samples were dehydrated up to 200 °C in two steps, followed by dehydroxylation above 300 °C. After the thermal treatment at 1000 °C, formation of oxides/spinels were observed for the shigaite and natroglaucocerinite phases, while for motukoreaite, oxides, spinels and MgSO 4 were detected. XRD indicated a reduction in the basal distance from around 11 Å for the fully hydrated phases to around 7 Å for the dehydrated phases. The thermal treatments of some samples at 100 °C, 150 °C and 200 °C indicated that in all phases, intercalated sulfate and alkaline metal ions can be dehydrated and rehydrated. As indicated by FTIR, at 200 °C sulfate could be grafted to the layers and at 300 °C, for all the phases, a stable mixture of amorphous materials was obtained, which could not be rehydrated. Graphic abstract
ISSN:1388-6150
1588-2926
DOI:10.1007/s10973-019-08955-6