Details
| Original language | English |
|---|---|
| Pages (from-to) | 347-358 |
| Number of pages | 12 |
| Journal | Microporous and Mesoporous Materials |
| Volume | 30 |
| Issue number | 2-3 |
| Early online date | 8 Jul 1999 |
| Publication status | Published - Sept 1999 |
Abstract
The synthesis of cancrinite in the system Na2O-SiO2-Al2O3-Na 2CO3-H2O was studied under low-temperature hydrothermal conditions in the 353K<T<473K interval. The aim was to reveal the suitable range for the crystallization of pure-phase carbonate cancrinite with the ideal composition Na8[AlSiO4]6CO3(H2O) 2 without cocrystallization of sodalite or intermediate disordered phases between cancrinite and sodalite. It was found that cancrinite formation reacts very sensitive on the temperature within the autoclaves whereas the concentration of reactants and the alkalinity of the hydrothermal solution have a much lower influence on the phase formation. Thus the temperature of crystallization of carbonate cancrinite without any by-products should not remain below 473K. At the lower reaction temperature of 353K the formation of a disordered intermediate phase between the cancrinite and the sodalite structure has been obtained in every case, independent of the template concentrations and the base. Some problems to detect this in a typical powder product mixture are discussed. Besides the 29Si and 27Al MAS NMR characterization of the products, the crystal structure refinement of pure carbonate cancrinite of ideal composition Na8[AlSiO4]6CO3(H2O) 3.4, has been carried out from X-ray powder data using the Rietveld method: P63, a=1271.3(1)pm, c=518.6(1)pm, RWP=0.073, RF=0.016 for 347 structure factors and 45 variable positional parameters.
Keywords
- Carbonate-cancrinite, Crystal structure, Identification, MAS NMR, Synthesis
ASJC Scopus subject areas
- Chemistry(all)
- General Chemistry
- Materials Science(all)
- General Materials Science
- Physics and Astronomy(all)
- Condensed Matter Physics
- Engineering(all)
- Mechanics of Materials
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In: Microporous and Mesoporous Materials, Vol. 30, No. 2-3, 09.1999, p. 347-358.
Research output: Contribution to journal › Article › Research › peer review
}
TY - JOUR
T1 - Synthesis and crystal structure of carbonate cancrinite Na8[AlSiO4]6CO3(H2O) 3.4, grown under low-temperature hydrothermal conditions
AU - Hackbarth, K.
AU - Gesing, Th M.
AU - Fechtelkord, M.
AU - Stief, F.
AU - Buhl, J. Ch
N1 - Funding Information: We thank Dr. W. Lutz (WITEGA GmbH, Berlin) for the water sorption measurements. This work was supported by Deutsche Forschungsgemeinschaft.
PY - 1999/9
Y1 - 1999/9
N2 - The synthesis of cancrinite in the system Na2O-SiO2-Al2O3-Na 2CO3-H2O was studied under low-temperature hydrothermal conditions in the 353K8[AlSiO4]6CO3(H2O) 2 without cocrystallization of sodalite or intermediate disordered phases between cancrinite and sodalite. It was found that cancrinite formation reacts very sensitive on the temperature within the autoclaves whereas the concentration of reactants and the alkalinity of the hydrothermal solution have a much lower influence on the phase formation. Thus the temperature of crystallization of carbonate cancrinite without any by-products should not remain below 473K. At the lower reaction temperature of 353K the formation of a disordered intermediate phase between the cancrinite and the sodalite structure has been obtained in every case, independent of the template concentrations and the base. Some problems to detect this in a typical powder product mixture are discussed. Besides the 29Si and 27Al MAS NMR characterization of the products, the crystal structure refinement of pure carbonate cancrinite of ideal composition Na8[AlSiO4]6CO3(H2O) 3.4, has been carried out from X-ray powder data using the Rietveld method: P63, a=1271.3(1)pm, c=518.6(1)pm, RWP=0.073, RF=0.016 for 347 structure factors and 45 variable positional parameters.
AB - The synthesis of cancrinite in the system Na2O-SiO2-Al2O3-Na 2CO3-H2O was studied under low-temperature hydrothermal conditions in the 353K8[AlSiO4]6CO3(H2O) 2 without cocrystallization of sodalite or intermediate disordered phases between cancrinite and sodalite. It was found that cancrinite formation reacts very sensitive on the temperature within the autoclaves whereas the concentration of reactants and the alkalinity of the hydrothermal solution have a much lower influence on the phase formation. Thus the temperature of crystallization of carbonate cancrinite without any by-products should not remain below 473K. At the lower reaction temperature of 353K the formation of a disordered intermediate phase between the cancrinite and the sodalite structure has been obtained in every case, independent of the template concentrations and the base. Some problems to detect this in a typical powder product mixture are discussed. Besides the 29Si and 27Al MAS NMR characterization of the products, the crystal structure refinement of pure carbonate cancrinite of ideal composition Na8[AlSiO4]6CO3(H2O) 3.4, has been carried out from X-ray powder data using the Rietveld method: P63, a=1271.3(1)pm, c=518.6(1)pm, RWP=0.073, RF=0.016 for 347 structure factors and 45 variable positional parameters.
KW - Carbonate-cancrinite
KW - Crystal structure
KW - Identification
KW - MAS NMR
KW - Synthesis
UR - http://www.scopus.com/inward/record.url?scp=0032681709&partnerID=8YFLogxK
U2 - 10.1016/S1387-1811(99)00046-3
DO - 10.1016/S1387-1811(99)00046-3
M3 - Article
AN - SCOPUS:0032681709
VL - 30
SP - 347
EP - 358
JO - Microporous and Mesoporous Materials
JF - Microporous and Mesoporous Materials
SN - 1387-1811
IS - 2-3
ER -