abstract
A new microporous zirconosilicate K2ZrSi3O9 center dot 2H(2)O (AV-15) has been prepared by high-temperature phase transformation at 910 degrees C. Its structure has been determined ab initio from powder x-ray diffraction data. The unit cell is orthorhombic, space group C222(1) (no. 20), Z=4 with cell dimensions: a=8.105(3), b=10.684(5), c= 12.030(5) angstrom, V=1041.76(7) angstrom(3). The framework connection of AV-15 is essentially the same as the previously reported sodium stannosilicate AV-10 while the locations of potassium and water molecules in the former are quite different from those of the sodium and water molecules in AV-10. In AV-10 sodium and water molecules form a sinucoidal chain, while potassium and water molecules build up a linear chain in AV-15. The water molecules in AV-15 are lost on heating with a typical zeolitic behaviour. SEM shows that the particle sizes and habits of AV-15 and parent umbite material are the same. The Si-29 MAS NMR spectrum of AV-15 displays two resonances at ca. -89.4 and -90.1 ppm in a 1:2 intensity ratio. Thermogravimetry analysis confirms the existence of water in this material. (c) 2010 Elsevier Inc. All rights reserved.
keywords
INITIO STRUCTURE DETERMINATION; POWDER DIFFRACTION DATA; STRUCTURAL-CHARACTERIZATION; AB-INITIO; FRAMEWORK ZIRCONIUM; ION-EXCHANGE; STANNOSILICATE; K2TISI3O9-CENTER-DOT-H2O; TRISILICATE; ZIRCONOSILICATES
subject category
Chemistry
authors
Ferreira, A; Lin, Z; Soares, MR; Rocha, J
our authors
acknowledgements
We greatly appreciate the financial support from FCT, POCI2010, PTDC, FSE, and FEDER.