Novel microporous zirconium silicate (K{sub 2}ZrSi{sub 3}O{sub 9}.2H{sub 2}O) from high temperature phase transformation

Journal Article · Wed Dec 15 00:00:00 EST 2010 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2010.10.013· OSTI ID:21494163

Ferreira, Artur ^[1]; Soares, Maria R ^[2]; Rocha, Joao ^[3]

---

1. ESTGA, CICECO, University of Aveiro, Apartado 473, 3754-909 Agueda (Portugal)
2. Central Laboratory of Analyses, CICECO, University of Aveiro, 3810-193 Aveiro (Portugal)
3. Department of Chemistry, CICECO, University of Aveiro, 3810-193 Aveiro (Portugal)

A new microporous zirconosilicate K{sub 2}ZrSi{sub 3}O{sub 9}.2H{sub 2}O (AV-15) has been prepared by high-temperature phase transformation at 910 {sup o}C. Its structure has been determined ab initio from powder X-ray diffraction data. The unit cell is orthorhombic, space group C222{sub 1} (no. 20), Z=4 with cell dimensions: a=8.105(3), b=10.684(5), c=12.030(5) A, V=1041.76(7) A{sup 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 {sup 29}Si 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. -- Graphical abstract: A new microporous zirconosilicate has been prepared by high temperature phase transformation at 910 {sup o}C. Its structure has been determined ab initio from powder X-ray diffraction data. The water molecules in this material are lost below 125 {sup o}C in a way typical of zeolites and molecular sieves. Display Omitted

• OSTI ID: 21494163
• Journal Information: Journal of Solid State Chemistry, Vol. 183, Issue 12; Other Information: DOI: 10.1016/j.jssc.2010.10.013; PII: S0022-4596(10)00467-6; Copyright (c) 2010 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
HEATING
LATTICE PARAMETERS
MOLECULAR SIEVES
NMR SPECTRA
ORTHORHOMBIC LATTICES
PARTICLE SIZE
PHASE TRANSFORMATIONS
POTASSIUM COMPOUNDS
SCANNING ELECTRON MICROSCOPY
SPACE GROUPS
TEMPERATURE RANGE 1000-4000 K
THERMAL GRAVIMETRIC ANALYSIS
WATER
X-RAY DIFFRACTION
ZEOLITES
ZIRCONIUM SILICATES
ADSORBENTS
ALKALI METAL COMPOUNDS
CHEMICAL ANALYSIS
COHERENT SCATTERING
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DIFFRACTION
ELECTRON MICROSCOPY
GRAVIMETRIC ANALYSIS
HYDROGEN COMPOUNDS
INORGANIC ION EXCHANGERS
ION EXCHANGE MATERIALS
MATERIALS
MICROSCOPY
MINERALS
OXYGEN COMPOUNDS
QUANTITATIVE CHEMICAL ANALYSIS
SCATTERING
SILICATE MINERALS
SILICATES
SILICON COMPOUNDS
SIZE
SPECTRA
SYMMETRY GROUPS
TEMPERATURE RANGE
THERMAL ANALYSIS
TRANSITION ELEMENT COMPOUNDS
ZIRCONIUM COMPOUNDS