Pöppl L., Tóth E., Tóth M., Paszli I., Izvekov
V., Gábor M. (1998): Synthesis and characterizations of hydroxy-aluminum
cross-linked montmorillonite J.Therm Anal.Calorim Vol 53, 2, pp 585-596
Abstract:
Cross-linked montmorillonite was prepared by reacting homoionic sodium
form of bentonite (Na-M) from Istenmezeje (Hungary) with high molecular
weight polyhydroxy-aluminum complex. The complex was prepared by controlled
hydrolysis of alumina macrocation. The intercalated clay (Na-Al-M) was
thermally treated to convert the hydroxy cations to oxide pillars. The
pillared products were characterized by X-ray powder diffraction (XRD),
Fourie transform infrared spectroscopy (FTIR), thermogravimetry (TG), differential
thermal analysis (DTA) and thermal analysis-mass spectrometry (TA-MS) methods.
The specific surface area as well as pore size and pore structure distribution
of samples were measured by nitrogen, water and carbon tetrachloride adsorption,
and the heat of immersion was also determined. The pillared products were
haracterized by d(001) reflections of 19 Angstrom, which is stable even
at 500 degrees C. The
interaction of polymer alumina caused several changes in the obtained
FTIR spectra due to the formation of different new bonds. The rate of dehydroxylation
of the pillared product is very moderate, the water release occurred in
different temperature ranges according to TA-MS results. Dehydration starts
at interfaces and at the wall of pores, occurring nearly with uniform rate
at 250-500 degrees C. DTA curve indicates the formation of a new phase
at 950 degrees C. The obtained surface area of the pillared product by
nitrogen adsorption becomes larger (208 m(2) g(-1)) with respect to the
non pillared clay, which decreases less than 10% upto 700 degrees C. The
pillared sample has a definite pore structure, the quantity of micropores
(0-40 Angstrom) decreased with increasing of macropores (>1000 Angstrom).
The obtained domestic pillared montmorillonite possesses a high degree
of thermal stability and may be used as adsorbent.
Author Keywords:
DTA, FTIR, Keggin ion, pillared montmorillonite, pore structure, TA-MS,
XRD
KeyWords Plus:
PILLARED MONTMORILLONITE, WATER-ADSORPTION, CLAY, SMECTITES, COMPLEXES