Silica pillaring of montmorillonite has been carried out using aminopropylt
riethoxysilane (APTS) as pillaring precursor. Several synthesis parameters,
i.e. reaction temperature, reaction time, concentration of components, etc
., are of importance in this synthesis. However, the concentrations of APTS
and H2O under which the hydrolysis is performed have a paramount effect on
the molecular structure and the degree of polymerization of the pillaring
precursors, and therefore, also on the porosity of the obtained silica inte
rcalated clay. X-ray diffraction (XRD) analysis and diffuse reflectance inf
rared Fourier transform (DRIFT) spectra reveal that the presence of water i
n the system is one of the most important parameters in the reaction sequen
ce. These results are refined and confirmed by transmission electron micros
copy (TEM). Combining the results of all the applied techniques, two types
of APTS interaction with the clay can be observed: internal and external ad
sorption depending on the conditions used. Besides the influence of the wat
er concentration, the influence of the use of templating ions (cetyltrimeth
ylammonium) on the synthesis is also studied. In the case of the templated
approach, in which the alkylammonium ions are pre-adsorbed on the clay prio
r to the pillaring with APTS, a surface area and a pore volume as high as 4
87 g(-1) and 0.45 cm(3) g(-1) have been obtained.