RESUMO
The [CTA]-MCM-41 hybrid silica is a useful and simply prepared heterogeneous basic catalyst for the transesterification reaction. Here, the effect of hydrothermal treatment during catalyst preparation was investigated, with the aim of improving the structural stability of this catalyst during the reaction. It was observed that the hydrothermal step led to the formation of a material with a higher degree of organization and a greater wall thickness, which improved its structural stability. However, the catalyst prepared using this treatment presented lower catalytic activity, due to the presence of fewer active sites.
RESUMO
Special preparation of Santa Barbara Amorphous (SBA)-15, mesoporous silica with highly hexagonal ordered, these materials have been carried out for creating adsorbents exhibiting an enhanced and partially selective adsorption toward CO2. This creation starts from an adequate conditioning of the silica surface, via a thermo-alkaline treatment to increase the population of silanol species on it. CO2 adsorption is only reasonably achieved when the SiO2 surface becomes aminated after put in contact with a solution of an amino alkoxide compound in the right solvent. Unfunctionalized and amine-functionalized substrates were characterized through X-ray diffraction, N2 sorption, Raman spectroscopy, electron microscopy, 29Si solid-state Nuclear Magnetic Resonance (NMR), and NH3 thermal programmed desorption. These analyses proved that the thermo-alkaline procedure desilicates the substrate and eliminates the micropores (without affecting the SBA-15 capillaries), present in the original solid. NMR analysis confirms that the hydroxylated solid anchors more amino functionalizing molecules than the unhydroxylated material. The SBA-15 sample subjected to hydroxylation and amino-functionalization displays a high enthalpy of interaction, a reason why this solid is suitable for a strong deposition of CO2 but with the possibility of observing a low-pressure hysteresis phenomenon. Contrastingly, CH4 adsorption on amino-functionalized, hydroxylated SBA-15 substrates becomes almost five times lower than the CO2 one, thus giving proof of their selectivity toward CO2. Although the amount of retained CO2 is not yet similar to or higher than those determined in other investigations, the methodology herein described is still susceptible to optimization.
RESUMO
Polypropylene composites with different filler contents were prepared by creating a masterbatch containing 3 wt%. filler. A variety of silanol groups were used to synthetized three compounds in different media trough a sol-gel process with acetic acid, formic acid and ammonium hydroxide as catalysts. Besides, four different nanotubular fillers were also used to analyze their behavior and compare it with the effect caused by the silanol groups. These tubular structures comprise: unmodified halloysite, carbon nanotubes and functionalized halloysite and carbon nanotubes. Morphological characterization in SEM and STEM/TEM showed dispersion in the polypropylene matrix. According to TGA and DSC measurements thermal behavior remain similar for all the composites. Mechanical test in tension demonstrate that modulus of the composites increases for all samples with a major impact for materials containing silanol groups synthetized in formic acid. Rheological measurements show a significantly increment in viscosity for samples containing unmodified and modified carbon nanotubes. No difference was found for samples containing silanol groups and halloysite when compared to neat polypropylene. Finally, the oxygen transmission rate increased for all samples showing high barrier properties only for samples containing natural and functionalized halloysite nanotubes.