Catalytic Deactivation of HY Zeolites in the Dehydration of Glycerol to Acrolein

The study of the deactivation of HY zeolites in the dehydration reaction of glycerol to acrolein has represented a challenge for the design of new catalysts. HY zeolites with SiO2/Al2O3 molar ratios between 3.5 and 80 were studied. The solids were characterized by XRD, N2 physisorption, SEM-EDXS, Raman and UV-vis spectroscopies, infrared spectroscopy of pyridine (FTIR-Py) and catalytic activity tests from 250 °C to 325 °C. It was found that the total amount of acid sites per unit area of catalyst decreased as the SiO2/Al2O3 molar ratio increased from 3.5 to 80, resulting in the decrease in the initial glycerol conversion. The initial acrolein selectivity was promoted with the increase of the Brønsted/Lewis acid sites ratio at any reaction temperature. The deactivation tests showed that the catalyst lifetime depended on the pore structure, improving with the presence of large surface areas as evidenced by the deactivation rate constants. The characterization of the deactivated catalysts by XRD, N2 physisorption and thermogravimetric analysis indicated that the deposition of coke resulted in the total obstruction of micropores and the partial blockage of mesopores. Moreover, the presence of large mesopores and surface areas allowed the amount of coke deposited at the catalyst surface to be reduced.

Optimization of Hydrothermal Temperature and Time Parameters in the Synthesis of Hierarchical ZSM-5 from Kaolin by Taguchi Method

Hierarchical ZSM-5 was successfully synthesized by hydrothermal crystallization of kaolin clay. A statistical experimental design Taguchi method with analysis of variance (ANOVA) with an L9 Orthogonal array (OA) was used to optimize the formation of high mesoporosity in hierarchical ZSM-5. Samples from kaolin mixtures crystallized at 80-175°C for 12, 24 and 48 h, respectively using hydrothermal followed by addition of mesoporogen cetyltrimethylammonium bromide (CTABr) surfactant. The presence of pentasil zeolite groups and large mesopores surface area and pore volume has observed on the samples by FTIR and N2 adsorption-desorption technique.The optimum synthesis conditions studied by Taguchi analysis based on S/N ratio for temperature and time of hydrothermal. The optimum condition was 127.5°C and 48 h giving the highest mesoporosity. Data analysis of interaction plot for S/N ratio showed there was interaction between temperature and time in the crystallization of hierarchical ZSM-5. Hydrothermal temperature was the most influencing factors for the formation of hierarchical ZSM-5 with a percent contribution of 83%.

Preparation of periodic mesoporous organosilica with large mesopores using silica colloidal crystals as templates

Periodic mesoporous organosilicas with precisely controlled pore sizes (>10 nm) were prepared using silica colloidal crystals as a template.