Facile ultrasound-assisted grafting of silica gel by aminopropyltriethoxysilane for aldol condensation of furfural and acetone

This work focuses on the development of a simple method to prepare heterogeneous catalysts with tunable basicity and stability for aldol condensation of furfural and acetone. Silica gel was grafted by aminopropyltriethoxysilane (APTES) with 20, 30, 40 and 50 wt. % of APTES using probe-type ultrasonicator with a power of 130 W and a frequency of 20 kHz. The grafted samples were studied by XRD, SEM, N₂ sorption, FTIR, XPS, CHN and TG analysis, and CO₂-TPD. The sonication facilitated the bond formation between APTES and the silica gel with less pore blocking than the conventional grafting method. The basicity of the samples was tunable with the quantity of APTES loading. The grafted samples were active catalysts for aldol condensation between furfural and acetone at 60 °C. The catalyst with 30 wt. % APTES grafting (30APS-U) provided a nearly complete furfural conversion and high furfurylbutenone selectivity. The conversion and selectivity increased with time and reached the highest values at 24 h. Thus, the catalysts with tunable basicity prepared by ultrasound-assisted grafting of silica with various APTES amounts were effective in furfural valorization.     

Suitability of commercial colloids for magnetic hyperthermia

Commercial nanoparticles supplied by Chemicell, Micromod and Bayer-Schering were characterised with regard to their nanocrystalline diameter, hydrodynamic diameter, total iron content and relative ferrous iron content. Additionally, calorimetric measurements were taken using a 900 kHz AC magnetic field of amplitude 5.66 kA/m. It was found that those samples containing relatively high (>18%) ferrous content generated a substantially smaller (12% on average) intrinsic loss power (ILP) than those samples with a lower ferrous content. Two nominally identical Chemicell samples that differed only in their production date showed significantly different ILPs, attributed to a variation in batch-to-batch crystallite sizes. The highest ILP values in the cohort, ca. 3.1 nHm²/kg, were achieved for particles with hydrodynamic diameters of ca. 70 nm and nanocrystalline diameters of ca. 12 nm. These compare favourably with most samples prepared in academic laboratories, although they are not as high as the ca. 23.4 nHm²/kg reported for naturally occurring bacterial magnetosomes.