Optimizing the Surface Properties of MgO Nanoparticles Towards the Transesterification of Glycerol to Glycerol Carbonate

Abstract

MgO nanoparticles (NPs) were successfully fabricated by a facile, inexpensive and green synthesis protocol using soluble starch as a green bio-template. The influence of calcination temperature on its textural properties and catalytic efficiency has been investigated in detail. The enhancement of MgO NPs crystallinity by increasing the calcination temperature is found from X-ray diffraction (XRD) and Transmission electron microscopy (TEM) analyses. N 2 -sorption studies and CO 2 -temperature programmed desorption (TPD) measurements revealed that the MgO NPs calcined at 500°C have superior textural properties and strong surface basicity. X-ray photoelectron spectroscopy (XPS) analysis conferred that the MgO-500 NPs furnished the optimized surface Lewis sites, consequently outperforms better transesterification activity. The fabricated MgO-500 NPs exhibited an excellent catalytic activity towards the efficient conversion of glycerol to glycerol carbonate (GC) with more than 93% selectivity. The intelligibility of the adopted synthesis is eco-benign and wide utility as a solid base catalyst for several organic transformations.

Highly Active and Recyclable CuxFe3‐xO4 NPs for Selective Oxidation of Benzyl Alcohol using TBHP as an Oxidant

“…The product samples have been collected at regular intervals and analyzed by Shimadzu GC 2014 gas chromatography with a flame ionization detector (FID), equipped with SH-Rxi-5Sil MS capillary column (30m × 0.25mm × 0.25 μm). [38] The formation of the product was also identified by 1 H-NMR analysis (Figure S2, SI). After completion of the reaction, the reaction mixture is applied to the external magnetic field to separate the product and catalyst.…”

“…Then, 50 mg of catalyst was introduced to the reaction mixture, and then the temperature is raised to 110 °C. The product samples have been collected at regular intervals and analyzed by Shimadzu GC 2014 gas chromatography with a flame ionization detector (FID), equipped with SH‐Rxi‐5Sil MS capillary column (30m×0.25mm×0.25 μm) [38] . The formation of the product was also identified by 1 H‐NMR analysis (Figure S2, SI).…”

“…[37] The Cu 2p core level binding energy at 933.4 eV and the presence of satellite peaks observed at 940.8 and 943.1 eV further substantiate the oxide nature of Cu species. [37] Furthermore, the deconvoluted O 1s features at 530.3 and two more peaks at 528 eV and 532.2 eV correspond to the presence of hydroxyl and oxide species, [38] respectively. The XPS core levels of Fe 2p (709.8 eV), Cu 2p (933.4 eV), and O 1s (530.3 eV) are highly consistent with ferrite-type materials, and the observed satellite peaks for both Fe 2p and Cu 2p levels further substantiated that the oxide form of ferrites.…”

Recent Advances in Glycerol Catalytic Valorization: A Review

“…Indirect routes normally lead to a higher yield of glycerol carbonate, where the catalysts play a key role. Starting with glycerol transesterification, some reviews have summarized the types of catalysts [207,211], which are very similar to other transesterification processes, including K 2 CO 3 , CaO, MgO [213], ZnO, and H 2 SO 4 . Several types of hydrotalcite have been tested, such as Al/Mg, Al/Li, Al/Ca, Mg/Al, etc.…”

Transesterification of Glycerol to Glycerol Carbonate over Mg-Zr Composite Oxide Prepared by Hydrothermal Process

“…In recent years, alkali catalysts such as MgO [15,16] and CaO [17] have been widely used in GC synthesis by transesterification. However, CaO can be dissolved into the reactant GL and form a calcium-glycerin bond [18].…”