ABSTRACT
This study investigates the production of solketal (2,2-dimethyl-1,3-dioxolane-4-methanol) from glycerol via ketalization reaction using M-ZSM-5 catalysts (M = Fe, Co, Ni, Cu, and Zn). The wet impregnation method ensured precise metal loading and versatility in catalyst preparation. We present a novel approach by employing a suite of characterization techniques, including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET), Thermogravimetric analysis (TGA), and Field-emission scanning electron microscopy (FE-SEM), to elucidate the catalyst's structure, bonding, surface area, thermal stability, and morphology, ultimately linking these properties to their performance. Solketal synthesis was optimized in a reactor, with parameters like temperature, glycerol:acetone molar ratio, catalyst amount, reaction time, and stirring speed. Optimal conditions were identified as 60 °C, 1:4, 0.2 g, 60 min, and 1200 rpm, respectively. Gas chromatography-mass spectrometry (GC-MS) analysis confirmed successful solketal formation. Among M-ZSM-5 catalysts tested, Cu-ZSM-5 emerged the most efficient, achieving an impressive 99% glycerol conversion and 96% solketal selectivity. Notably, Cu-ZSM-5 catalyst displayed exceptional reusability, regaining its initial activity through calcination, thus minimizing waste generation. This research unveils Cu-ZSM-5 as a highly efficient catalyst and promotes sustainability by utilizing a renewable glycerol feedstock to produce valuable solketal with applications in fuel additives, solvents, and pharmaceuticals. This work paves the way for developing environmentally friendly processes for waste valorization and producing valuable bio-based chemicals.
Subject(s)
Glycerol , Zeolites , Zeolites/chemistry , Glycerol/chemistry , Catalysis , Metals/chemistry , Green Chemistry Technology , X-Ray Diffraction , Spectroscopy, Fourier Transform InfraredABSTRACT
Potatoes inoculated with Pectobacterium carotovorum spp., Aspergillus flavus and Aspergillus niger, along with healthy (control) samples, were stored at different storage temperatures (4 ± 1 °C, 8 ± 1 °C, 25 ± 1 °C) for three weeks. Volatile organic compounds (VOCs) were mapped using the headspace gas analysis through solid phase micro extraction-gas chromatography-mass spectroscopy every week. The VOC data were arranged into different groups and classified using principal component analysis (PCA) and partial least square discriminant analysis (PLS-DA) models. Based on a variable importance in projection (VIP) score > 2 and the heat map, prominent VOCs were identified as 1-butanol and 1-hexanol, which can act as biomarkers for Pectobacter related bacterial spoilage during storage of potatoes in different conditions. Meanwhile, hexadecanoic acid and acetic acid were signature VOCs for A. flavus, and hexadecane, undecane, tetracosane, octadecanoic acid, tridecene and undecene were associated with A. niger. The PLS-DA model performed better at classifying the VOCs of the three different species of infection and the control sample compared to PCA, with high values of R2 (96-99%) and Q2 (0.18-0.65). The model was also found to be reliable for predictability during random permutation test-based validation. This approach can be adopted for fast and accurate diagnosis of pathogenic invasion of potatoes during storage.