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Research data supporting Microwave-assisted valorization of glycerol to solketal using biomass-derived heterogeneous catalyst


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Research data supporting the full paper entitled "Microwave-assisted valorization of glycerol to solketal using biomass-derived heterogeneous catalyst " by S. Ao et al. in Fuel, 2023, 345, 128190. A heterogeneous biomass-based carbonaceous solid acid catalyst (SAFACAM) whose preparation we reported in https://doi.org/10.1016/j.renene.2021.12.001 was used multiple times in the production of solketal. The following supporting data are deposited here: X-ray powder diffraction (XRD) used a PANalytical X’Pert Pro diffractometer (Cu Kα radiation, 2theta = 10-60°, 100 mA current and 40 kV operating voltage). Brunauer-Emmet-Teller (BET) analysis used a Micromeritics ASAP 2010 surface area and porosity analyzer after sample degassing for 10 h and 150 °C. Thermogravimetric analysis (TGA) and derivative thermogravimetry (DTG) used a Metter Toledo TGA/DSC 1. Heating rate 10 °C min–1 and constant N2 flow in the range 50-600 °C. FT-IR analysis was by Nicolet iS50 spectrometer (Thermofisher). Solid-state magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy used a Bruker AVANCE 400 MHz (9.4 T) instrument with a 4 mm double resonance probe. 1H-13C cross-polarization (CP) used 100 kHz 1H broadband SPINAL64, at 10 kHz MAS, 4 ms CP contact time (75 kHz ramped 1H, 65 kHz square 13C contact pulses), and a 2 s recycle delay. Shifts were referenced externally against the methylene 13C signal of glycine (43.1 ppm). 20 Hz exponential line broadening was applied when processing. Experiments used Bruker TopSpin 2.1. The catalyst was used to prepare solketal. Product analysis used an Agilent 7890 runing in head-space injector mode, and using a CPSIL 8CB capillary column (30 m × 0.25 mm × 0.25 μm) and a GC FID detector. Oven temperature was increased from 55 °C to 230 °C at 10 °C min–1. The temperature of the detector and the injector were 300 °C and 250 °C, respectively. Dimethyl sulfoxide internal standard. A Shimadzu QP 2010 Ultra mass spectrometer was used in HRMS. 1H and 1H 13C NMR spectra were obtained on a Bruker Avance II 500 MHz spectrometer. Deuterated solvent was stored over molecular sieves (3 Å). Chemical shifts were internally referenced to the deuterated solvent. Data collected at 28 °C.

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Bruker TopSpin 2.1 (www.bruker.com) or Mestrec MNova (www.mestrelab.com) Origin Pro 8.0 MS Excel 2016 MS Wordpad Adobe Reader or other pdf viewer

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Except where otherwised noted, this item's license is described as Attribution 4.0 International (CC BY 4.0)