Research data supporting Green biodiesel production from Jatropha curcas oil using a carbon-based solid acid catalyst: A process optimization study

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Ruatpuia, Joseph 
Changmai, Bishwajit 
Pathak, Ayush 
Alghamdi, Lana 

Research data supporting the full paper entitled " Green biodiesel production from Jatropha curcas oil using a carbon-based solid acid catalyst: A process optimization study" by JVL Ruatpuia et al. accepted for publication in Renewable Energy, 2023.

A heterogeneous biomass-based carbonaceous solid acid catalyst (SAFACAM) whose preparation we reported in was used multiple times in the production of biodiesel from Jatropha curcas oil (JCO). The following supporting data are deposited: Modified Boehm titration for the density of acid groups on SAFACAM. For –COOH/–SO3H density and total acid density, NaHCO3 and NaOH were used, respectively. –OH density was extrapolated. –SO3H density was from inductively coupled plasma-optical emission spectroscopy (ICP-OES, see below), allowing –COOH density to be extrapolated. 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) used a continuous flow of N2 with heating at 10 °C min–1. A Mettler Toledo TGA/DSC1 was used in the range 50-600 °C. ICP-OES and C, H, N elemental analyses used a Thermo Scientific iCAP 7400 ICP-OES spectrometer and an Exeter analytical CE 440 elemental analyzer (975 °C), respectively. FT-IR analysis was by Nicolet iS50 spectrometer (Thermofisher). X-ray photoelectron spectroscopy (XPS) data were obtained using an ESCALAB Xi+ instrument equipped with a micro-focused dual-anode Al/Mg Kα source. 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. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) used a JEOL JSM-7600F microscope (80 mA beam current, 20 kV accelerating voltage, 1500x magnification power). Transmission electron microscopy (TEM) used a JEOL JEM2100 microscope operating in brightfield mode. Biodiesel analysis used an Agilent 7890 with a FID detector for gas chromatography-high resolution mass spectrometry (GC-HRMS). 55–230 °C, 10 °C min−1. Detector and injector were at 300 °C and 250 °C, respectively. Biphenyl used as internal standard. A Jeol AccuTOF GCV with a mass range of 10-2000 amu and a mass resolution of 6000 was used in HRMS. 1H and 1H 13C NMR spectra were obtained on a Bruker ASCEND-600. TMS internal standard and CDCl3 solvent. Data collected at 28 °C. Biodiesel was compared to conventional American Society for Testing Materials (ASTM) parameters.

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Bruker TopSpin 2.1 Excel 2016
Biodiesel, Heterogeneous catalysis, Response surface methodology, sulfonic acid functionalized carbonaceous catalyst, Transesterification