This study aims to synthesize and characterize nickel oxide (NiO) nanoparticles as heterogeneous catalysts for biodiesel production from used cooking oil through transesterification. The synthesis was conducted using the sol-gel method with NiCl2·6H2O as a precursor and NaOH as an alkaline agent. Characterizations were then performed using Particle Size Analysis (PSA), X-ray Diffraction (XRD), Scanning Electron Microscopy with Energy Dispersive Spectroscopy (SEM-EDS), and Specific Surface Area (SAA) analysis. The PSA results showed that the samples had an average particle size of 37.0 nm with a narrow distribution (PDI = 0.010). XRD confirmed a cubic crystal structure corresponding to JCPDS No. 47-1049, while SEM images showed revealed uniform spherical morphology. In addition, EDS analysis verified the composition of Ni and O as the main elements. The SAA of 489.26 m2/g showed high catalytic activity potential. Catalyst performance tests with methanol-to-oil molar ratios of 1:3, 1:6, and 1:9 showed the highest biodiesel yield of 97.79% at a 1:9 ratio. The produced biodiesel met the Indonesian National Standard (SNI 7182:2015) with a density of 0.86–0.89 g/mL, acid number of 0.40–0.50 mg KOH/g, iodine number of 67.73–93.13 g I2/100 g, and cetane number of 76.87–114.86. GC-MS analysis showed methyl ester chains between C15–C21, confirming compliance with APEC standards. Based on these results, NiO nanoparticles showed high efficiency as an eco-friendly heterogeneous catalyst for biodiesel production.
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