In this study, a heterogeneous basic catalyst was synthesized from a catalyst composite material (CCM) of coffee husk ash and char mixture (A/C) impregnated with KNO 3 and employed to transesterify crude waste frying oil (WFO). The effect of CCM calcination temperature (CCMCT) (500−700 °C) on the catalyst physicochemical properties was investigated. A differential scanning calorimeter was used to examine potential phase changes during the calcination of A/C and CCM. The catalysts from each CCMCT were characterized by X-ray diffraction (XRD), Brunauer−Emmet−Teller surface area analyzer, scanning electron microscopy (SEM), SEM with energy-dispersive X-ray diffractometer, colorimeter, and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectrometer. The methoxy functional group FTIR peak integral value and the dynamic viscosity of the biodiesel synthesized by each catalyst were used to determine the qualitative WFO conversion. Furthermore, the quantitative WFO conversion was determined using nuclear magnetic resonance ( 1 H NMR) analysis. Crystallinity, elemental composition, basicity, and morphology of catalysts were highly dependent on the CCMCT. Without transesterification condition optimization (reaction temperature of 45 ± 2.5 °C, catalyst loading of 3 wt %, methanol to oil molar ratio of 12:1, and reaction time of 1 h), a higher catalytic performance (72.04% WFO conversion) was reached using a catalyst from the CCMCT of 600 °C. When using a coffee husk ash catalyst without KNO 3 impregnation (C-00-600), the WFO conversion was only 52.92%. When comparing the C-25-600 and C-00-600 catalysts, it was observed that KNO 3 impregnation had a substantial impact on the catalyst crystallinity, basicity, and morphology.