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Abstract Biodiesel (BD) is a promising alternative fuel to fossil-based diesel principally owing to its virtues, e.g., biodegradability, non-toxicity together with reduced pollutants emissions and is a domestic, renewable resource. However, the higher cost of biodiesel in comparing with petrodiesel is the key obstacle that hindered its commercialization. Herein, this study targets the development of heterogeneous catalysts in replacement of the currently used homogeneous catalysts. This has already been achieved by two approaches; the first is to use a hybrid catalyst of heterogeneous nickel oxide (NiOx) nanoparticles with the least amount of NaOH catalyst. And the second approach targets the developing of waste-derived solid state catalysts for the efficient transesterification reaction of sunflower oil into BD. Physicochemical properties of the proposed catalysts are probed by TGA{u2013}DTG, XRF, XRD, FT-IR, SEM, BET, and CO2-TPD techniques. Also, four independent variables (i.e., catalyst loading, methanol/oil molar ratio, reaction temperature and time) have been selected to inspect their influence on BD conversion% as a dependent response variable of the process. Experimental results are compared to model predictions brought about using Design Expert Software. The proposed catalysts reveal high activity towards BD conversion while utilizing the least amount of catalyst and methanol/oil ratio at optimized reaction temperature and time. BD conversions % reached as high as 99% in several successive process batches. Moreover, The thus-produced biodiesel fuel compiles the ASTM D-6751 and EN-14214 specifications |