<p>Ferrites belong to the wonder class of materials, which is distinguished by their wide range of applications. Applications for nickel ferrites, which are soft, highly magnetic materials with remarkable electrical, magnetic, and optical qualities, are numerous. Using nickel ferrite as a nano-catalyst, our study attempted to convert defatted rice bran into a variety of compounds with added value used in the chemical and pharmaceutical industries. Nickel ferrite is an environmentally friendly substance that lowers waste, purifies water, and conserves energy. It is useful for green technology and environmental preservation because of its effective energy conversion, water-cleaning catalyst function, and ease of recycling substances. Here, Nickel ferrite nanoparticles acts as a heterogeneous catalyst during in-situ acetalisation reaction were prepared by microwave-assisted solution combustion method. The structural, morphological and elemental measurements of the prepared nanocatalysts were determined and characterized in detail by PXRD which gives the crystallite size of 24&#xa0;nm, SEM with EDAX analysis shows the agglomeration of nanoparticles and Brunauer–Emmett–Teller surface area (BET) measurements give the surface area of 2.71 m²/g. This innovative approach utilizes nickel ferrites in a microwave-assisted in-situ acetalization reaction of furfural (a derivative of DRB) with various solvents such as methanol, 1-propanol, and ethanol, resulting in the production of acetals and other important chemicals. These are noteworthy because they offer mild reaction conditions, high yields, short reaction times, and a selective, efficient and versatile process.</p>