Organic dyes are a substantial contribution to environmental pollution and are considered as hazardous. These compounds are widely used in various industries like textiles, food, paper, cosmetics, and printing. A cationic dye, such as Fast Blue (FB) and Congo Red (CR), is an example of organic compound with several commercial uses but dangerous for environment and human beings. Copper Magnesium Vanadate NPs (CuMgV NPs) were successfully prepared using the combustion method in which Neem extract was used as a fuel. The XRD, FTIR, and FESEM techniques were used to analyze the sample's structure and morphology. The XRD reveals monoclinic structure of the CuMgV NPs with average particle size around 30 nm. The presence of tiny particles that prefabricated to form a widely distributed, spherical shape, and size between 15 and 25 nm was observed by HRTEM microscopic investigations. The CuMgV NPs were assessed using several electrochemical techniques. In photocatalytic tests, 120 min of UV light irradiation was sufficient to achieve a 58% and 55.52% decolorization rate for the industrial pollutants CR and Fast FB dyes. CuMgV NPs were found to have a specific capacitance value of 560.5 Fg−1 at 1 Ag−1 and a retention rate of 89% after 4000 cycles. These features promote the production of NPs for energy and environmental applications and provide greater insight into the characteristics of the material.