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A novel bi-ligand nickel-based metal–organic framework (Ni-BTC-PYDC MOF) was synthesized using benzene tricarboxylic acid (BTC) and pyridine-2,3-dicarboxylic acid (PYDC) as ligands. This MOF showed improved surface area, structural stability, and electron transfer compared to mono-ligand Ni-MOFs. Characterization by SEM, EDX, EDS mapping, XRD, and FT-IR confirmed its enhanced morphology and nickel content. The catalyst rapidly reduced methyl orange (MO) dye in water, achieving rapid and significant decolorization within 90 s using sodium borohydride (NaBH₄) under mild conditions. It maintained high activity over ten reuse cycles with minimal loss, performing best at pH 5 due to efficient hydride generation and proton-assisted electron transfer. These findings demonstrate that the bi-ligand Ni-MOF is a promising, stable, and reusable catalyst for removing toxic azo dyes from wastewater.