We have intended and preparation of hierarchically absorbent materials were covered with a NiMn2O4 and acts as a catalyst for azo dye degradation. The polyaromatic-based (PA) absorbent compounds were initially constructed by bromomethylated aromatic hydrocarbons which undergo self-polymerization in presence of ZnBr as a reagent and cross linker is bromomethyl methyl ether. The absorbent black materials with a 3D network were prepared by direct carbonization and activation of the as-prepared PA. The hydrothermal method was adapted for the preparation of carbon hybrid material C@NiMn2O4 powder's catalytic activity is effective in reducing p-nitrophenol to p-aminophenol and decolorizing carbon-based dyes like methyl orange (MO), methyl yellow (MY), and Congo red (CR) in aqueous media at 25 °C when NaBH4 is added. UV–visible spectroscopy was used to analyze the dyes' breakdown at regular interval.