Graphene zirconium oxide nanocomposite (Gr@ZrO2‐NC) has been functionalized with cetyltrimethylammonium bromide (CTAB or CT) or butanediyl‐1,4, bis (N, N‐hexadecyl ammonium) dibromide (cationic gemini surfactant (CGS)). Structural, morphological, optical and thermal properties of synthesized adsorbents (Gr@ZrO2‐NC, CT‐Gr@ZrO2‐NC and CGS‐Gr@ZrO2‐NC) are investigated using XRD, FTIR, electron microscopy and TGA. CGS‐Gr@ZrO2‐NC showed faster removal efficacy (90 % within the first 25 min) for anionic azo dyes (methyl orange, MO and Congo red, CR) compared to other adsorbents. This effect may be due to the creation of stronger hydrophobic region at the surface of adsorbent with CGS. Effects of concentration, contact time and pH were also seen. The adsorption efficacy remained better even in the simultaneous presence of MO and CR. Adsorption data with time showed that the pseudo‐second‐order kinetic model has been obeyed. Adsorbents were regenerated successfully with ethylene glycol (∼83 %).

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