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In the present study, adsorption of colour and other pollutants from agro-based paper mill effluent onto fabricated coal fly ash nanoparticles (CFA-N) have been investigated. Response surface methodology was applied to evaluate the operational conditions for maximum ouster of colour from effluent by nano structured CFA-N. Maximum reduction in colour (92.45%) and other pollutants were obtained at optimum conditions: 60 min interaction time, 60 g/L adsorbent dosage and 80 rpm agitation rate. The regression coefficient values (adjusted R2 = 0.7169; predicted R2 = 0.7539) established harmony between predicted and the experimental data. The adsorption equilibrium results matched perfectly with both Langmuir and Freundlich isotherms with maximum adsorption capacity of 250 platinum–cobalt/g. Additionally, the efficacy of CFA-N was also assessed in a continuous column mode. Furthermore, the feasibility of treated effluent for irrigation purpose was checked by growing the plant Solanum lycopersicum. Overall, the findings demonstrated the outstanding role of inexpensive and abundantly available CFA-N in treatment of paper mill effluent to the required compliance levels. HIGHLIGHTS Nano fly ash was successfully utilized for removal of colour and other pollutants from agro-based paper mill effluent.; RSM using BBD was used to optimize the operational conditions.; Quadratic models have been established for the response variables.; Fixed-bed column adsorption studies illustrated the feasibility of nano fly ash for pilot-scale applications.; The reusability of treated effluent for irrigation was examined.