This paper describes the optimization of synthesis of fly ash based geopolymer (FAGP) for removing the anionic surfactant sodium dodecylbenzene sulfonate (SDBS) using response surface methodology (RSM) by varying the synthesis parameters of silica to alumina (Si/Al), sodium to alumina (Na/Al) and water to solid (W/S) ratios with the adsorption capacity as the response. The geopolymer samples were designed, synthesized, characterized, used for removing SDBS surfactant, and regenerated. Surface area and pore size analysis, Fourier Transform Infrared Spectroscopy (FTIR) analysis, phase analysis, and microstructural analysis confirmed the synthesis of mesoporous and amorphous geopolymers with the presence of pores, cavities and rods in the geopolymer structure. Geopolymer sample synthesized with the composition of Si/Al-2.87, Na/Al-1.0 and W/S-0.35 (FAGP-2) achieved maximum surface area of 59.512 »m2/g and displayed the highest adsorption capacity of 743.706 »mg/g and removal efficiency of 84.5. The ANOVA analysis showed a correlation coefficient (R2) of 0.952, F-value of 22.27, and p value of 0.05 which indicated the significance of the model and lack of fit was non-significant which showed good fitting of the experimental data to the quadratic model with 95 confidence level. The proposed geopolymer composition of Si/Al-2.353, Na/Al-1.056, and W/S-0.339 achieved adsorption capacity of 730.212 »mg/g which is 99 similar to the predicted adsorption capacity. Thermal method successfully regenerated SDBS adsorbed geopolymer with only 13.8 loss of adsorption capacity after five cycles of regeneration. The adsorption capacity of optimized geopolymer is higher than other adsorbents such as cross-linked chitosan films, commercial activated carbon, surface functionalized mesoporous silica nanoparticles, multi-walled carbon nanotubes (MWCNTs), and others used for removing SDBS surfactant and only amino crosslinked chitosan microspheres (ACCMs) has higher adsorption capacity than geopolymer. This shows that geopolymer can also be effectively used to adsorb SDBS surfactant from wastewater. © 2020 Elsevier Ltd.