This work presents the preparation of inorganic–organic hybrid nanocomposites, namely three-dimensional polyaniline (Pani)/activated silica gel (ASG) (3D Pani@ASG), their characterization, and in removing application as a potential adsorbent for cationic brilliant green (BG), crystal violet (CV), and anionic Congo red (CR), and methyl orange (MO) dyes. Pani@ASG nanocomposites have been prepared by the in situ polymerization method and characterized using various techniques such as Fourier transform infrared (FTIR), X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) with selected area electron diffraction, thermogravimetric analysis with derivative thermogravimetry, zeta potential analyses, and Brunauer–Emmett–Teller (BET). The scanning electron microscopy (SEM) study confirms the average particle size of the Pani@ASG nanocomposite is in the range of 5 nm. FESEM, TEM, FTIR, and XRD analysis proved the successful decoration of ASG over Pani. The BET result of Pani@ASG shows a mesoporous nature with a pore diameter of less than 3 nm and a surface area of 423.90 m2 g–1. Both SEM and TEM analyses show the proportional distribution of ASG over Pani’s surface. The adsorption trend of BG and MO on the studied materials at pH 7 was found as follows: Pani@ASG > Pani > ASG. The highest sorption capacities of MO and BG on Pani@ASG were 161.29 and 136.98 mg/g (T = 298.15 K, and Pani@ASG dose: 0.04 g for MO and 0.06 g for BG), which were greater compared with bare Pani and bare ASG, respectively. The interaction mechanism behind the adsorption of BG and MO dyes onto the Pani@ASG nanocomposite includes electrostatic interaction, π–π interaction, and hydrogen bonding. The mechanistic pathway and the interactions between the targeted dyes and Pani@ASG were further studied using adsorption isotherm, adsorption kinetics, and thermodynamics.

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