| Summary: | A volatile organic compound adsorbent based on a porous clay heterostructure (PCH) with alginate biopolymer was successfully prepared. From N<sub>2</sub> adsorption–desorption analysis, the specific surface area, pore volume, and pore size of bentonite were dramatically increased after introducing the porous structure. Following complexation with alginate (Alg-PCH), the pore volume and pore size were not significantly affected by pore structure. The thermal stability of Alg-PCH shows enhanced thermal stability compared to alginate and alginate beads. The morphology layered structure of Alg-PCH was carried out by transmission electron microscopy (TEM), suggesting the disorder and re-order of the <i>c</i>-axis layer stacking by porous structure and complexation with alginate, respectively, which was well-matched with X-ray diffraction results. To optimize the preparation of Alg-PCH, various reaction conditions (alginate, CaCl<sub>2</sub> concentration, bead size, and weight ratio between alginate and PCH) were utilized. According to the toluene adsorption–desorption experiments, the preparation conditions for Alg-PCH were selected as a 2 mm extrusion tip, 0.5% of alginate, and 2% of CaCl<sub>2</sub> solution with a 1:50 alginate:PCH weight ratio. Additionally, it shows 61.63 mg/g adsorption capacity with around 49% desorption efficacy under atmospheric temperature and pressure.
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