Porous carbon is a carbon material with a high surface area and abundant pore structure, holding extensive potential applications in the adsorption field. However, current porous carbon materials are complicated to prepare, and most are in powder form, making them difficult to separate from water after adsorption and prone to secondary pollution. This study uses sodium alginate (SA) as a precursor and K2CO3 one-step method to prepare sodium alginate-based macromaterials that can skillfully solve the above problems and explore its adsorption kinetics and thermodynamic characteristics for dimethyl phthalate (DMP). This study's meticulous control of experimental details enabled the fabrication of macroscopic materials. The appropriate temperature and activator blending ratio are critical to material agglomeration. (At 800 °C in a small ceramic boat, macroscopic material C800–2 was prepared with an activator ratio of K2CO3: sodium alginate at 2:1 and under low acid concentration acid washing (0.2 mol/L HCl)). Excessive pyrolysis temperature can lead to severe chemical bond loss, potentially preventing material agglomeration. Excessive doping of the activator may result in carbon framework collapse. While maintaining the macroscopic structure, C800–2 enhanced a 3.8-fold increase in total pore volume and a 4.6-fold increase in surface area. Moreover, at 313 K, its saturated adsorption of DMP reached an impressive 614.98 mg/g. C800–2 material exhibits excellent interference resistance and regeneration capability. The study achieves one-step fabrication of macroscopic materials while retaining superior adsorption performance, providing fundamental data for material engineering applications.