This work explores the polymerization of sodium 4-styrenesulfonate (NaSS) inside filter paper using dielectric barrier discharge (DBD) plasma and its application in the environmental field. The plasma-based technique, performed under mild conditions, solves common problems associated with conventional polymerization inside porous materials. The polymerization process was monitored using Fourier-transform infrared (FTIR) spectroscopy, which confirmed the consumption of double bonds, particularly in NaSS samples containing the optimal concentration of crosslinker divinyl benzene (DVB) (0.25% wt). Our work demonstrates the effectiveness and promise of DBD plasma as a substitute polymerization approach, especially for those in porous materials.