First-flush rainwater is of great interest in the research on urban environmental protection and rainwater harvesting. It deteriorates the chemical, physical, and microbiological quality of the collected/stored water as well as the water body in an urban area. Accordingly, effective and economic treatment of first-flush rainwater is highly required. This study aimed to develop a technology for the treatment of first-flush rainwater using new filters made of wood fiber mat, dental cotton, and feldspar. The removal of pollutants in first-flush rainwater with each filter material was evaluated. Experiments were carried out using an artificial rainwater solution made of road dust particles (less than 200 um small) and D.I. water that contained ionic species. The SS concentration of the solution was set between 30 and 150 mg/L. Prior to the experiments, the fiber materials were pretreated with NaOH, FeCl3, and Al2O3. The batch test results indicated that the phosphate removal efficiency of the wood fiber mat was 8.6%; of the dental cotton, 34.7%; and of the feldspar, 1.7%. On the other hand, the heavy metal removal efficiency of the wood fiber mat was 91%; of the dental cotton, 26%; and of the feldspar, 0%. The highest cation exchange capacity of the wood fiber mat that was pretreated with NaOH was attributed to the existence of carboxyl and hydroxyl functional groups in the wooden polymers. Combinations of filter materials were found to have been effective in removing particles in the rainwater. The combination of the wood fiber mat with polyethylene beads resulted in 97-98% particle removal. Other combinations such as DP (dental cotton and polyethylene beads), MF (wood fiber mat and feldspar), and DF (dental cotton and feldspar) showed particle removal rates of 90-95%, 84-96%, and 87-94%, respectively. After 30 minutes, all the combinations had a particle removal rate of over 90%.