A C/CdS/TiO.sub.2 composite was prepared by a calcination method using sodium alginate (SA) as a medium. Remarkably, two nano-photocatalysts, TiO.sub.2 and CdS, were formed onto the carbon-based materials during calcination. The as-prepared hybrid materials were characterized and analyzed by XRD, SEM, TEM, XPS, UV-vis DRS, and PL techniques. The results showed that the coating of SA on the CH.sub.4N.sub.2S surface decreased the volatilization of CH.sub.4N.sub.2S. The carbon-based materials can not only play the role of a bridge connecting CdS and TiO.sub.2 for the efficient absorption of UV light, but also promote the construction of Z-scheme heterojunctions. The prepared photocatalysts were used in simultaneous adsorption and photocatalysis processes for the removal of organic dyes (cationic yellow X-GL) from aqueous solutions. After 60 min of UV irradiation, the photocatalytic decolorization rate of cationic yellow X-GL in aqueous solutions by C/CdS/TiO.sub.2 composite could reach 97.02%, which was 27% higher than that of TiO.sub.2. The reason was mainly due to the synergistic effect including the interface enhancement effect of hierarchical structure and the separation efficiency of photogenerated carriers. Additionally, it showed good recyclability making a promising photocatalyst material for the degradation of textile dyes.