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Slow kinetics is one of the capital issues of photocatalytic technology because of its heterogeneous nature, which involves multi-step processes. Herein, we show that the simple modification of the sol-gel-based TiO2-smectite composite by hexadecyltrimethylammonium bromide (HDTMA) significantly boosts adsorption and photocatalytic efficient sol-gel-based light towards the removal of diclofenac from water. Three photocatalysts were prepared, including TiO2, TiO2-smectite, and HDTMA-TiO2-smectite. The materials were characterized to understand the surface interaction and crystal characteristics. In terms of photoactivity, it was found that the addition of HDTMA to TiO2-smectite improved the removal rate by twice. HDTMA changes the functional groups to TiO2-smectite composite allowing enhanced adsorption and photoactivity through the so-called Adsorb and Shuttle process. The recycling tests show that HDTMA-TiO2-smectite can be used up to four times with good performance. This modification approach could intensify the removal of pollutants from water instead of using complicated and costly techniques.