Montmorillonite interlayer is a special site in chemical reaction for absorption and photolysis. Three kinds of Ti/CTAB (cetyltrimethylammonium bromide) pillared clays were synthesized by controlling the addition sequences and amounts of the Ti and CTAB pillar agents. The X-ray results indicated that the pillared clays by Ti/CTAB pillar agents gave two d 001 values, which may be attributed to the different pillar sizes formed in the clay interlayer due to the interaction of hydrolyzed Ti-polycations and CTAB. Additionally, compared with FT-IR spectroscopy, FT Raman is a powerful analytic tool for characterizing the chemical structures of the pillared clays. After being heated at 500℃ for 1 h, the pillared POMT(A) can be changed to the composite containing anatase TiO₂, and then CTAB could be introduced again for preparing a new TiO₂/CTAB pillared clay. It is expected that this new material could be developed as potential environmental materials for absorbing and photolyzing organic pollutants from water.

Key words: montmorillonite, composite pillared clay, XRD, FT-Raman