H_2La_2Ti_3O_(10)/CdS nanocomposite with higher photoactivity was synthesized by a stepwise exchange process from H_2La_2Ti_3O_ 10 , which was obtained by H+-exchanging reaction of K_2La_2Ti_3O_ 10 with HCl other than the normally used HNO_3. The pillaring process was investigated by XRD, TEM, FT-IR and BET methods. The photocatalytic decomposition of aniline was used as the model system to evaluate the photochemical properties of H_2La_2Ti_3O_ 10 /CdS, H_2La_2Ti_3O_ 10 and K_2La_2Ti_3O_ 10 . It is found that the photoactivity of layered H_2La_2Ti_3O_ 10 is greatly improved by the intercalation of CdS in the interlayer. In general, the excellent photoactivity of the H_2La_2Ti_3O_ 10 /CdS nanocomposite might be attributing to the extremely small particle size of incorporated CdS and good contact between CdS and La_2Ti_3O_ 10 2- layers. On the other hand, the coupling of two semiconductor particles with different energy gap is useful to achieve effective charge separation. In H_2La_2Ti_3O_ 10 /CdS, a photo-generated electron can transfer from CdS to the La_2Ti_3O_ 10 2- layer, while the holes remain in the CdS particles. This helps to diffuse the electrons and holes before reaching the interface, and the holes and electrons can be effectively captured by the electrolyte in the solution. Simultaneously, the optimal operating condition of photodecomposition aniline was investigated. H_2La_2Ti_3O_ (10) / CdS nanocomposite with higher photoactivity was synthesized by a stepwise exchange process from H_2La_2Ti_3O_10, which was obtained by H + -exchanging reaction of K_2La_2Ti_3O_10 with HCl other than the normally used HNO_3. The pillaring process was investigated by XRD, TEM , FT-IR and BET methods. The photocatalytic decomposition of aniline was used as the model system to evaluate the photochemical properties of H_2La_2Ti_3O_10 / CdS, H_2La_2Ti_3O_10 and K_2La_2Ti_3O_10. It is found that the photoactivity of layered H_2La_2Ti_3O_ 10 is greatly improved by In general, the excellent photoactivity of the H_2La_2Ti_3O_10 / CdS nanocomposite might be attributing to the extremely small particle size of the incorporated CdS and good contact between CdS and La_2Ti_3O_10 2-layers. On the other hand, the coupling of two semiconductor particles with different energy gap is useful to achieve effective charge separation. In H_2La_2Ti_3 O_10 / CdS, a photo-generated electron can transfer from CdS to the La_2Ti_3O_ 10-layer, while the holes remain in the CdS particles. This helps to diffuse the electrons and holes before reaching the interface, and the holes and electrons can be effectively captured by the electrolyte in the solution. Simultaneously, the optimal operating condition of photodecomposition aniline was investigated.