In recent years, chitosan/inorganic composites have attracted increasing attention due to its fascinating properties and potential applications in biodegradable materials, drug release, electrochemical sensor, packaging materials and so on. Chitosan/inorganic composites are expected to be as an effective way to overcome shortcomings of slow flocculating speed of chitosan particles, not good enough to meet those wide range of applications in wasterwater treatment. In this study, novel chitosan/clay/PAC (polyaluminium chloride) composite was prepared, and it was used in treating effluent from dying and finishing process. One set of orthogonal experiments were conducted to optimize the experimental condition, and the results showed that removal of waste dye is affected by the dosage of chitosan, PAC, clay, pH and treatment time. The experiments results indicated that the effluent from dying and finishing process treated by the prepared composites became obviously fade, and its COD (chemical oxygen demand) decreased from original 1398.2mg/L to 197.6mg/L, the removing rate reached 85.9%.