Phase-pure layered perovskite La(4)Ni(3)O(10) powders were synthesized by a solution combustion approach. It is found that, in the presence of the La(4)Ni(3)O(10) powders, aqueous azo dyes can be degraded catalytically and efficiently under ambient conditions. Neither light nor additional reagents are needed in the catalytic reaction. The dye degradation procedure can be accelerated markedly by magnetic stirring. A systemic series of chemical and electrochemical experiments suggested that the dye degradation proceeds through electron transfers from the dye molecules to the catalyst and then to electron acceptors such as dissolved oxygen. The present catalytic degradation requires no additional reagents or external energy input, which hence provides a potentially low-cost alternative for the remediation of azo-dye effluents.