With the rapid development of nuclear energy, one of the main constraints restricting the development of nuclear energy is the long‐term safe disposal of strong uranium waste. Here it is a great significance that we use four new synthetic Ln (III)‐based coordination polymers to test the uranium solution. In this study, four three‐dimensional coordination polymers 1–4 (CPs‐(1–4); Ln = Eu, Gd, Sm, Nd) were successfully synthesized through 1:1 complexation of Ln (NO3)3·6H2O with poly‐carboxylic acid ligand H3TIBTC (2,4,6‐Triiodo‐1,3,5‐benzene tricarboxylic acid) which contains substituents of the carboxylic acid group and halogen atom, respectively. Based on the ligand being excellent fluorescent properties in the solution, it prompted us to further study the fluorescence properties of the coordination polymers. Experimental results show that the coordination polymers are favorable materials for the simultaneous selective detection uranium solution from water, being potentially useful in monitoring water quality and treating uranium‐wastewater.