Two new Cd 2+ coordination polymers (CPs), namely {Cd(L)(1,4-PDA)·0.7(C 2 H 5 OH)} n ( 1 ) and {Cd(L) 0.5 (1,8-NDC)·H 2 O} n ( 2 ) L = 1,4-bis(5,6-dimethybenzimidazol-1-yl)-2-butene, 1,4-H 2 PDA = 1.4-phenylenediacetic acid, 1,8-H 2 NDC = 1,8-naphthalenedicarboxylic acid, were hydrothermally synthesized and characterized. 1 is a (4,4)-layered structure and further extended into a 3D supramolecular network via π-π stacking interactions. 2 features a 2D (3,4)-connected 3,4L83 framework. 1 and 2 can act as luminescence sensors for detecting acetylacetone (acac) and Fe 3+ with high sensitivity, selectivity and recyclability. This is the first dual fluorosensors employing CPs for the detection of Fe 3+ and acac. The mechanism for the luminescent sensing of acac and Fe 3+ was suggested. Two new CPs, namely {Cd(L)(1,4-PDA)·0.7(C 2 H 5 OH)} n ( 1 ) and {Cd(L) 0.5 (1,8-NDC)·H 2 O} n ( 2 ) were fabricated. 1 shows a sql 2D network. 2 shows a 2D 3,4L83 network. Both 1 and 2 were highly selective and sensitive fluorescent chemosensors toward acetylacetone and Fe 3+ .