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© Three new metal–organic frameworks (MOFs), namely, [Pb7(TTPCA)4Cl2]·3H2O (1), [Pb7(TTPCA)4(DMA)2(HCOO)2]·H2O (2), and [Pb4(TTPCA)3]·3DMF·2H2O·H3O (3), were synthesized by the H3TTPCA ligand [H3TTPCA = 1,1′,1″–(1,3,5–triazine–2,4,6–triyl)–tripiperidine–4–carboxylic acid], with lead(II) nitrate under solvothermal conditions. They were characterized by CHN analysis, IR spectroscopy, UV–vis spectroscopy, and single–crystal and powder X–ray diffraction. In addition, their thermogravimetric analysis and fluorescence properties were studied. Compounds 1–3 were 3D MOF structures with different Pbx(COO)y clusters: ([Pb7(COO)12Cl2]), ([Pb7(COO)12]), and [Pb8(COO)18]. Fluorescence detection of compounds 1–3 shows that they can act as excellent sensors of nitrophenols with a low limit of detection and a high quenching constant.