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The three zinc(II) metal–organic frameworks [Zn₂(oba)₂(4-bpdb)]·(DMF)_x (TMU-4), [Zn(oba)(4-bpdh)_0.5]_n·(DMF)_y (TMU-5), and [Zn(oba)(4-bpmb)_0.5]_n·(DMF)_z (TMU-6) [DMF = dimethylformamide, H₂oba = 4,4′-oxybisbenzoic acid, 4-bpdb = 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene, 4-bpdh = 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene, and 4-bpmb = N¹,N⁴-bis((pyridin-4-yl)methylene)benzene-1,4-diamine], which contain azine-functionalized pores, have been successfully synthesized by mechanosynthesis as a convenient, rapid, low-cost, solventless, and green process. These MOFs were studied for the removal and extraction of some heavy-metal ions from aqueous samples, and the effects of the basicity and void space of these MOFs on adsorption efficiency were evaluated. The results showed that, for trace amounts of metal ions, the basicity of the N-donor ligands in the MOFs determines the adsorption …