Adsorptive　C2H2/C2H4　separation　using　metal-organic　frameworks　(MOFs)　has　emerged　as　a　promising　technology　for　the　removal　of　C2H2　(acetylene)　impurity　(1　%)　from　C2H4　(ethylene).　The　practical　application　of　these　materials　involves　the　optimization　of　separation　performance　as　well　as　development　of　scalable　and　green　production　protocols.　Herein,　we　report　the　efficient　C2H2/C2H4　separation　in　a　MOF,　Cu(OH)INA　(INA:　isonicotinate)　which　achieves　a　record　C2H2　packing　density　of　351　mg　cm-3　at　0.01　bar　through　high　affinity　towards　C2H2.　DFT　(density　functional　theory)　calculations　reveal　the　synergistic　binding　mechanism　through　pore　confinement　and　the　oxygen　sites　in　pore　wall.　The　weakly　basic　nature　of　binding　sites　leads　to　a　relatively　low　heat　of　adsorption　(Qst)　of　approximately　36　kJ/mol,　which　is　beneficial　for　material　regeneration　and　thermal　management.　Furthermore,　a　scalable　and　environmentally　friendly　synthesis　protocol　with　a　high　space-time　yield　of　544　kg　m-3　day-1　has　been　developed　without　using　any　modulating　agents.　This　material　also　demonstrates　enduring　separation　performance　for　multiple　cycles,　maintaining　its　efficacy　after　exposure　to　water　or　air　for　three　months.