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Herein, we developed a viable synthetic protocol to scale\u2010up a series of ultramicroporous Zr\u2010MOFs (ZrFA\/ZrFA\u2010D\/ZrFA\u2010D\u2010Cu(I)) with the simplest monocarboxylate, formate (FA), through consecutive production by recycling solvent\/modulator. Besides a size\u2010exclusion effect disfavoring C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    adsorption, introduction of defective and Cu(I) sites was found to enhance gas affinity and uptake capacity. A comprehensive evaluation of C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    separation and economic efficiency has been proposed, suggesting the improvement of C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    uptake capacity is effective for the binary C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    separation, while the separation process of the ternary C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    \/C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    mixtures depends on subtle tradeoff of complex factors and limited by challenging CO\n                    <jats:sub>2<\/jats:sub>\n                    \/C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    separating. Notably, the large\u2010scale separation has been testified to significantly improve separation efficiency, and the low\u2010cost preparation benefits high economic efficiency. The distinct C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    adsorption mechanism in ZrFA\/ZrFA\u2010D\/ZrFA\u2010D\u2010Cu(I) has been elucidated by the theoretical calculations. This work may shed a light on the future C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>4<\/jats:sub>\n                    purification technology by pushing MOF\u2010syntheses toward low\u2010cost, scale\u2010up, and recyclable production.\n                  <\/jats:p>","DOI":"10.1002\/anie.202505978","type":"journal-article","created":{"date-parts":[[2025,5,2]],"date-time":"2025-05-02T12:31:50Z","timestamp":1746189110000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["Synthesis and Modification of Formate Zr\u2010MOF (ZrFA) Toward Scalable and Cost\u2010Cutting Gas Separation"],"prefix":"10.1002","volume":"64","author":[{"given":"Xiao\u2010Hong","family":"Xiong","sequence":"first","affiliation":[{"name":"MOE Laboratory of Bioinorganic and Synthetic Chemistry GBRCE for Functional Molecular Engineering LIFM IGCME School of Chemistry Sun Yat\u2010Sen University  Guangzhou 510275 China"},{"name":"Department of Chemistry and Chemical Engineering Key Laboratory for Preparation and Application of Ordered Structural Materials of Guangdong Province Shantou University  Shantou 515063 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liang","family":"Song","sequence":"additional","affiliation":[{"name":"MOE Laboratory of Bioinorganic and Synthetic Chemistry GBRCE for Functional Molecular Engineering LIFM IGCME School of Chemistry Sun Yat\u2010Sen University  Guangzhou 510275 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wei","family":"Wang","sequence":"additional","affiliation":[{"name":"MOE Laboratory of Bioinorganic and Synthetic Chemistry GBRCE for Functional Molecular Engineering LIFM IGCME School of Chemistry Sun Yat\u2010Sen University  Guangzhou 510275 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