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Based on the ligand construction strategy, this study selected 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine as the main ligand and coordinated it with 3-methyl-1H-1,2,4-triazole and 3,5-dimethyl-1H-1,2,4-triazole, respectively, to assemble metal-organic frameworks (MOFs), successfully preparing two double-walled MOF crystal materials: Zn-TATB-fmtrz and Zn-TATB-dmtrz. Among them, Zn-TATB-fmtrz has a larger pore size (11.64 \u00d7 6.63 \u00c5), while the pore size of the comparative material Zn-TATB-dmtrz is only 4.94 \u00d7 4.30 \u00c5; in addition, the specific surface area of Zn-TATB-fmtrz (1403.4 m2\/g) is also significantly higher than that of Zn-TATB-dmtrz (826.4 m2\/g). Benefiting from the above structural advantages, both MOF materials can achieve efficient separation of C2H2\/CO2. Systematic adsorption tests indicate that under conditions of 298 K and 1 bar, the maximum acetylene adsorption capacity of Zn-TATB-fmtrz reaches 58.6 cm3\/g, much higher than the 37.5 cm3\/g of Zn-TATB-dmtrz; moreover, the adsorption selectivity of Zn-TATB-fmtrz for C2H2\/CO2 is 3.0, slightly better than 2.9 for Zn-TATB-dmtrz. Dynamic breakthrough experiments based on real binary mixtures further visually confirm that Zn-TATB-fmtrz shows potential for practical C2H2\/CO2 separation.<\/jats:p>","DOI":"10.1021\/acsami.6c10729","type":"journal-article","created":{"date-parts":[[2026,8,9]],"date-time":"2026-08-09T14:01:53Z","timestamp":1786284113000},"page":"44313-44321","source":"Crossref","is-referenced-by-count":1,"title":["Dual-Ligand Synergistic Construction of Double-Walled Cage Zn-MOFs: Methyl Modification Regulates Pore Size and Selective C2H2\/CO2 Separation Performance"],"prefix":"10.1021","volume":"18","author":[{"given":"Hongke","family":"Dong","sequence":"first","affiliation":[{"name":"China University of Petroleum (East China) , , , ,","place":["Qingdao, Shandong, P. R. 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China, 266580"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shaohua","family":"Cheng","sequence":"additional","affiliation":[{"name":"China University of Petroleum (East China) , , , ,","place":["Qingdao, Shandong, P. R. China, 266580"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jie","family":"Song","sequence":"additional","affiliation":[{"name":"China University of Petroleum (East China) , , , ,","place":["Qingdao, Shandong, P. R. China, 266580"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mingliang","family":"Chen","sequence":"additional","affiliation":[{"name":"China University of Petroleum (East China) , , , ,","place":["Qingdao, Shandong, P. R. 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