To further verify the practical separation performance of NKCOF-62, the transient fixed-bed column breakthrough ex- ). It was observed that C 2 H 4 breakthrough occurred first at 26 min, followed by C 2 H 6 at 45 min and C 2 H 2 at 50 min, and the separation time was finally determined to be 19 min/g. Excitingly, this is the first case of a single COF adsorbent for onestep C 2 H 4 purification from the ternary mixture of C 2 H 2 /C 2 H 4 /C 2 H 6 , and the C 2 H 4 productivity of NKCOF-62 was higher than that of HIAM-210, NPU-1 and even comparable to some top-performing materials like UiO-67-(NH 2 ), UPC-612 and UPC-66 (Table ). Notably, NKCOF-62 could be easily scaled up to kilogram level, while these MOFs could not be prepared on a large scale. Furthermore, the cost of NKCOF-62 is far lower than those of benchmark MOFs, thus making NKCOF-62 great potential in the industrial-scale separation scenario. Additionally, the cycling dynamic breakthrough tests of C 2 H 2 /C 2 H 4 /C 2 H 6 were conducted to assess the recyclability of NKCOF-62 under the same conditions (Figure ). The breakthrough time and the PXRD pattern remained almost unchanged with five continuous cycles, which indicated that it had outstanding stability and recyclability (Figure ).