Both n-butane and iso-butane are important petrochemical raw materials, and their separation is of great significance and full of challenge because of their close boiling characteristic. The ZIF-8 slurry formed with a novel mixed solvent M-water solution as sorption media was adopted to separate the mixture with high efficiency. The iso-/n-butane selectivity of ZIF-8/M-water slurries is as high as 890 with high kinetic performance, even transcending the upper limit of the new materials or membranes. More encouragingly, continuous pilot separation device was established and test results show that the purity and recovery ratio of iso-butane product achieved 99.46 mol% and 87% respectively, which are remarkably superior to the corresponding performance (98.56 mol% and 54%) of the industrial distillation tower. To our best knowledge, this is the first industrial pilot test using MOFs for gas separation, and also an important step forward to the commercial application of MOFs in gas separation.