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A high‐quality filler within mixed matrix membranes, coupled with uniform dispersity, endows a high‐efficiency transfer pathway for the significant improvement on separation performance. In this work, a zeolite‐typed MCM‐22 filler is reported that is doped into polydimethylsiloxane (PDMS) matrix by ultrafast photo‐curing technique. The unique structure of nanosheets assembly layer by layer endows the continuous transfer channels towards penetrate molecules because of the inter‐connective nanosheets within PDMS matrix. Furthermore, an ultrafast freezing effect produced by fast photo‐curing is used to overcome the key issue, namely filler aggregation, and further eliminates defects. When pervaporative separating a 5 wt% ethanol aqueous solution, the resulting MCM‐22/PDMS membrane exhibits an excellent membrane flux of 1486 g m−2 h−1 with an ethanol separation factor of 10.2. Considering a biobased route for ethanol production, the gas stripping and vapor permeation through this membrane also shows a great enrichment performance, and the concentrated ethanol is up to 65.6 wt%. Overall, this MCM‐22/PDMS membrane shows a high separation ability for ethanol benefited from a unique structure deign of fillers and ultrafast curing speed of PDMS, and has a great potential for bioethanol separation from cellulosic ethanol fermentation. [ABSTRACT FROM AUTHOR]