Promising advances in membrane technology can lead to energy-saving and eco-friendly solutions in industrial sectors. This work demonstrates a highly selective membrane with ultrathin and highly interconnected organosiloxane polymer nanolayers by initiated chemical vapor deposition to effectively separate solutes within the molecular weight range of 150-300 g mol-1. We optimize the poly(1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasiloxane) membrane by adjusting both the thickness of the selective layer and the pore sizes of its support membranes. Notably, the 29 nm selective layer imparts a uniformly narrow molecular sieving property, providing a record-high solute-solute selectivity of 39.88 for different-sized solutes. Furthermore, a solute-solute selectivity of 11.04 was demonstrated using the real-world active pharmaceutical ingredient mixture of Acyclovir and Valacyclovir, key components for Herpes virus treatment, despite their molecular weight difference of less than 100 g mol-1. The highly interconnected membrane is expected to meet rigorous requirements for high-standard active pharmaceutical ingredient separation.
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