Laboratory prepared and commercial poly(2‐2,2,2‐trifluoroethoxy‐2‐methyl)oxetane, P[3FOx] and poly(2‐2,2,2‐pentafluoropropoxy‐2‐methyl)oxetane, P[5FOx] polyols contain varying amounts of cyclics and low molar mass (LMW) constituents as byproducts of ring opening polymerization. Guided by phase diagrams determined by cloud point measurements, P[3FOx] diol separation is achieved. The impact of purification is explored via the preparation of P[3FOx] and P[5FOx] polyurethanes from cyclic/LMW‐free diols. Mechanical properties are improved because of higher polyurethane molecular weights. AFM revealed complex rugosity that is correlated with dynamic contact angles free from effects of water contamination.

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