Abstract: | Segmented polymer networks with LCST‐behavior have been prepared by free radical initiated copolymerization of α,ω‐bis‐methacrylate terminated poly(methyl vinyl ether) (PMVE) with 2‐hydroxy ethyl methacrylate (HEMA) or butyl acrylate (BA). The PMVE bis‐macromonomers have been obtained via a semi‐continuous process by end‐capping the living cationic polymerization of methyl vinyl ether (MVE) with HEMA. The phase separation temperature can be varied by changing the PMVE/comonomer ratio. Incorporation of PMVE‐grafts in the hydrogels increases the rate of deswelling and improves the mechanical properties. The application of the segmented networks for thermo‐controllable solid phase extraction has been demonstrated by their thermosensitive adsorption behavior of toluene from a water solution. |