Precise preparation and characterization of ladder-like vinylpolymers by intramolecular ATRP compartmentalized in a nano-sized test tube

Abstract

A multi-vinyl polymer (MOI-EO-26) which has many pendant methacrylate groups on a rigid helical isocyanate backbone and an ATRP initiation functional group at the ¡-end was compartmentalized in a 100 nm3 volume nano-test tube. The nano-test tube was prepared by an inversed nano-emulsion consisting of 2,2,2-trifluoroethanol as the dispersed phase, heptane as the continuous phase, and 3-[dimethyl(octadecyl)ammonio]propane-1-sulfonate as the surfactant. The ladder polymer having a narrow polydispersity and a high double bond consumption rate has successfully been prepared by the intramolecular ATRP of MOI-EO-26 in the nano-test tube. The small angle X-ray scattering (SAXS) profile from MOI-EO-26 in a tetrahydrofuran can be perfectly described by the cylinder model with a length of 5.39 nm and a diameter of 0.96 nm. The SAXS profile of the nano-test tube containing MOI-EO-26 at 55°C was also described by a cylinder with a length of 17.6 nm and a diameter of 2.8 nm and /or an ellipsoid with a long axis of 11.4 nm and a short axis of 1.45 nm. Intramolecular ATRP of MOI-EO-26 compartmentalized in the nano-test tube was carried out at 55°C to afford the well-defined ladder polymer with 61% double bond consumption rate at 100% recovery.