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Synthesis and characterization of polyamine‐based cyclophosphazene hybrid microspheres
Authors:Helmut Keul  Martin Möller  Andrij Pich
Affiliation:1. Institute of Technical and Macromolecular Chemistry, RWTH Aachen University, , 52056 Aachen, Germany;2. Functional and Interactive Polymers, DWI an der RWTH Aachen e.V., , 52056 Aachen, Germany
Abstract:Starting with hexachlorocyclotriphosphazene (HCCP) and branched polyethylenimine (bPEI) crosslinked cyclomatrix polyphosphazene poly(HCCP‐cobPEI) microspheres are prepared by precipitation polymerization in acetonitrile at 50 °C under ultrasound irradiation. The influence of varying reagent ratios on the chemical composition, morphology, and physical and chemical properties of the microspheres is investigated. Furthermore, the microspheres are characterized by Fourier‐transform infrared spectroscopy, dynamic light scattering (DLS), X‐ray photoelectron spectroscopy, elemental analysis, as well as 31P MAS NMR. FESEM and DLS analysis show microspheres of smooth and spherical shape which swell both in water and acetonitrile. The particle diameters in the dry state range from 0.4 to 0.9 μm, but due to swelling a size increase between 45 and 140% is observed depending on the chemical composition and the solvent medium. The thermal stability of the microspheres ranges from 262 to 351 °C. The presence of reactive amine groups on the surface is proven by electrophoretic mobility measurements and chemical modification with two model compounds. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 527–536
Keywords:hexachlorotriphosphazene  microspheres  polyethylenimine  precipitation polymerization
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