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Determination of methylene bridge crosslinking in chloromethylated PS‐DVB resins
Authors:G Leslie Burnett  John C Rohanna  Steve Rosenberg  Alfred K Schultz  Javier Read de Alaniz
Institution:1. Materials Research Laboratory, University of California, Santa Barbara, California;2. The Dow Chemical Company, Collegeville, Pennsylvania;3. The Dow Chemical Company, Edina, Minnesota;4. Department of Chemistry and Biochemistry, University of California, Santa Barbara, California
Abstract:We present the development of a method for the determination of methylene bridge crosslinking in 13C‐labeled chloromethylated polystyrene‐divinylbenzene resins. Our system uses a new room temperature reduction of the chloromethyl groups that circumvents the possible challenges associated with additional crosslinking. We demonstrate how the reduction of the chloromethyl groups allowed for the determination of methylene bridging, derived from the methylenebis(ethenylbenzene) crosslinker, based on the integration of the methylene signal in the 13C NMR spectra. Utilizing this method, the total crosslinking within the chloromethylated resin generated at 35 °C was determined to be upward of 10 wt %, which increased from 6 wt % in the unfunctionalized resin. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 54, 1955–1960
Keywords:chloromethylated polystyrene–  divinylbenzene  crosslinking  methylene bridge  NMR  resins
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