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A new high-throughput approach to measure copolymerization reactivity ratios using real-time FTIR monitoring

Authors

  • Sohel Shaikh,

    1. Department of Chemical and Biochemical Engineering, University of Western Ontario, London, Ontario, Canada N6A 5B9
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  • Judit E. Puskas,

    Corresponding author
    1. Department of Chemical and Biochemical Engineering, University of Western Ontario, London, Ontario, Canada N6A 5B9
    • Department of Chemical and Biochemical Engineering, University of Western Ontario, London, Ontario, Canada N6A 5B9
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  • Gabor Kaszas

    1. Rubber Division, Bayer Incorporated, 1265 Vidal St. South, Sarnia, Ontario, Canada, N7T 7M2
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  • This paper is dedicated to Tibor Kelen, Ferenc Tüdös, and Béla Turcsányi.

Abstract

This paper presents a novel high-throughput approach to measure copolymerization reactivity ratios from a single experiment using high-speed real-time Fourier transform infrared (FTIR) monitoring of the isobutylene/isoprene (IB/IP) system initiated by 2-chloro-2,4,4-trimethyl-pentane (TMPCl)/TiCl4 in hexane/methyl chloride (Hx/MeCl) 60:40 v/v solvent at −80 °C. Traditional polymer analysis is severely limited in this system, which is riddled by side reactions. The reactivity ratios calculated by linear (Mayo-Lewis and Kelen-Tüdös) methods and by a nonlinear least square (NLLS) method (van Herk algorithm) showed good agreement with r1 =1.32 and r2 = 0.74 calculated using Mayr's nucleophilicity scale. Combination of the Kelen-Tüdös and NLLS methods yielded r1 = 1.17 ± 0.01 and r2 = 0.99 ± 0.02. These values agree well with those reported by Thaler et al. but disagree with most reported data. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 4084–4100, 2004

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