Abstract
Industrial samples of a copolymer of isobutylene with isoprene (butyl rubber) produced through cationic polymerization via the conventional slurry process (a Lewis acid (AlCl3) as a coinitiator, methyl chloride as a diluent) have been studied with the use of proton magnetic resonance spectroscopy at an Larmor frequency of 600 MHz. Spectra were recorded for different types of deuterated solvents and concentrations of test solutions. The signals were processed via selective improving the resolution and signal-to-noise ratio. The use of these procedures, in combination with conformational representations, made it possible to increase the information content of the spectra.
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G. W. Ver Strate and D. J. Lohse, in Polymer Data Handbook, Ed. by J. E. Mark (Oxford Univ. Press, Oxford, 2009).
Worldwide Rubber Statistics 2009, Ed. by J. L. McGraw (Int. Inst. Synth. Rubber Prod., 2009).
H. Yu. Chen and J. E. Field, J. Polym. Sci., Polym. Lett. 5, 501 (1967).
H. Yu. Chen and J. E. Field, Rubber Chem. Technol. 42, 392 (1969).
Y. Tanaka, H. Sato, Y. Ozeki, M. Ikeyama, and T. Sato, Polymer 16, 709 (1975).
C. Y. Chu and R. Vukov, Macromolecules 18, 1423 (1985).
J. Kuntz and K. D. Rose, J. Polym. Sci., Part A: Polym. Chem. 27, 107 (1989).
D. M. Cheng, J. J. Gardner, H. C. Wang, C. B. Frederick, A. N. Dekmezian, and P. Hous, Rubber Chem. Technol. 63, 265 (1990).
J. L. White, T. D. Shaffer, Ch. J. Ruff, and J. P. Cross, Macromolecules 28, 3290 (1995).
F. C. Stehling and K. W. Bartz, Anal. Chem. 38, 1467 (1966).
J. P. Kennedy and T. Chou, J. Macromol. Sci. A 10, 1357 (1976).
C. Corno, A. Proni, A. Priola, and S. Cesca, Macromolecules 13, 1092 (1980).
G. R. Fulmer, A. J. M. Miller, N. H. Sherden, H. G. Gottlieb, A. Nudelman, B. M. Stoltz, J. E. Bercaw, and K. I. Goldberg, Organometallics 29, 2176 (2010).
J. P. Cohen-Addad, A. Guillermo, and J. P. Messa, Polymer 20, 536 (1979).
A. V. Lubnin and J. P. Kennedy, J. Macromol. Sci. A 32, 191 (1995).
N. Makhiyanov, in Current Aspects of NMR Spectroscopy of Polymers (St. Petersburg, 1994), p. 40.
T. Saito, S. Nakaie, M. Kinoshita, T. Ihara, Sh. Kinugasa, A. Nomura, and T. S. Maeda, Metrologia 41, 213 (2004).
E. Alvarado, http://www.umich.edu/~chemnmr/docs/Quantitative-NMR.pdf
J. C. Lindon and A. G. Ferrige, Prog. NMR Spectrosc. 14, 27 (1980).
S. G. Gallo, H. K. Wiese, and J. F. Nelson, Ind. Eng. Chem. 40, 1277 (1948).
E. W. Garbisch, J. Am. Chem. Soc. 86, 5561 (1964).
N. Makhiyanov, I. G. Akhmetov, and A. M. Vagizov, Vysokomol. Soedin., Ser. A 54, 1722 (2012).
N. Makhiyanov, I. G. Akhmetov, and A. M. Vagizov, Polym. Sci., Ser. A 54, 942 (2012).
K. Kunal, M. Paluch, C. M. Roland, J. E. Puskas, Y. Chen, and A. P. Sokolov, J. Polym. Sci., Part B: Polym. Phys. 46(13), 1390 (2008).
N. E. Moe and M. D. Ediger, Macromolecules 28, 2329 (1995).
N. M. Sergeev, NMR Spectroscopy for Organic Chemists (Mosk. Gos. Univ., Moscow, 1981) [in Russian].
J. Emsley, J. Feeney, and L. Sutcliffe, High Resolution Nuclear Magnetic Resonance Spectroscopy (Oxford Univ. Press, Oxford, 1965; Mir, Moscow, 1968), Vol. 1.
L. J. Fetters, D. J. Lohsey, and R. H. Colby, in Handbook of Physical Properties of Polymers, Ed. by J. E. Mark (Springer, New York, 2007).
F. Barsan, A. R. Karam, M. A. Parent, and M. C. Baird, Macromolecules 31, 8439 (1998).
S. A. Francis and E. D. Archer, Anal. Chem. 35, 1363 (1963).
I. Puskas, E. M. Banas, and G. Nerheim, J. Polym. Sci., Polym. Symp. 56, 191 (1976).
St. L. Manatt, J. D. Ingham, and J. A. Miller, Org. Magn. Res. 10, 198 (1977).
J. Si and J. P. Kennedy, J. Polym. Sci., Part A: Polym. Chem. 32, 2011 (1994).
T. Kuroki, T. Sawaguchi, K. Suzuki, Sh. Ide, and T. Ikemura, Polymer 24, 428 (1983).
S. Nemes, J. Si, and J. P. Kennedy, Polym. Bull. (Berlin) 23, 597 (1990).
A. V. Lubnin and J. P. Kennedy, J. Macromol. Sci. A 31, 655 (1994).
J. Spevacek, L. Toman, and P. Vicek, Polym. Bull. (Berlin) 34, 461 (1995).
Y. Qiu, Y. Wu, X. Gu, X. Xu, and G. Wu, Eur. Polym. J. 41, 349 (2005).
L. K. Kemp, J. E. Poelma, T. R. Cooper, and R. F. Storey, J. Macromol. Sci. A 45, 137 (2008).
Ph. Dimitrov, J. Emert, J. Hua, S. Keki, and R. Faust, Macromolecules 44, 1831 (2011).
Q. Liu, Y. Wu, P. Yan, Y. Zhang, and R. Xu, Macromolecules 44, 1866 (2011).
V. Volkis, R. K. Shoemaker, and J. Michl, Macromolecules 45, 9250 (2012).
N. Makhiyanov and R. Kh. Sadykov, Zh. Prikl. Spectrosk. 53, 432 (1990).
N. Makhiyanov and R. Kh. Sadykov, J. Appl. Spectrosc. 53, 959 (1990).
G. Allegra, E. Benedetti, and C. Pedone, Macromolecules 3, 727 (1970).
R. H. Boyd and Sh. M. Breitling, Macromolecules 5, 1 (1972).
U. W. Suter, E. Saiz, and P. J. Flory, Macromolecules 16, 1317 (1983).
M. Vacatello and D. Y. Yoon, Macromolecules 25, 2502 (1992).
N. Makhiyanov, Candidate’s Dissertation in Physics and Mathematics (St. Petersburg, 1992).
V. Cooper, in The Chemistry of Cationic Polymerization, Ed. by P. Plesch (Oxford Univ. Press, Oxford, 1963; Mir, Moscow, 1966).
J. Kennedy, Cationic Polimerisation of Olefins (Wiley, New York, 1975; Mir, Moscow, 1978).
V. A. Rozentsvet, V. G. Kozlov, and Yu. B. Monakov, Cationic Polymerization of Conjugated Dienes (Nauka, Moscow, 2011) [in Russian].
W. S. Richardson, J. Polym. Sci. 13, 325 (1954).
H. Gunter, NMR Spectroscopy (Wiley, Chichester, 1980; Mir, Moscow, 1984).
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Original Russian Text © N. Makhiyanov, 2014, published in Vysokomolekulyarnye Soedineniya. Ser. A, 2014, Vol. 56, No. 3, pp. 247–262.
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Makhiyanov, N. 1H NMR spectra (600 MHz) and structure of an industrial isobutylene-isoprene copolymer (butyl rubber). Polym. Sci. Ser. A 56, 241–255 (2014). https://doi.org/10.1134/S0965545X14030109
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DOI: https://doi.org/10.1134/S0965545X14030109