Abstract
The resolution and the relaxation time of poly(butyl acrylate) in latex-state 13C-NMR spectroscopy are associated with local motions of the polymer in a dispersoid. Latexes were prepared by emulsion polymerization of butyl acrylate with ammonium persulfate. The latex-state 13C-NMR spectra were measured at 323–353 K with a spectrometer operating at 399.7 and 100.4 MHz for 1H and 13C, respectively. The half width of the latex-state 13C-NMR spectrum depends on the temperature. The half width and the spin-spin relaxation time, T2, are superimposed onto the master curve with a reference temperature, TX.
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References
Ribelles JLG, Duenas JMM, Pradas MM (1989) Dielectric relaxation in poly(methyl acrylate), poly(ethyl acrylate), and poly(butyl acrylate). J Appl Polym Sci 38:1145–1157. https://doi.org/10.1002/app.1989.070380612
Gaborieau M, Graf R, Kahe S, Pakula T, Spiess HW (2007) Chain dynamics in poly(n-alkyl acrylates) by solid-state NMR, dielectric, and mechanical spectroscopies. Macromolecules 40:6249–6256. https://doi.org/10.1021/ma0706531
Dejean de la Batie R, Laupretre F, Monnerie L (1988) Carbon-13 NMR investigation of local dynamics in bulk polymers at temperatures above the glass transition temperature. 1. Poly(vinil methyl ether). Macromolecules 21:2045–2052. https://doi.org/10.1021/ma00185a028
Kikuchi H, Tokumitsu H, Seki K (1993) Molecular motins of poly(ethyl acrylate) and poly(n-butyl acrylate) studies by solid-state NMR and molecular dynamics computer experiments. Macromolecules 26:7326–7332. https://doi.org/10.1021/ma00078a032
Kawahara S, Bushimata S, Sugiyama T, Hashimoto C, Tanaka Y (1999) A novel method for 13C-NMR spectroscopy of polymer in emulsion: quantitative analysis of microstructure of crosslinked polybutadiene in latex. Rubber Chem Technol 72:844–853. https://doi.org/10.5254/1.3538836
kawahara S, Washio K, Morita T, Tanaka Y, Isono Y (2001) Hight-resolution latex-state 13C-NMR spectroscopy: PartIIEffect of particle size and temperature. Rubber Chem Technol 74:295–302. https://doi.org/10.5254/1.3544951
Munie GC, Jonas J, Rowland TJ (1980) NMR relaxation study of crosslinked cis-1,4-polybutadiene. J Polymer Sci,ChemEd 18:1061–1070. https://doi.org/10.1002/pol.1980.170180324
Folland R, Steven JH, Charlesby A (1978) Proton spin relaxation in liquid polydimethylsiloxane: molecular motion and network formation. J Polym Sci Phys Ed 16:1041–1057. https://doi.org/10.1002/pol.1978.180160611
Folland R, Charlesby A (1979) Pulsed n. m. r. of cis-polyisoprene: 1. Polymer 20:207–210. https://doi.org/10.1016/0032-3861(79)90223-4
Folland R, Charlesby A (1979) Pulsed n. m. r. of cis-polyisoprene: 2. Polymer 20:211–214. https://doi.org/10.1016/0032-3861(79)90224-6
Ukawa J, Kawahara S, Sakai J (2007) Structural characterization of vulcanized natural rubber by latex-state 13C NMR spectroscopy. J Polym Sci: PartB: Polym Physics 45:1003–1009. https://doi.org/10.1002/polb.21076
Kwahara S (2011) Latex-state and solid-state NMR spectroscopy of elastomers, in ACS symposium series, 1077 (NMR Spectroscopy of Polymers), pp. 475–494. https://doi.org/10.1021/bk-2011-1077.ch029
Sea-heng K et al (2017) Latex-state NMR spectroscopy for quantitative analysis of epoxidized deprotenized natural rubber. Polym Adv Technol 28:1156–1161. https://doi.org/10.1002/pat.4008
Fukuhara L et al (2015) Study on the resolution of latex-state NMR spectroscopy. Kobunshi Ronbunshu 72:22–30. https://doi.org/10.1295/koron.2014-0066
Lovell PA, Shah TH, Heatley F (1991) Chain transfer to polymer in emulsion polymerization of n-butyl acrylate studied by carbon-13 NMR spectroscopy and gel premeation chromatography, polymer communications, 32, 98–103
Kawamura T, Toshima N, Matsuzaki K (1995) Assingment of finely resolved 13C-NMR spectra of polyacrylates. Macromol Chem Phys 196:3415–3424. https://doi.org/10.1002/macp.1995.021961026
Pichot C, Llauro MF, Pham QT (1981) Microstructure of vinyl acete-butyl acrylate copolymers studied dy 13C-NMR spectroscopy: influence of emulsion polymerization process. J Polym Sci Part A Polym Chem 19:2619–2633. https://doi.org/10.1002/pol.1981.170191021
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This work was supported in part by a Grant-in-Aid (16H02291) for Scientific Research (A) from the Japan Society for the Promotion of Science.
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Iizuka, Y., Yamamoto, Y. & Kawahara, S. Latex-state 13C-NMR spectroscopy for poly(butyl acrylate). Colloid Polym Sci 297, 133–139 (2019). https://doi.org/10.1007/s00396-018-4444-2
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DOI: https://doi.org/10.1007/s00396-018-4444-2