Advertisement

Colloid and Polymer Science

, Volume 297, Issue 1, pp 133–139 | Cite as

Latex-state 13C-NMR spectroscopy for poly(butyl acrylate)

  • Yusuke Iizuka
  • Yoshimasa Yamamoto
  • Seiichi KawaharaEmail author
Original Contribution
  • 47 Downloads

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.

Keywords

Latex-state 13C-NMR Poly(butyl acrylate) Local motion 

Notes

Funding information

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.

Compliance with ethical standards

This work complies with ethical standards.

Conflict of interest

The authors declare that they have no conflict of interest.

References

  1. 1.
    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 CrossRefGoogle Scholar
  2. 2.
    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 CrossRefGoogle Scholar
  3. 3.
    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 CrossRefGoogle Scholar
  4. 4.
    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 CrossRefGoogle Scholar
  5. 5.
    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 CrossRefGoogle Scholar
  6. 6.
    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 CrossRefGoogle Scholar
  7. 7.
    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 CrossRefGoogle Scholar
  8. 8.
    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 CrossRefGoogle Scholar
  9. 9.
    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 CrossRefGoogle Scholar
  10. 10.
    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 CrossRefGoogle Scholar
  11. 11.
    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 CrossRefGoogle Scholar
  12. 12.
    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
  13. 13.
    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 CrossRefGoogle Scholar
  14. 14.
    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 CrossRefGoogle Scholar
  15. 15.
    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, 98–103Google Scholar
  16. 16.
    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 CrossRefGoogle Scholar
  17. 17.
    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 CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Yusuke Iizuka
    • 1
  • Yoshimasa Yamamoto
    • 2
  • Seiichi Kawahara
    • 1
    Email author
  1. 1.Department of Material Science and TechnologyNagaoka University of TechnologyNiigataJapan
  2. 2.Department of Mechanical Engineering, National Institute of TechnologyTokyo CollegeTokyoJapan

Personalised recommendations