Two-Phase Network Formation in Sulfur Crosslinking Reaction of Isoprene Rubber

Synchrotron in situ zinc K‐edge X‐ray absorption near‐edge structure measurements are conducted during sulfur crosslinking reactions of isoprene rubber at 140 °C. A two‐phase network formation via two different reactions is revealed in a benzothiazolesulfenamide‐accelerated curing system with zinc o...

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Bibliographic Details
Published in:Macromolecular chemistry and physics 2014-05, Vol.215 (10), p.971-977
Main Authors: Yasuda, Yoritaka, Minoda, Shinya, Ohashi, Takumi, Yokohama, Hiroyuki, Ikeda, Yuko
Format: Article
Language:English
Subjects:
Applied sciences
Chemical reactions and properties
Crosslinking
Crosslinking, vulcanization
Exact sciences and technology
in situ measurements
Isoprene rubber
Network formation
network inhomogeneity
Networks
Organic polymers
Physicochemistry of polymers
Sulfur
sulfur crosslinking
Synchrotrons
Vulcanization
Vulcanizing
Zinc
zinc K-edge X-ray absorption fine structure spectroscopy
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Summary:Synchrotron in situ zinc K‐edge X‐ray absorption near‐edge structure measurements are conducted during sulfur crosslinking reactions of isoprene rubber at 140 °C. A two‐phase network formation via two different reactions is revealed in a benzothiazolesulfenamide‐accelerated curing system with zinc oxide and stearic acid. DSC measurements support this observation. The results are in good agreement with previous work using small‐angle neutron scattering, where network domains of high network‐chain density are proposed to be embedded in a mesh network. A formation of the mesh network is found to occur a little earlier than that of the network domains, and its fraction is unexpectedly observed to be larger than that calculated on the basis of a concentration of zinc stearate. The result is ascribable to amounts of zinc intermediates forming the mesh network. This study may be the first in situ evaluation for the inhomogeneous network formation during vulcanization. Synchrotron time‐resolved zinc K‐edge X‐ray absorption near‐edge structure measurements show two‐phase network formation at 140 °C via two different reactions during the benzothiazolesulfen­amide‐accelerated sulfur crosslinking reaction of isoprene rubber with ZnO and stearic acid. DSC measurements support the observation. This study may be the first in situ evaluation for the inhomogeneous network formation during the vulcanization.
ISSN:1022-1352
1521-3935
DOI:10.1002/macp.201400066