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• W2016072040 abstract "Accelerated-sulfur-vulcanized 13C-labeled EPDM with and without carbon black and extender oil was analyzed using 13C solid-state NMR to determine the chemical structure of the network. High-resolution solid-state 13C NMR reveals that sulfur cross-linking takes place at the allylic positions of the ENB independent of the presence of carbon black and oil. From the integrated intensities of the 13C signals, the conversion of ENB into a cross-link can be quantitatively determined during the vulcanization process. The ENB conversion for gumstock EPDM is ∼10% after 10 min of vulcanization at 150 °C, which is a typical optimum vulcanization time in commercial applications. In the presence of carbon black the ENB conversion is marginally faster and reaches ∼12% in 10 min, while a maximum conversion of ∼20% was obtained. The efficiency of the ENB conversion was ∼20% less at 150 °C and ∼30% less at 180 °C in the compound with carbon black and oil compared to the compound without carbon black and oil. The substitution at the 9-position of ENB is always preferred over each of the two 3-positions. In turn, the substitution on the 3-exo position is always preferred over the 3-endo position, which is different from earlier model studies. When the material is heated for extended periods (10−20 min), oxidation and reversion of the cross-links starts to occur. Reversion is enhanced upon a temperature increase to 180 °C and yields a 4,5,6,7-tetrahydro-4,7-methanobenzo[b]thiophene compound. The length of the sulfur bridge in compound A and B is rather short, i.e., 1 or 2." @default.
• W2016072040 created "2016-06-24" @default.
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• W2016072040 date "2002-01-26" @default.
• W2016072040 modified "2023-10-01" @default.
• W2016072040 title "Solid-State ¹³C NMR Study of Accelerated-Sulfur-Vulcanized ¹³C-Labeled ENB−EPDM" @default.
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• W2016072040 doi "https://doi.org/10.1021/ma001716h" @default.
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