Mr. Krejsa et Jl. Koenig, SOLID-STATE C-13 NMR-STUDIES OF ELASTOMERS .11. N-T-BUTYL BENZOTHIAZOLE SULFENIMIDE ACCELERATED SULFUR VULCANIZATION OF CIS-POLYISOPRENE AT75 MHZ, Rubber chemistry and technology, 66(1), 1993, pp. 73-82
The network structure of TBSI-accelerated vulcanization of cis-polyiso
prene was studied using C-13 solid-state NMR. The initial crosslink pr
oducts consisted of A1c (cis) and A2c (cis) polysulfides. As the perce
nt cure is increased, the A1c and A2c structures reduce in rank to mon
osulfides, and polysulfidic B1c (cis) and B1t (trans) structures are f
ormed. During the maturation period C1c (cis) polysulfidic structures
are also formed. The percent of sulfurization was shown to vary direct
ly with sulfur concentration, while the efficiency of sulfurization (c
rosslink/cyclic-structure ratio) was shown to vary with accelerator co
ntent. TBSI-accelerated vulcanization was found to be more inefficient
(lower crosslink/cyclic-structure ratio) than TBBS-accelerated vulcan
ization during the initial cure region. However, this results in short
er sulfur chains, which decreases the reactivity of TBSI vulcanizates
as compared to TBBS vulcanizates during the reversion regime.