화학공학소재연구정보센터
Macromolecules, Vol.31, No.4, 1214-1220, 1998
Location of the antiplasticizer in cross-linked epoxy resins by H-2, N-15, and C-13 REDOR NMR
Carbon-13 rotational-echo double-resonance (REDOR) NMR with N-15 or H-2 dephasing, combined with N-15 REDOR NMR with C-13 dephasing, has been obtained for a fully cross-linked epoxy resin prepared from a nominally uniform mixture of two parts of diglycidyl ether of Bisphenol A, one part of hexamethylenediamine, and 19% (by weight) antiplasticizer made from a carbonyl-C-13-labeled aromatic acetamide. The antiplasiticizer contains the hydroxypropyl ether moiety of the epoxy repeat unit. A partially cross-linked resin was formed from five parts of epoxide, one part of hexamethylenediamine, three parts of hexylamine, and 19% (by weight) antiplasticizer. Labels were introduced into the resin by replacing both methyl groups of the isopropylidene moiety of Bisphenol A with CD3 groups and by using [N-15(2)]hexamethylenediamine and [N-15]hexylamine (and their unlabeled counterparts) in various combinations. The antiplasticizer C-13-carbonyl carbon is 4.9 +/- 0.5 Angstrom from an amine N-16 (With no preference for free or cross-linked sites) and 6.7 +/- 1 Angstrom from a quaternary carbon of the isopropylidene moiety.