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Preparation, characterization, and thermal properties of controllable metal–imidazole complex curing agents for epoxy resins

✍ Scribed by Julie Brown; Ian Hamerton; Brendan J. Howlin


Publisher
John Wiley and Sons
Year
2000
Tongue
English
Weight
229 KB
Volume
75
Category
Article
ISSN
0021-8995

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✦ Synopsis


A series of complexes incorporating the epoxy-imidazole adduct of phenyl glycidyl ether with 2-ethyl-4-methylimidazole (PGE-EMI), has been prepared with the acetato and chloro transition metal salts of Mn, Co, Ni, Cu, Zn, and Ag. These complexes have been characterized using spectroscopic methods (IR, UV-Vis, 1 H-and 13 C-NMR, where appropriate) and their thermal stabilities have been determined using elevated temperature NMR techniques. These high-temperature NMR results indicated that the chloro complexes studied (of Mn 2ϩ , Co 2ϩ , Ni 2ϩ , Cu 2ϩ , and Zn 2ϩ ) exist in equilibrium (i.e., they dissociate reversibly in a solution of dimethylsulphoxide, DMSO, at elevated temperatures), while the corresponding acetato complexes dissociate irreversibly. For the silver complexes, thermogravimetric analysis (TGA) was used to monitor the dissociation, showing that the weight loss recorded was consistent with the dissociation of the metal salt to liberate the PGE-imidazole ligand. The thermal stabilities of the metal complexes were influenced by changing both the transition metal (e.g., from Mn to Zn) and varying the anion (e.g., from acetate to chloride). From 1 H-NMR analysis, a decrease of ca. 10°C was observed in the thermal dissociation of the acetato complexes when compared with the chloro complexes, showing that the series of PGE-EMI complexes with acetate anions is less thermally stable than the corresponding chlorides. This finding suggests that these PGE-EMI complexes may be modified to accommodate their use in a variety of different curing schedules when used to cure epoxy resins.


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