The reaction of gibbsite (a modification of Al(OH) 3 ) in glycol at elevated temperatures yielded the glycol derivative of boehmite together with a small amount of well-crystallized boehmite and a residue of unreacted gibbsite. The addition of water to the medium increased the reactivity of gibbsite and yielded a novel phase having a large basal spacing. Pure product of this phase was obtained by the reaction of microcrystalline gibbsite (<0.2 μm) in 75 vol % ethylene glycol−water or in 95% 1,4-butanediol−water at 250 °C for 2 h. XRD analysis showed that the products had the boehmite layer structure and that the difference between the basal spacings of the present products and those of the corresponding glycol derivatives of boehmite obtained in pure glycols was about the same as the thickness of a boehmite layer. IR spectra of the present products exhibited a band due to hydrogen bonding between the boehmite layers. These results suggest that the products are the glycol derivatives of boehmite having the second stage structure. 2-Methoxyethyl and 2-(dimethylamino)ethyl derivatives of boehmite having the second stage structure were also formed by the similar reactions in 2-methoxyethanol and N,N -dimethylethanolamine, respectively.
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Inoue et al. (1997) studied this question.
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