Abstract
Attempts have been made to accelerate the direct reaction of coal OH groups with phosphorylating reagents, e.g. Ph 2PCl, (PhO) 2PCl and (EtO) 2PCl, by use of microwave heating. Results for coals and model compounds, e.g. 2,4,6-tri- t-butylphenol and 2-phenylphenol, show that various reactions are accelerated, e.g. oxidation, P(III)→P(V), hydrolysis, PCl→POH, solvolysis, PEtO→POH, and in some cases replacement of -OEt by -OR, where R = 2,4,6-tri- t-butylphenyl. Surprisingly, under these circumstances some progress could be made identifying the origin of some 31P MAS n.m.r. resonances from coals phosphorylated with (EtO) 2PCl under microwave heating. These data are discussed. No possibility was found of developing quantitative methods of analysis based on rapid ‘one-pot’ derivation using phosphorylating reagents followed by in situ quantitative 31P MAS n.m.r. spectroscopy.
Published Version
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