Two synthetic routes were used for the preparation of aromatic poly(ether ketones): Friedel‐Crafts acylation and aromatic nucleophilic substitution. The first route involved the reaction of diphenyl ether and terephthalic acid dichloride in trifluoromethane‐sulfonic acid. The addition of trifluoromethanesulfonic anhydride or phosphorus pentoxide resulted in increased molecular weights. The second synthetic route involved the synthesis of an amorphous tert ‐butyl‐substituted poly(ether ketone) prepolymer. Subsequently, the tert ‐butyl groups were removed by a reversed Friedel‐Crafts alkylation reaction yielding the crystalline polymer PEEK. The dealkylation reaction was performed in trifluoromethanesulfonic acid. The addition of a tert ‐butyl group acceptor resulted in high dealkylation conversions.
SynopsisAn atmospheric-pressure, vapor-phase polymerization technique was used to deposit thin (1-10 pm) poly(p-phenyleneterephthalamide) coatings onto polyester film and other sheet substrates. A minimum deposition temperature of 17OOC was found to be critical. When substrate temperatures were below 17OoC, coatings were loosely adhered, powdery, and of low molecular weight; above 17OoC, coherent, well-adhered, high molecular weight coatings were obtained. These vapor-deposited coatings exhibited exceptionally good oxygen barrier properties and were found to consist of fused 0.1-pm particulates. Scanning electron microscopy (SEM) of the top surfaces of these coatings clearly revealed their particulate origin. Similar evidence was also obtiined from SEM examination of fracture surfaces and transmission electron microscopy of microtomed sections. The coalescence of these coatings was demonstrated by SEM of plasma-etched surfaces and oxygen permeability information. The uniplanar orientation of the polymer crystals in these multiparticulate coatings was strong evidence for the epitaxial growth of the crystals.
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