POLY(ARYL ETHER KETONE) BLOCK AND CHAIN-EXTENDED COPOLYMERS .1. PREPARATION AND CHARACTERIZATION OF A NEW CLASS OF FUNCTIONAL POLY(ARYL ETHER KETONE) OLIGOMERS
Ra. Clendinning et al., POLY(ARYL ETHER KETONE) BLOCK AND CHAIN-EXTENDED COPOLYMERS .1. PREPARATION AND CHARACTERIZATION OF A NEW CLASS OF FUNCTIONAL POLY(ARYL ETHER KETONE) OLIGOMERS, Macromolecules, 26(9), 1993, pp. 2361-2365
A series of poly(aryl ether ketone) (PAEK) oligomers with controlled m
olecular weights and end groups has been prepared via the Friedel-Craf
ts reaction of terephthaloyl chloride with diphenyl ether in the prese
nce of either p-fluorobenzoyl chloride or fluorobenzene as the chain-t
erminating agents. The p-fluorobenzoyl chloride route is preferred, an
d the reaction is carried out in 1,2-dichloroethane, at 20-30 wt % sol
ids, in the presence of a 30-40 mol % excess of aluminum chloride. A t
roublesome side reaction involving alkylation of the benzene rings is
minimized under these conditions and is further minimized by the addit
ion of a complexing agent. The oligomers were characterized by fluorin
e content, C-13 NMR, laser desorption-mass spectrometry, and GPC, whic
h proved to be a powerful tool for the determination of purity. The fl
uorine contents agreed well with calculated values indicating a high d
egree of difunctionality.