Preparation of poly(arylene ether ketones) by sequential oligomerization and polymerization in distinct reaction zones

摘要

A method of preparing a poly(arylene ether ketone) by a Friedel-Crafts polymerization wherein a gelled reaction mixture is produced, comprising the steps of:PP(A) forming, in a first reactor, a reaction mixture for polymerization comprisingP P(I) a monomer system comprisingPP(a) (i) phosgene or an aromatic dicarboxylic acid dihalide and (ii) a substantially stoichiometric amount of a polynuclear aromatic comonomer having two active hydrogen atoms orPP(b) a polynuclear aromatic carboxylic acid halide having an active hydrogen atom; and P P(II) a Lewis acid in an amount of at least one equivalent per equivalent of carbonyl groups in the monomer system, plus an amount effective to act as a catalyst for the polymerization;PP (B) permitting the reaction mixture to polymerize in the first reactor until substantial partial polymerization has occurred, but before substantial gelation of the reaction mixture;PP(C) transferring the partially polymerized reaction mixture into a second reactor having a nozzle at one end thereof and a piston which, in its retracted position, is at the other end of the second reactor and has a stroke substantially equal to the length of the second reactor;P P(D) permitting polymerization to continue in the second reactor until a gelled, polymerized reaction mixture containing polymer of the desired molecular weight has been obtained;PP(E) discharging the gelled, polymerized reaction mixture from the second reactor through the nozzle by stroking the piston the length of the second reactor; andPP(F) recovering and purifying the polymer.