Highly active, recyclable catalyst for the manufacture of viscous, low molecular weight, CO-ethene-propene-based polyketone, base component for a new class of resins

A highly active, recyclable homogeneous palladium(II) catalyst is described for the manufacture of viscous, low molecular weight CO-ethene-propene-based polyketone (Carilite Oligomer), used for the manufacture of a new class of resins (Carilite Resins). The catalyst is composed of palladium acetate, and a sulfonated diphosphine ligand, bdompp-S (1,3-bis(di-(2-methoxy, 5-sulfonatophenyl)phosphino)propane). In comparison with its non-sulfonated counterpart this catalyst not only exhibits a much more favourable partitioning coefficient in liquid-liquid separation of the polyketone product and solvent, but it also exhibits an approximately 2.5 times higher catalytic activity (up to 11.2 kg PK (g Pd)(-1)h(-1)) in the manufacture of PK-PE-30 (polyketone terpolymer built up of CO, ethene and propene in a molar ratio of 100:30:70). A variety of salts were found to exert a positive influence on the activity of the catalyst. Possible origins of this 'salt-effect' are briefly discussed. The bdompp-S ligand was synthesised by sulfonation of bdompp using either a boric acid-oleum mixture or sulfuric acid as the sulfonation reagent. The product was isolated either as sodium-salt (bdompp-S[Na](4)(.)nNa(2)SO(4)), by extraction with methanol after neutralisation, or, in acidic, hydrated form (bdompp-S[H}(4)(.)nH(2)O), via a new and highly efficient procedure, i.e. cooling the reaction mixture after dilution with water. The X-ray crystal structure of bdompp-S[H](4)(.)nH(2)O is discussed. (C) 2002 Elsevier Science B.V. All rights reserved.