Preparation of metallocene compound, useful e.g. in the preparation of isotactic polypropylene, comprises using a cyclopentadienyl derivative that is recycled from the filtrate obtained from the preparation of e.g. metallocene compound

摘要

Preparation of metallocene compound (III) comprises using recycled cyclopentadienyl derivative (I) or (Ib) and/or its double bonded isomer or biscyclopentadienyl derivative (II) and/or its double bonded isomer, where (I) or (Ib) and/or (II) is recycled by partially removing from the filtrate, mother liquor, reaction residues and/or reconditioning residue that are obtained in the preparation of (III) and/or biscyclopentadienyl ligand and subsequently purified by means of liquid-solid-chromatography. Preparation of metallocene compound of formula (III) comprises using recycled cyclopentadienyl derivative of formula (I) or (Ib) and/or its double bonded isomer or biscyclopentadienyl derivative of formula (II) and/or its double bonded isomer, where (I) or (Ib) and/or (II) is recycled by partially removing from the filtrate, mother liquor, reaction residues and/or reconditioning residue that are obtained in the preparation of (III) and/or biscyclopentadienyl ligand and subsequently purified by means of liquid-solid-chromatography. Either R 1>,R1a : 1-40C organic residue; and R 2>,R2a : H or 1-40C organic residue; or R 1>R 2>,R1aR2a : optionally saturated and substituted 3-40 (preferably 5-12)C mono- or polycyclic ring (containing a heteroatom such as Si, Ge, N, P, As, Sb, O, S, Se or Te); T,Ta : double bonded 1-40C organic group that forms together with the cyclopentadienyl ring, respectively at least a further optionally saturated and substituted ring system shows a ring size of 5-12 atoms, where T, Ta in the cyclopentadienyl annealed ring system contains heteroatom such as Si, Ge, N, P, As, Sb, O, S, Se or Te; Z : a bond between both substituted cyclopentadienyl ligand containing double bonded atom or double bonded group; M : an element of the 3rd, 4th, 5th or 6th group or lanthanide; X : an organic or inorganic residue, where two residues can be connected; n : 0-3; and m : 0-1. An independent claim is included for a procedure for the recovery of cyclopentadienyl derivative comprising aqueous treating of the filtrate, mother liquor, reaction residues and/or reconditioning residue that are obtained in the preparation of silicon-bound metallocene and/or silicon-bound biscyclopentadienyl ligand with one or more acid or base and isolating and optionally concentrating to purify using liquid-solid chromatography. [Image] [Image].