Multistage continuous preparation of (cyclo) aliphatic...

C - Chemistry – Metallurgy – 07 – C

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C07C 263/06 (2006.01) C07C 265/14 (2006.01)

Patent

CA 2478743

Disclosed is a multistage process for a continuous and phosgene-free preparation of a (cyclo)aliphatic diisocyanate. The process comprises (A) reacting a (cyclo)aliphatic diamine of the formula: H2N-R-NH2 (in which R is a bivalent (cyclo)aliphatic hydrocarbon radical) with urea and an alcohol of the formula: R1-OH (in which R1 is an aliphatic or cycloaliphatic radical) to form a (cyclo)alkylenebisurea of the formula: H2N-OC-HN-R-NH-CO-NH2; (B) converting the (cyclo)alkylenebisurea with the alcohol to a (cyclo)alkylenediurethane of the formula: R1O-OC-HN-R-NH-CO-OR1 in a reaction mixture which also contains low, medium and high boiler by-products; (C) removing the low, medium and high boiler impurities from the (cyclo)alkylenediurethane; (D) thermally cleaving the (cyclo)alkylenediurethane to form the (cyclo)aliphatic diisocyanate of the formula: OCN-R-NCO; (E) discharging a portion of a cleavage residue from a cleavage apparatus and reurethanizing it with the alcohol to obtain a reurethanization product; and (F) recycling the reurethanization product directly into the low-boiler impurity removed.

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