Preparing methyl formate comprises e.g. homogeneous-catalyzed reaction of mixture of e.g. hydrogen, catalyst and tertiary amine compound, phase separation of hydrogenated mixture, and extraction of catalyst residue with the compound

摘要

Preparing methyl formate comprises (a) homogeneous-catalyzed reaction of a reaction mixture containing e.g. a polar solvent and a tertiary amine compound (I) to obtain hydrogenated mixture comprising e.g. solvent containing (I) and a formic acid amine adduct (II); (b) phase separation of hydrogenated mixture to obtain lower phase and upper phase; (c) extraction of residues of catalyst with (I) to obtain raffinate and extract; (d) optionally partial separation of polar solvent from the raffinate to obtain a distillate and a regenerated raffinate; and (e) partially reacting (II) with methanol. Preparing methyl formate comprises (a) homogeneous-catalyzed reaction of a reaction mixture containing carbon dioxide, hydrogen, at least one catalyst containing at least one element of group 8-10 of the periodic system, at least one polar solvent and at least one tertiary amine compound of formula (NR1R2R3) (I), in a hydrogenation reactor (I-1) to obtain a hydrogenated mixture comprising at least one catalyst and the polar solvent that comprises (I) and at least one formic acid amine adduct of formula (NR1R2R3.x iHCOOH) (II); (b) phase separation of the hydrogenated mixture in a first phase separation device (II-1) to obtain a lower phase comprising (II), the polar solvents and the residues of the catalyst, and an upper phase comprising the catalyst and (I); (c) extraction of the residues of the catalyst in an extraction unit (III-1) with (I) to obtain a raffinate comprising (II) and the polar solvents and an extract comprising (I) and the residue of the catalyst; (d) optionally at least partial separation of the polar solvent from the raffinate in a first distillation device to obtain a distillate comprising the polar solvents and a regenerated raffinate comprising (II); and (e) at least partially reacting (II) contained in the raffinate and/or regenerated raffinate, with methanol in a reactive distillation column (V-1) to methyl formate, water and (I). Either R1-R3 : optionally branched 1-16C-acyclic or -cyclic, 1-16C-aliphatic, -araliphatic or -aromatic groups, where the groups are optionally substituted by a hetero atom comprising O or N, preferably 2-8C-alkyl, 5-8C-cycloalkyl, benzyl or phenyl; or two or all R1-R3 linked together : four atom containing chain; and x i0.4-5.