Recovery of trialkylamines and methyl formate from mixtures obtained in the preparation of trimethylolalkanes

US5149861A · kind A · utility

Assignee

• BASF SE

Inventors

• Franz Merger · Bischofswerda, DE
• Peter Hettinger · Haus Ferring, DE
• Leopold Hupfer · Friedelsheim, DE
• Juergen Paetsch · Monsheim, DE
• Heribert Deck · Ludwigshafen, DE
• Heinz Auer · Neulußheim, DE
• Erwin Brunner · Meiningen, DE

Key dates

• Filing date: Mar 1, 1991
• Grant date: Sep 22, 1992
• Expiry date: Mar 1, 2011

Classification

• Technology area (CPC C): Chemistry; Metallurgy
• CPC primary: C07C67/03
• WIPO field: Organic fine chemistry
• WIPO sector: Chemistry

Abstract

Trialkylamines and methyl formate are recovered from reaction mixtures obtained in the preparation of trimethylolalkanes by reaction of n-alkanals with from 2.2 to 4.5 moles of formaldehyde in aqueous solution in the presence of from 0.6 to 3 mole of trialkylamine, each quantity based on 1 mole of alkanal, and subsequent hydrogenation in a process wherein the crude reaction mixture PA1 a) is heated to from 100.degree. to 200.degree. C., the water present in the reaction mixture is substantially separated off by distillation, together with any excess free trialkylamine, the trialkylamine present in the form of a trialkylammonium formate is freed to form a trimethylolalkane formate, the trialkylamine is distilled off and the trimethylolalkane formate is transesterified with methanol to trimethylolalkane and methyl formate in the presence or absence of a catalytic amount of an alkali metal alkoxide or alkaline earth metal alkoxide, or PA0 b) is substantially dewatered, any excess free trialkylamine being removed at the same time, the trialkylamine present in the form of a trialkylammonium formate is separated off by admixing the remaining mixture with methanol and heating the admixtur…