C - Chemistry – Metallurgy – 07 – C
Patent
C - Chemistry, Metallurgy
07
C
202/69, 260/482.
C07C 69/54 (2006.01) C07C 67/08 (2006.01)
Patent
CA 1083601
ABSTRACT OF THE DISCLOSURE: Alkyl acrylates free from ether are made continuously by reacting acrylic acid with a C1-C4- alkanol, in a molar ratio of 1:1 to 1:2, in liquid phase, at 80 to 130°C, under 100 to 760 mm Hg, in the presence of an acid catalyst. More specifically, a reaction mixture of acrylic acid, alkanol and a sulfuric acid or organic sulfonic acid catalyst is continuously introduced into a reaction zone, the reaction mixture containing sulfuric acid in a concentration of 0.1 to 3 weight %, or the organic sulfonic acid in a concentration of 1 to 8 weight %. Reacting the reaction mixture over a period of 4 to 10 hours in the reaction zone. An azeotropic mixture of alkyl acrylate, reaction water and unreacted alkanol is distilled off near the head of a first distilling zone mounted on the reaction zone. The mixture is condensed and separated into an aqueous phase and organic phase. A portion of the organic phase and, in the event of the alkanol used being a C3 or C4-alkanol, also a portion of the aqueous phase are recycled to the head of the first distilling column, and remaining aqueous phase is removed. The - 2 - balance portion of the organic phase is delivered to a second distilling zone, an azeotropic mixture of alkanol and ester, is distilled off overhead, condensed and recycled to the reaction zone, and ether-free alkyl acrylate is removed from the base portion of the second distilling zone. A portion of reaction mixture is continuously taken from the reaction zone, distillatively freed from high-boiling matter, the resulting distillate is admixed with a quantity of catalyst equivalent to that removed together with said high-boiling matter, and then recycled to the reaction zone.
266125
Erpenbach Heinz
Gehrmann Klaus
Kubbeler Hans-Klaus
Lork Winfried
Fetherstonhaugh & Co.
Hoechst Aktiengesellschaft
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