| US 7,468,456 B2 | ||
| Azeotropic distillation process for separating acetic acid, methylacetate and water in the production of an aromatic carboxylic acid | ||
| Myron Myonkee Lee, Seongnam-si (Korea, Republic of); Duk-Jun Kwon, Seoul (Korea, Republic of); Dong-Won Lee, Anyang-si (Korea, Republic of); and Alexander Jongwon Lee, Seongnam-si (Korea, Republic of) | ||
| Assigned to ANT Corporation, Gyeonggi-do (Korea, Republic of) | ||
| Filed on Jul. 11, 2006, as Appl. No. 11/484,801. | ||
| Claims priority of application No. 10-2005-0070358 (KR), filed on Aug. 01, 2005. | ||
| Prior Publication US 2007/0027340 A1, Feb. 01, 2007 | ||
| Int. Cl. C07C 51/16 (2006.01); C07C 51/265 (2006.01) | ||
| U.S. Cl. 562—409 [562/414] | 7 Claims |
| 1. In a process of manufacturing an aromatic carboxylic acid in which an aromatic alkyl hydrocarbon is oxidized with an oxygen-containing
gas in acetic acid solution, at a temperature within the range of 150 to 220° C. and at a pressure within the range of 10
to 25 kg/cm (abs.), and in the presence of a catalyst system containing cobalt, manganese and bromine, whereby water and methyl
acetate are produced as the by-products of oxidation, and a portion of the condensed liquid from the overhead vapor stream
of the oxidation reactor and other dilute acetic acid streams, containing mostly water and methyl acetate, the portion of
the condensed liquid and the other dilute acetic acid are collectively called “said feed stream” below, are sent to the dehydration
unit where water and methyl acetate are separated from acetic acid, the improvement in the recovery of the acetic acid and
the methyl acetate comprises the following steps:
(a) feeding said feed stream containing mostly acetic acid, water and methyl acetate to an azeotropic distillation column
in which the azeotropic agent is the same aromatic alkyl hydrocarbon as the feedstock used for the production of the aromatic
carboxylic acid;
(b) withdrawing concentrated acetic acid from the bottom of said azeotropic distillation column, condensing the vapor stream
of said azeotropic distillation column that is comprised of the azeotropic agent, water and methyl acetate, feeding the liquid
condensate to a decanter, separating said condensate into an aqueous phase and an organic phase, refluxing a small portion
of the aqueous-phase liquid and a major portion of the organic-phase liquid to the top region of said azeotropic distillation
column, withdrawing a major portion of the aqueous-phase liquid comprised predominantly of water and methyl acetate, withdrawing
a small portion of the organic-phase liquid comprised predominantly of the azeotropic agent and small amounts of methyl acetate
and water;
(c) recycling said concentrated acetic acid and the withdrawn organic-phase liquid to the oxidation reactor section of the
aromatic alkyl hydrocarbon, and supplying the withdrawn aqueous-phase liquid to a distillation column in which water and methyl
acetate are separated from the bottom and the top of said distillation column, respectively,
wherein the azeotropic agent is the very same aromatic alkyl hydrocarbon which is supplied as the reactant for the oxidation
reaction, without separately adding any other azeotropic agent in the azeotropic distillation column.
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