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EP0350635B1 Expired / Lapsed EP ⏱️ 0.0 years remaining

Process for the preparation of acetic acid and acetic anhydride

Assignee: Celanese Sales Germany GmbH
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Filing: 1989-06-14
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Granted: 1993-09-29
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Expires: 2009-06-14
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Abstract

Abstract For the preparation of acetic acid and acetic anhydride, methanol and methyl acetate are reacted under anhydrous conditions with carbon monoxide in the presence of a carbonyl complex of group VIII noble metals, methyl iodide, and catalyst systems containing alkali metal or quaternary organophosphonium or organoammonium acetate or iodide. The hot carbonylation mixture is depressurised, the evaporated components are added to a first distillation zone, and the remaining catalyst solution is fed back to the reaction zone. In the first distillation zone, the volatile carbonylation products are fractionally distilled; the low-boiling components methyl iodide and methyl acetate pass back into the reaction zone, and a mixture of acetic acid and acetic anhydride is obtained as a bottom product which is separated into the pure components in a second and third distillation zone.

Inventors

  • 👤 Heinz Dr. Erpenbach
  • 👤 Klaus Dr. Gehrmann
  • 👤 Erhard Dr. Jägers
  • 👤 Georg Kohl

Bibliographic Details

Application Number —
Jurisdiction EP
Data Source google_patents
Last Synchronized 2026-11-08 20:16
CPC Classifications
C; C07; C07C; C07C53/00; C07C53/08; C07C51/00; C07C51/10; C07C51/12; C07C51/54; C07C51/56; C07C53/12

Claims Analysis

Total Claims: 11
Claim 1
Independent Claim 362 words
A process for the preparation of acetic acid and acetic anhydride by reacting methanol and methyl acetate with carbon monoxide, wherein a) methanol and methyl acetate in the molar ratio 10 : 1 to 1 : 10 are reacted under anhydrous conditions with carbon monoxide or mixtures of carbon monoxide and hydrogen in the presence of a carbonyl complex of noble metals from group VIII of the Periodic Table of the Elements, methyl iodide and, as promoter, a catalyst system containing an acetate or iodide of an alkali metal, quaternary organophosphonium or organoammonium, in a reaction zone at temperatures of from 150 to 250 ° C and pressures of from 5 to 120 bar; b) the carbonylation mixture leaving the reaction zone at a temperature of from 150 to 250 °C is decompressed to a pressure of from 1 to 3.5 bar in a vapor-liquid deposition zone, the major part of the volatile components evaporating immediately and, in order to prevent entrainment of liquid drops, being fed via a mist eliminator to a first distillation zone for removal of the low-boiling components; the major part of the still-volatile components is distilled off in a separation zone at a pressure of from 0.05 to 1 bar and a bottom temperature of from 50 to 170°C from the liquid stream produced in the vapor-liquid deposition zone and in the mist eliminator and is likewise fed to the first distillation zone, and the catalyst solution which remains as the bottom product is fed back to the reaction zone; c) the volatile carbonylation products are split in the first distillation zone by fractional distillation under atmospheric pressure into a low-boiling component predominantly comprising methyl iodide and methyl acetate, and are fed back into the reaction zone, and the bottom product obtained is a mixture of acetic acid and acetic anhydride; d) in order to remove traces of iodine-containing compounds, the mixture of acetic acid and acetic anhydride is passed over a carrier containing a silver salt or treated with peracetic acid, and is split into the pure components, acetic acid and acetic anhydride, by fractional distillation in a second distillation zone and a third distillation zone.
Claim 2
Dependent Claim 362 words
A process for the preparation of acetic acid and acetic anhydride by reacting methanol and methyl acetate with carbon monoxide, wherein a) methanol and methyl acetate in the molar ratio 10 : 1 to 1 : 10 are reacted under anhydrous conditions with carbon monoxide or mixtures of carbon monoxide and hydrogen in the presence of a carbonyl complex of noble metals from group VIII of the Periodic Table of the Elements, methyl iodide and, as promoter, a catalyst system containing an acetate or iodide of an alkali metal, quaternary organophosphonium or organoammonium, in a reaction zone at temperatures of from 150 to 250 ° C and pressures of from 5 to 120 bar; b) the carbonylation mixture leaving the reaction zone at a temperature of from 150 to 250 °C is decompressed to a pressure of from 1 to 3.5 bar in a vapor-liquid deposition zone, the major part of the volatile components evaporating immediately and, in order to prevent entrainment of liquid drops, being fed via a mist eliminator to a first distillation zone for removal of the low-boiling components; the major part of the still-volatile components is distilled off in a separation zone at a pressure of from 0.05 to 1 bar and a bottom temperature of from 50 to 170°C from the liquid stream produced in the vapor-liquid deposition zone and in the mist eliminator and is likewise fed to the first distillation zone, and the catalyst solution which remains as the bottom product is fed back to the reaction zone; c) the volatile carbonylation products are split in the first distillation zone by fractional distillation under atmospheric pressure into a low-boiling component predominantly comprising methyl iodide and methyl acetate, and are fed back into the reaction zone, and the bottom product obtained is a mixture of acetic acid and acetic anhydride; d) in order to remove traces of iodine-containing compounds, the mixture of acetic acid and acetic anhydride is passed over a carrier containing a silver salt or treated with peracetic acid, and is split into the pure components, acetic acid and acetic anhydride, by fractional distillation in a second distillation zone and a third distillation zone.
Claim 3
Dependent Claim 75 words
A process as claimed in claim 1, wherein, during fractional distillation in the first distillation zone, an offgas, predominantly comprising C0 2 , CO, CH 4 and N 2 , is withdrawn at the head of the column, freed from residual methyl iodide by washing with the total amount of the starting materials methanol and methyl acetate, and passed to combustion, and the mixture of methanol and methyl acetate is fed to the reaction zone.
Claim 4
Dependent Claim 38 words
A process as claimed in any one of the preceding claims, wherein the catalyst system contains, as additional promoter, a compound of a carbonyl-forming non-noble metal from groups IV to VIII of the Periodic Table of the Elements.
Claim 5
Dependent Claim 64 words
4. A process as claimed in any one of the preceding claims, wherein the residence times of the starting materials in the reaction zone are from 2 to 50 minutes, depending on the flow rates of the catalyst solution fed back to the reaction zone and of the low-boiling components methyl iodide and methyl acetate and of the starting materials methanol and methyl acetate.
Claim 6
Dependent Claim 25 words
A process as claimed in any one of the preceding claims, wherein the starting material methyl acetate is replaced fully or partly by dimethyl ether.
Claim 7
Dependent Claim 57 words
A process as claimed in any one of the preceding claims, wherein a noble metal:promoter:methyl iodide : methyl acetate molar ratio of 1 : 2 - 100 : 10 - 300 : 10 - 1000 is maintained in the overall stream fed to the reaction zone at a noble metal concentration of from 0.005 to 0.05 mol/I.
Claim 8
Dependent Claim 45 words
A process as claimed in any one of the preceding claims, wherein the carbonylation mixture leaving the reaction zone flows through a subsequent reactor at 150 to 250 °C and residence times of from 0.5 to 15 minutes in order to convert dissolved carbon monoxide.
Claim 9
Dependent Claim 43 words
A process as claimed in any one of the preceding claims, wherein the distillative separation of the volatile components from the catalyst solution in the separation zone is carried out in the presence of carbon monoxide or mixtures of carbon monoxide and hydrogen.
Claim 10
Dependent Claim 27 words
A process as claimed in any one of the preceding claims, wherein the mixtures of carbon monoxide and hydrogen contain up to 5% by volume of hydrogen.
Claim 11
Dependent Claim 28 words
A process as claimed in any one of the preceding claims, wherein the mist eliminator contains filter fabrics made from corrosion-resistant substances, preferably glass fibers or stainless steel.

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