IP Library Granted Patent US 9,815,760
Granted Patent B2
US 9,815,760 · App. 15/311,925 · Granted Nov 14, 2017

Process for the co-production of acetic acid and dimethyl ether

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Quick Facts
Patent No.
US 9,815,760
App. No.
15/311,925
Granted
Nov 14, 2017
Kind
B2
Abstract

Catalytic dehydration-hydrolysis process for the co-production of acetic acid and dimethyl ether from a mixture of methanol and methyl acetate and water in which the amount of water fed to the process is controlled by the steps of dehydrating a methanol feed to provide a crude product containing dimethyl ether, unconverted methanol and water, recovering therefrom a stream containing dimethyl ether, water and methanol and a water stream and separating dimethyl ether from the dimethyl-ether containing stream to produce a methanol stream containing methanol and water. At least part of the methanol stream and methyl acetate is supplied to the dehydration-hydrolysis process.

Claims (22)

1. A process for the co-production of acetic acid and dimethyl ether by dehydration-hydrolysis of a mixture of methanol and methyl acetate carried out at a temperature of 100 to 350° C. and at atmospheric or greater pressure in the presence of at least one solid acid catalyst and water to generate a reaction product comprising dimethyl ether and acetic acid in which process the amount of water to the dehydration-hydrolysis is controlled by:

dehydrating a methanol feed comprising methanol and water to generate a crude dehydration product comprising dimethyl ether, unconverted methanol and water

recovering from the crude dehydration product i) a dimethyl ether stream comprising dimethyl ether, water and methanol and ii) a water stream;

separating dimethyl ether from the dimethyl ether stream to produce a methanol stream comprising methanol and water; and

supplying to the dehydration-hydrolysis reaction the methanol stream or a part thereof, methyl acetate and optionally one or more recycle streams comprising one or more of methanol, methyl acetate and water.

2. A process according to claim 1 wherein recovery of the water stream from the crude dehydration product is carried out by fractional distillation in a single distillation column equipped with a reboiler to recover the dimethyl ether stream as a heads product from the column and the water stream as a base stream from the column.

3. A process according to claim 2 wherein the amount of water recovered as a base stream from the distillation column is controlled by adjusting one or both of reflux ratio and reboiler duty (boil-up ratio) to the column.

4. A process according to claim 2 wherein distillation is carried out at a reflux ratio of from 0.05 to 1.

5. A process according to claim 4 wherein the distillation is carried out at a boil-up ratio of 0.01 to 5.

6. A process according to claim 2 wherein distillation is carried out at a pressure of 5 to 30 barg (500 to 3000 kPa) and at a heads temperature of 120 to 180° C.

7. A process according to claim 1 wherein the water stream recovered from the crude dehydration product comprises 90 mol % or more water.

8. A process according to claim 7 wherein the dimethyl ether stream recovered as a heads product from the column comprises >0 to 60 mol % methanol, 5 to 45 mol % water and the balance dimethyl ether.

9. A process according to claim 1 wherein the methanol feed to dehydration comprises water in an amount of from >0 to 35 mol %.

10. A process according to claim 9 wherein the methanol feed to dehydration comprises 50 to 99 mol % methanol, >0 to 35 mol % water and 0 to 10 mol % dimethyl ether.

11. A process according to claim 1 wherein the methanol feed to dehydration is derived from conversion of a gaseous mixture of carbon monoxide, hydrogen and optionally carbon dioxide in the presence of a methanol synthesis catalyst.

12. A process according to claim 1 wherein the dehydration is conducted as a vapour phase process at a pressure of atmospheric to 30 barg (atmospheric to 3000 kPa) and at a temperature of 100° C. to 450° C.

13. A process according to claim 1 wherein the dehydration is conducted as a liquid phase process at a pressure of 40 to 100 barg (4000 to 10000 kPa) and at a temperature of 140° C. to 210° C.

14. A process according to claim 1 wherein the dehydration of the methanol feed is carried out in the presence of a solid acid catalyst which solid acid catalyst is a zeolite selected from zeolites having a 2-dimensional or 3-dimensional channel system and at least one channel of which has a 10-membered ring.

15. A process according to claim 1 wherein dimethyl ether is separated from the dimethyl ether stream comprising dimethyl ether, water and methanol to produce a methanol stream comprising methanol and water by distillation in a single distillation column.

16. A process according to claim 1 wherein water is introduced to the dehydration-hydrolysis reaction in an amount of 0.1 to 50 mol % based on the total feed of methyl acetate, water and methanol.

17. A process according to claim 1 wherein the solid acid catalyst for the dehydration-hydrolysis reaction is selected from one or more heteropolyacids and salts thereof and zeolites.

18. A process according to claim 1 wherein the process is operated as a continuous process.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 26, 2021
From: BP CHEMICALS LIMITED
To: INEOS ACETYLS UK LIMITED
Reel/Frame 055746/0075 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 17, 2016
From: BRISTOW, TIMOTHY CRISPIN
To: BP CHEMICALS LIMITED
Reel/Frame 040354/0197 →