Process to control HI concentration in residuum stream

Patent metadata

Field	Value
Publication number	US-10413840-B2
Application number	US-201515549114-A
Country	US
Kind code	B2
Filing date	Oct 2, 2015
Priority date	Feb 4, 2015
Publication date	Sep 17, 2019
Grant date	Sep 17, 2019

Abstract

A process directed to acetic acid production comprising providing a feed stream comprising methyl iodide, water, acetic acid, methyl acetate, and at least one PRC to a distillation column comprising a distillation zone and a bottom sump zone and distilling the feed stream at a pressure and a temperature sufficient to produce an overhead stream comprising methyl iodide and at least one PRC, and a residuum stream flowing from the bottom sump zone comprising water and greater than or equal to about 0.11 weight percent HI is disclosed herein.

First claim

We claim:

1. A process to separate a mixture comprising methyl iodide, water, acetic acid, methyl acetate, and at least one permanganate reducing compound (PRC) derived from a condensed, biphasically separated first overhead stream produced by distilling a portion of a reaction medium of a carbonylation reactor in a first distillation column to yield an acetic acid product side stream and the first overhead stream, the process comprising:
providing a second distillation column feed stream comprising the mixture to a second distillation column comprising a distillation zone and a bottom sump zone;
directing a top flush stream comprising water into the distillation zone;
distilling the second distillation column feed stream to produce a second column overhead stream comprising methyl iodide and at least one PRC, a second column residuum stream flowing from the bottom sump zone comprising HI; and a second column sidestream of the second distillation column comprising methyl acetate, wherein the total amount of HI exiting the second distillation column in the second column overhead stream, the second column residuum stream, and the second column sidestream is greater than a total amount of HI entering the second distillation column, if any, in the second distillation column feed stream.

2. The process of claim 1 , wherein the second column residuum stream comprises greater than or equal to about 0.11 weight percent HI, based on the total amount of the second column residuum stream.

3. The process of claim 1 , wherein a portion of the second column overhead stream is condensed, separated, and directed back into the second distillation column.

4. The process of claim 1 , wherein the second column sidestream is recycled back into the process.

5. The process of claim 1 , wherein a mass flow rate of the top flush stream into the second distillation column is greater than or equal to about 0.1 percent of a mass flow rate of the second column feed stream.

6. The process of claim 1 , further comprising directing a bottom flush stream comprising water, acetic acid, or both into the distillation zone of the second distillation column, the bottom sump zone of the second distillation column, or both, at a mass flow rate of greater than or equal to about 0.1 percent of a mass flow rate of the second column feed stream.

7. The process of claim 6 , wherein the bottom flush stream is directed into the second distillation column between an exit of the second column sidestream and the bottom of the second distillation column.

8. The process of claim 1 , wherein the second column sidestream exits the second distillation column from the distillation zone of the second distillation column.

9. The process of claim 1 , wherein the second column overhead comprises dimethyl ether.

10. The process of claim 1 , wherein the biphasically separated first overhead stream comprises a light aqueous phase comprising greater than about 30 wt % water, and a heavy phase comprising greater than about 30 wt % methyl iodide, and wherein the second column feed stream is derived from, or comprises a portion of the light aqueous phase.

11. The process of claim 1 , wherein:
i. the reaction medium of a carbonylation reactor comprises a lithium acetate concentration between 0.3 and 0.7 wt % in the reaction medium;
ii. the concentration of hydrogen iodide is from 0.1 to 1.3 wt % in the reaction medium, based on the total weight of the reaction medium;
iii. the concentration of a rhodium catalyst is from 100 to 3000 wppm in the reaction medium, based on the total weight of the reaction medium;
iv. the concentration of water is from 0.1 to 4.1 wt % in the reaction medium, based on the total weight of the reaction medium;
v. the concentration of methyl acetate is from 0.6 to 4.1 wt % in the reaction medium, based on the total weight of the reaction medium;
or a combination thereof.

12. The process of claim 1 , wherein a butyl acetate concentration in the acetic acid product side stream is 10 wppm or less without directly removing butyl acetate from the acetic acid product side steam, wherein the butyl acetate concentration in the acetic acid product side stream is controlled by:
i. maintaining an acetaldehyde concentration in the reaction medium at 1500 ppm or less, based on the total weight of the reaction medium;
ii. controlling a temperature in the carbonylation reactor from 150° C. to 250° C.;
iii. controlling a hydrogen partial pressure in the carbonylation reactor from 0.3 to 2 atm;
iv. controlling a rhodium metal catalyst concentration in the reaction medium from 100 to 3000 wppm, based on the total weight of the reaction medium;
or a combination thereof.

13. The process of claim 1 , wherein an ethyl iodide concentration in the reaction medium is less than or equal to 750 wppm, wherein the acetic acid product side stream comprises less than 250 wppm propionic acid without directly removing propionic acid from the acetic acid product stream, or a combination thereof, wherein:
i. ethyl iodide in the reaction medium and propionic acid in the acetic acid product side stream are present in a weight ratio from 3:1 to 1:2;
ii. acetaldehyde and ethyl iodide are present in the reaction medium in a weight ratio from 2:1 to 20:1;
iii. methanol introduced into the carbonylation reactor comprises less than 150 wppm ethanol;
iv. an ethyl iodide concentration in the reaction medium is controlled by adjusting a hydrogen partial pressure in the carbonylation reactor, a methyl acetate concentration in the reaction medium, a methyl iodide concentration in the reaction medium;
or a combination thereof.

14. A process to produce acetic acid, comprising:
a. carbonylating a reaction medium comprising a reactant feed stream comprising methanol, methyl acetate, dimethyl ether, or mixtures thereof, water, a rhodium catalyst, an iodide salt and methyl iodide in a reactor to form acetic acid and directing a portion of the reaction medium into a flasher to produce a vapor product stream comprising acetic acid, water, methyl iodide, methyl acetate and at least one permanganate reducing compound (PRC), and a non-volatile stream and directing the non-volatile stream back into the reaction medium;
b. directing the vapor product stream from the flasher into a first distillation column to produce an acetic acid side stream, and a first column overhead stream comprising methyl iodide, water, acetic acid, methyl acetate, and at least one PRC;
c. biphasically separating the first column overhead stream into a light phase comprising methyl iodide, acetic acid, methyl acetate, at least one PRC, and greater than about 30 wt % water, and a heavy phase comprising water, acetic acid, methyl acetate, at least one PRC, and greater than about 30 wt % methyl iodide;
d. directing a second distillation column feed stream comprising or derived from a portion of the light phase, the heavy phase, or a combination thereof, into a second distillation column comprising a distillation zone and a bottom sump zone;
e. directing a top flush stream comprising water into the distillation zone at a mass flow rate greater than or equal to 0.1% of the mass flow rate of the second distillation column feed stream;
f. distilling the second distillation column feed stream at a pressure and a temperature sufficient to produce a second distillation column overhead stream comprising methyl iodide, and at least one PRC, a second column residuum stream comprising HI flowing out of the second column from the bottom sump zone, and a second column sidestream comprising methyl acetate flowing out of the second distillation column at a poin

Assignees

• Celanese Int Corp
• Celanese Int Coporation

Inventors

• Scates Mark O
• Shaver Ronald David
• Liu Yaw-Haw

Classifications

• B01D3/36

  Azeotropic distillation · CPC title

• B01D3/40

  Extractive distillation · CPC title

• B01D3/143

  by two or more of a fractionation, separation or rectification step · CPC title

• C07C51/48

  by liquid-liquid treatment · CPC title

• B01D3/4283

  Bottom stream · CPC title