Acrylic acid purification via dividing wall columns

Patent metadata

Field	Value
Publication number	US-11214534-B2
Application number	US-201716471233-A
Country	US
Kind code	B2
Filing date	Dec 15, 2017
Priority date	Dec 22, 2016
Publication date	Jan 4, 2022
Grant date	Jan 4, 2022

Abstract

The present disclosure relates to a process for producing high-purity acrylic acid using a dividing wall distillation column and in some instances using water as an entrainer and azeotroping agent. This disclosure provides a process for separating acrylic acid from recovered feed streams which comprise saturated organic acids including propionic acid. The resulting acrylic acid product is of sufficient purity to produce acrylate esters and high molecular weight acrylic acid polymers.

First claim

We claim:

1. A process for purifying acrylic acid from a feed stream composition comprising water, acrylic acid, acetic acid, and propionic acid using a dividing wall column, the process comprising:
supplying the feed stream into the dividing wall column operated at a temperature and pressure such that the feed stream is separated into at least a product top stream, a product bottom stream, and a product side stream and optionally a concentrated product upper side stream; and
wherein the feed stream and the product side stream are located on opposite sides of the column and are separated by the dividing wall and wherein the dividing wall extends vertically through the column from a dividing wall-free column top zone to a dividing wall-free column bottom zone; and
adding entraining water as an entrainer and azeotroping agent, into the dividing wall-free column top zone in the column; and
wherein the entraining water to feed ratio (wt/wt) in the column is greater than 1.0; and
wherein the product top stream comprises water, acetic acid, propionic acid and low boiling by-products, the product bottom stream comprises high-boiling by-products, and the product side stream comprises acrylic acid and the optional concentrated product upper side stream is located near the top of the column and comprises a concentrated acid side-stream comprising acetic acid, and wherein the optional concentrated product upper side stream is located above the dividing wall in the wall-free column top zone.

2. A process for purifying acrylic acid from a feed stream composition comprising water, acrylic acid, acetic acid, and propionic acid using a dividing wall column, the process comprising:
supplying the feed stream into the dividing wall column operated at a temperature and pressure such that the feed stream separated into: two product top streams, one on each side of the column; two product bottom streams, one on each side of the column; a product stream on the side of the column wall opposite the feed stream; and optionally two concentrated product upper side streams, one on either side of the column; and
wherein the feed stream and the product stream on the side of the column wall opposite the feed stream are located on opposite sides of the column and are completely separated by the dividing wall and wherein the dividing wall extends vertically through the entire column from the top of the column to the bottom of the column; and
adding entraining water as an entrainer and azeotroping agent, near the top of the column wherein the entrainer is fed on each side of the column; and
wherein the entraining water to feed ratio (wt/wt) in the column is greater than 1.0; and
wherein the product top streams comprise water, acetic acid, propionic acid and low boiling by-products, the product bottom streams comprise high boiling by-products, and the product stream on the side of the column wall opposite the feed stream comprises acrylic acid and the optional concentrated product upper side streams are located near the top of the column and comprise concentrated acid side-streams comprising acetic acid.

3. A process according to claim 1 , wherein the feed stream comprises 1-80 wt % acrylic acid, up to 80 wt % acetic acid, and up to 60 wt % additional components where the total composition does not exceed 100 wt % and wherein the product side stream is high purity acrylic acid with less than 500 ppm acetic acid.

4. A process according to claim 1 , wherein the feed stream comprises 5-50 wt % acrylic acid, 50-80 wt % acetic acid, 1-20 wt % water, and 0.5-1 wt % propionic acid or wherein the feed stream comprises 50-80 wt % acrylic acid, 0.1-20 wt % acetic acid, 0.1-10 wt % water, and 0.001-0.5 wt % propionic acid and wherein the product side stream is high purity acrylic acid with less than 500 ppm acetic acid and less than 100 ppm propionic acid.

5. A process according to claim 1 , wherein greater than 80 wt % of the acrylic acid in the feed stream is recovered in the product side stream.

6. A process according to claim 1 , wherein the feed stream is recovered from the production of acrylic acid by propylene oxidation, said feed stream comprising acrylic acid, acetic acid, propionic acid, water, and heavy by-products.

7. A process according to claim 1 , wherein the feed stream is recovered from the production of acrylic acid by an aldolization reaction, said feed stream comprising acrylic acid, acetic acid, propionic acid, water, and heavy by-products.

8. A process according to claim 1 , wherein the feed stream is recovered from the production of acrylic acid from propane oxidation or bio-based processes which comprise the use of 3-hydroxypropionic acid, glycerol, or lactic acid as starting materials/reactants, said feed stream comprising acrylic acid, acetic acid, propionic acid, water, and high boiling by-products.

9. A process according to claim 1 or 2 , wherein the product top stream(s) further comprises other organic compounds forming minimum boiling azeotropes with water.

10. A process according to claim 1 or 2 , wherein the product top stream(s) contains at least 90 wt % of the propionic acid in the feed stream.

11. A process according to claim 1 , wherein the acrylic acid in the product side stream is in a higher concentration than in the feed stream.

12. A process according to claim 1 , wherein the column operates at a pressure less than or equal to 1000 torr.

13. A process according to claim 1 , wherein the column temperature is controlled to less than 140° C. when the concentration of acrylic acid is greater than 35 wt % in the column.

14. A process according to claim 1 , wherein the column temperature is controlled to less than 115° C. when the concentration of acrylic acid is greater than 35 wt % in the column.

15. A process according to any one of claim 1 or 2 wherein the water to feed ratio (wt/wt) in the column is greater than 1.4.

16. A process according to claim 1 , wherein the feed stream comprises less than 80 wt % acrylic acid.

Assignees

• Eastman Chem Co

Inventors

• Hoyme Craig Alan
• Huss Robert Scott
• Puhr Joseph Jerome

Classifications

• C07C51/44 Primary

  by distillation · CPC title

• C07C51/46

  by azeotropic distillation · CPC title

• C07C57/04

  Acrylic acid; Methacrylic acid · CPC title