Method for the continuous dehydration of 3-hydroxypropionic acid to form acrylic acid

Patent metadata

Field	Value
Publication number	US-9809526-B2
Application number	US-201515311541-A
Country	US
Kind code	B2
Filing date	May 13, 2015
Priority date	May 19, 2014
Publication date	Nov 7, 2017
Grant date	Nov 7, 2017

Abstract

The invention relates to a process for dehydrating aqueous 3-hydroxypropionic acid to acrylic acid, wherein an aqueous mixture of 3-hydroxypropionic acid and oligomeric 3-hydroxypropionic acid is converted to acrylic acid in the liquid phase in a first step and aqueous acrylic acid is distilled out of the liquid phase, and the aqueous acrylic acid is separated by distillation into an acrylic acid-rich phase and a water-rich phase in a second step.

First claim

The invention claimed is:

1. A process for continuously dehydrating aqueous 3-hydroxypropionic acid to acrylic acid, which comprises, in a first step i), converting an aqueous mixture of 3-hydroxypropionic acid and oligomeric 3-hydroxypropionic acid to acrylic acid in the liquid phase and at a pressure of less than 900 mbar and separating aqueous acrylic acid from the liquid phase by distillation and, in a second step ii), separating the aqueous acrylic acid obtained in step i) at a pressure of less than 900 mbar, by distillation into a crude acrylic acid phase and a water phase.

2. The process according to claim 1 , wherein the aqueous mixture of 3-hydroxypropionic acid and oligomeric 3-hydroxypropionic acid used in step i) comprises from 15 to 35% by weight of water.

3. The process according to claim 1 , wherein the aqueous mixture of 3-hydroxypropionic acid and oligomeric 3-hydroxypropionic acid used in step i) comprises from 25 to 45% by weight of monomeric 3-hydroxypropionic acid.

4. The process according to claim 1 , wherein the liquid phase in step i) comprises an organic solvent having a boiling point at 1013 mbar of at least 160° C.

5. The process according to claim 1 , wherein the aqueous acrylic acid is removed in step i) by means of a rectification column.

6. The process according to claim 1 , wherein an entraining agent is used in step ii).

7. The process according to claim 1 , wherein the aqueous acrylic acid is separated in step ii), by means of a rectification column, into a crude acrylic acid phase and a water phase.

8. The process according to claim 1 , wherein the removal of the aqueous acrylic acid from the liquid phase in step i) and/or separation of the aqueous acrylic acid into a crude acrylic acid phase and a water phase in step ii) is performed in a single rectification column, with removal of the aqueous acrylic acid from the liquid phase below a side draw in the single rectification column, separation of the aqueous acrylic acid into a crude acrylic acid phase and a water phase above the side draw and withdrawal of the crude acrylic acid phase in liquid form in the side draw.

9. The process according to claim 8 , wherein the single rectification column is a dividing wall column, with the feed to the single rectification column and the side draw from the single rectification column on different sides of the dividing wall.

10. The process according to claim 1 , wherein the crude acrylic acid phase obtained in step ii) is purified by crystallization.

11. The process according to claim 10 , wherein the mother liquor from the crystallization is recycled into the single rectification column below the side draw.

12. The process according to claim 4 , wherein the organic solvent has a boiling pint at 1013 mbar of 200 to 350° C.

Assignees

• Basf Se

Inventors

• Blaschke Tim
• Lang Ortmund
• Zajaczkowski-Fischer Marta
• Hartmann Marco

Classifications

• C07C51/377

  by splitting-off hydrogen or functional groups; by hydrogenolysis of functional groups {(C07C51/36 - C07C51/373 take precedence)} · CPC title

• C07C51/43

  by change of the physical state, e.g. crystallisation · CPC title

• C07C51/46 Primary

  by azeotropic distillation · CPC title

• C07C57/04

  Acrylic acid; Methacrylic acid · CPC title