Method for purifying (meth)acrylic esters using a divided wall column

Patent metadata

Field	Value
Publication number	US-11926588-B2
Application number	US-202017424204-A
Country	US
Kind code	B2
Filing date	Jan 21, 2020
Priority date	Jan 22, 2019
Publication date	Mar 12, 2024
Grant date	Mar 12, 2024

Abstract

The invention relates to the production of (meth)acrylic esters according to a process by direct esterification, and in particular to the purification of a crude reaction mixture comprising a C 4 -C 12 (meth)acrylic ester using a dividing wall column employed in a particular configuration. The dividing wall column is equipped with a separating wall creating separation zones in the column, the wall not being joined to the upper dome of the column in the top part and being joined to the bottom of the column in the bottom part. The process according to the invention guarantees a product of very high purity, independently of the back-cracking reactions of the heavy by-products liable to arise during the purification of the product sought.

First claim

The invention claimed is:

1. A process for recovering a purified C 4 -C 12 (meth)acrylic ester, starting from a crude reaction mixture including Michael adducts obtained by direct esterification of the (meth)acrylic acid with the corresponding C 4 -C 12 alcohol wherein said process comprises the step of:
using a purification system comprising a dividing wall column equipped with a separating wall which is not joined to the upper dome of the column in the top part and is joined to the bottom of the column in the bottom part, and associated at the top with a single condenser and at the bottom with two boilers, said dividing wall column comprising a common rectification section above the wall, a prefractionation section comprising a feed of the crude reaction mixture of the column, and a withdrawal section separated from the prefractionation section by the wall and comprising the withdrawal of the purified ester; wherein said dividing wall column further comprises an outlet at the upper dome of the column, two outlets at the bottom part of the column and one outlet at the withdrawal section.

2. The process as claimed in claim 1 , wherein a gas stream is extracted at the top of the rectification section and recycled after condensation at least in part into an esterification reactor.

3. The process as claimed in claim 1 wherein a stream is withdrawn at the bottom of the prefractionation section and recycled at least in part into an esterification reactor.

4. The process as claimed in claim 1 wherein a stream is withdrawn at the bottom of the withdrawal section and recycled at least in part into the prefractionation section of the dividing wall column.

5. The process as claimed in claim 1 wherein a stream of purified (meth)acrylic ester is withdrawn as a sidestream from the withdrawal section at a point situated above the bottom withdrawal of said withdrawal section.

6. The process as claimed in claim 1 wherein the purification system is stabilized using a single polymerization inhibitor, the purified (meth)acrylic ester being withdrawn as a sidestream from the dividing wall column in the form of an already stabilized liquid or gas stream.

7. The process as claimed in claim 1 wherein the purification system is stabilized using a first polymerization inhibitor, the purified (meth)acrylic ester being withdrawn as a sidestream from the dividing wall column in the form of a gas stream which, after condensation, is subsequently stabilized with a polymerization inhibitor that is different from the first inhibitor.

8. The process as claimed in claim 1 wherein the number of theoretical stages of the prefractionation section is between 1 and 15.

9. The process as claimed in claim 1 wherein the number of theoretical stages of the withdrawal section is between 2 and 15.

10. The process as claimed in claim 1 wherein the number of theoretical stages of the rectification section is between 5 and 15.

11. The process as claimed in claim 1 wherein the (meth)acrylic ester is 2-ethylhexyl acrylate or 2-octyl acrylate.

12. A process for producing a C 4 -C 12 (meth)acrylic ester of high purity by direct esterification of the (meth)acrylic acid with the corresponding C 4 -C 12 alcohol, wherein the crude reaction mixture is subjected to the recovery process using the purification system as claimed in claim 1 .

13. The process as claimed in claim 1 where the prefractionation section and the withdrawal section further comprise liquid reflux provided by a collecting means thereby allowing controlled distribution of liquid from a bottom of the rectification section to the prefractionation and withdrawal sections.

Assignees

• Arkema France

Inventors

• Tretjak Serge
• Cabon Yves
• Levray Andre
• Hilpert Camille
• Moreliere Anne

Classifications

• C07C67/08 Primary

  by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds · CPC title

• C07C67/54

  by distillation · CPC title

• C07C69/54

  Acrylic acid esters; Methacrylic acid esters · CPC title