Process for preparing oligo ethylene glycol methyl ether borate

Patent metadata

Field	Value
Publication number	US-11926639-B2
Application number	US-202017756443-A
Country	US
Kind code	B2
Filing date	Nov 19, 2020
Priority date	Nov 29, 2019
Publication date	Mar 12, 2024
Grant date	Mar 12, 2024

Abstract

A process for preparing oligo ethylene glycol methyl ether borate involves feeding boric acid and oligo ethylene glycol monomethyl ether into a reactor, and reacting to obtain a raw product containing oligo ethylene glycol methyl ether borate, water, and unreacted boric acid and oligo ethylene glycol monomethyl ether. The raw product is fed to a reactive distillation device and boric acid is reacted with oligo ethylene glycmonomethyl ether for full conversion of boric acid. A distillate stream containing water is transferred from the top of the reactive distillation device to a condenser, and a condensed liquid stream is recycled to the top of the reactive distillation device. A bottom product stream containing oligo ethylene glycol methyl ether borate is withdrawn from the reactive distillation device. The bottom product stream is partially recycled to a reboiler. The resulting vapor stream is recycled to the bottom of the reactive distillation device.

First claim

The invention claimed is:

1. A process for preparing oligo ethylene give ether borate, comprising:
feeding boric acid and oligo ethylene glycol monomethyl ether into a reactor and reacting a resulting mixture to obtain a raw product which comprises oligo ethylene glycol methyl ether borate, water, unreacted boric acid, and unreacted oligo ethylene glycol monomethyl ether;
(b) feeding the raw product to a reactive distillation device and reacting the unreacted boric acid with the unreacted oligo ethylene glycol monomethyl ether for full conversion of boric acid;
(c) transferring a distillate stream containing the water from a top of the reactive distillation device to a condenser and recycling a condensed liquid stream to the top of the reactive distillation device; and
(d) withdrawing a bottom product stream containing the oligo ethylene glycol methyl ether borate from the reactive distillation device, transferring part of the bottom product stream to a reboiler and recycling a resulting vapor stream to a bottom section of the reactive distillation device.

2. The process according to claim 1 , wherein the oligo ethylene glycol monomethyl ether is triethylene glycol tnonomethyl ether, and the oligo ethylene glycol methyl ether borate is triethylene glycol methyl ether borate.

3. The process according to claim 1 , wherein a molar ratio of the oligo ethylene glycol monomethyl ether to the boric acid fed to the reactor in (a) is from 3.01: 1 to 3.4: 1.

4. The process according to claim 1 , wherein a temperature in the reactor is from 60° C. to 90° C., and a pressure in the reactor is from 1.0 bar (abs) to 2.0 bar (abs).

5. The process according to claim 1 , wherein a residence time of the resulting mixture in the reactor in (a) is from 2 hours to 5 hours.

6. The process according to claim 1 , wherein a conversion of the boric acid in the reactor is from 30% to 90%.

7. The process according to claim 1 , wherein the reaction in (a) is performed discontinuously, and the raw product is buffered in a tank, and
wherein (b) to (d) are performed continuously with a feed stream of the raw product taken from the tank.

8. The process according to claim 1 , wherein a mass fraction of the oligo ethylene glycol monomethyl ether in the bottom product stream in (d) is from 0 wt.-% to 12 wt.-%.

9. The process according to claim 1 , wherein a mass fraction of the water in the bottom product stream in (d) is below 0.05 wt.-%.

10. The process according to claim 1 , wherein an APHA color number of the bottom product stream is below 50.

11. The process according to claim 1 , wherein the reactive distillation device is operated at a pressure at the top of from 10 mbar (abs) to 30 mbar (abs) and a temperature at the bottom of from 150° C. to 200° C.

12. The process according to claim 1 , wherein the a reflux ratio of the condensed liquid stream to the distillate stream withdrawn from the top of the reactive distillation device is from 0.2 to 0.5 by mass.

13. The process according to claim 1 , wherein a ratio of number of theoretical stages of a rectifying section to a number of theoretical stages of a stripping section of the reactive distillation device is from 1:2 to 1:4.

14. The process according to claim 1 , wherein a nutlether of theoretical stages of a stripping section of the reactive distillation device is from 2 to 15.

15. The process according to claim 1 , wherein in (c) a stream of not condensed vapor is transferred from the condenser to a further condenser in which water is withdrawn as liquid condensate.

16. The process according to claim 3 , wherein the molar ratio of the oligo ethylene glycol mon.omethyl ether to the boric acid fed to the reactor in (a) is from 3.25:1 to 3.35.1.

17. The process according to claim 4 , wherein the temperature in the reactor is from 75° C. to 85° C., and the pressure in the reactor is from 1.1 bar (abs) to 1.3 bar (abs).

18. The process according to claim 1 , wherein the bottom product stream in (d) comprises a mass fraction of the oligo ethylene glycol monomethyl ether from 1 wt.-% to 9 wt.-%, and a mass fraction of the water below 0.02 wt.-%.

19. The process according to claim 13 , wherein the ratio of the number of theoretical stages of the rectifying section to the number of theoretical stages of the stripping section of the reactive distillation device is front 1:2.5 to 1:3.5.

20. The process according to claim 14 , wherein the number of theoretical stages of the stripping section of the reactive distillation device is from 5 to 10.

Assignees

• Basf Se

Inventors

• Werth Kathrin Luise Mariethres
• Holtmann Thomas
• Papp Rainer
• Haider Mirko
• Wulff-Doering Joachim

Classifications

• C07F5/04 Primary

  Esters of boric acids · CPC title

• Y02P20/10

  Process efficiency · CPC title