IP Library Granted Patent US 12673909
Granted Patent B2
US 12673909 · App. 18/039,504 · Granted Jul 7, 2026

Method for controlling a reactive distillation column

Inventors: Wolf-Steffen Weissker (Ludwigshafen am Rhein, DE); Edward Richmond (Ludwigshafen am Rhein, DE)
Assignee: BASF SE
C07C29/705B01D3/009B01D3/4277C07C31/30
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12673909
App. No.
18/039,504
Granted
Jul 7, 2026
Kind
B2
Abstract

A method for controlling a reactive distillation column for effecting a transalcoholisation reaction, comprising feeding a metal methoxide into the reactive distillation column via a side feed; feeding a reactant alcohol into a lower part of the reactive distillation column; withdrawing methanol from the top of the reactive distillation column; and withdrawing a solution of a product metal alkoxide in the reactant alcohol from the bottom of the reactive distillation column; wherein the method comprises a process control scheme selected from: Scheme A: establishing a signal S 1 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and manipulating in response to the signal S 1 the feed amount of the reactant alcohol; Scheme B: establishing a signal S 1 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and manipulating in response to the signal S 1 the heat supplied to the bottom of the reactive distillation column. The invention also relates to a method for controlling a reactive distillation column for effecting a transalcoholisation reaction, comprising feeding a metal methoxide into the reactive distillation column via a side feed; feeding a reactant alcohol into a lower part of the reactive distillation column; causing an auxiliary alcohol to be present in the reactive distillation column; and optionally replenishing the auxiliary alcohol via a side feed located above the feed of the reactant alcohol and below the top of the column; withdrawing methanol from the top of the reactive distillation column; and withdrawing a solution of a product metal alkoxide in the reactant alcohol from the bottom of the reactive distillation column; wherein the method comprises a process control scheme selected from: Scheme C: establishing a signal S 2 which is responsive to a temperature at a point located between the feed of the metal methoxide and the bottom of the reactive distillation column; and manipulating in response to the signal S 2 the feed amount of the reactant alcohol; Scheme D: establishing a signal S 2 which is responsive to a temperature at a point located between the feed of the metal methoxide and the bottom of the reactive distillation column; and manipulating in response to the signal S 2 the heat supplied to the bottom of the reactive distillation column. The methods of the invention allow for improved controlling of a reactive distillation column for effecting a transalcoholisation reaction.

Claims (39)

1 . A method for controlling a reactive distillation column for effecting a transalcoholisation reaction, comprising

feeding a metal methoxide into the reactive distillation column via a side feed;

feeding a reactant alcohol into a lower part of the reactive distillation column;

withdrawing methanol from the top of the reactive distillation column; and

withdrawing a solution of a product metal alkoxide in the reactant alcohol from the bottom of the reactive distillation column;

wherein the method comprises a process control scheme selected from:

Scheme A:

establishing a signal S 1 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and

manipulating in response to the signal S 1 the feed amount of the reactant alcohol;

Scheme B:

establishing a signal S 1 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and

manipulating in response to the signal S 1 the heat supplied to the bottom of the reactive distillation column.

2 . The method according to claim 1 , wherein the reactant alcohol is selected from ethanol, 2-propanol, 2-butanol, 3-methyl-2-butanol, 3-methyl-3-methoxybutanol, 1-methoxy-2-propanol, 2-methyl-2-pentanol, 3-methyl-3-pentanol, 3-ethyl-3-pentanol, 2-methyl-2-hexanol, 3-methyl-3-hexanol, and 3,7-dimethyl-3-octanol.

3 . The method according to claim 1 , wherein the metal methoxide is an alkali metal methoxide.

4 . The method according to claim 3 , wherein the alkali metal methoxide is sodium methoxide or potassium methoxide.

5 . The method according to claim 1 , wherein the metal methoxide is fed into the column as a solution in methanol and the solution comprises 20 to 40% by weight of the metal methoxide, relative to the total weight of the solution of the metal methoxide.

6 . The method according to claim 1 , wherein the reactive distillation column comprises a forced circulation reboiler and the reactant alcohol is fed into a stream supplied to the forced circulation reboiler in liquid form.

7 . The method according to any claim 1 , wherein the product metal alkoxide is liquid at a temperature of 20° C. and a pressure of 1 bar absolute.

8 . A method for controlling a reactive distillation column for effecting a transalcoholisation reaction, comprising

feeding a metal methoxide into the reactive distillation column via a side feed;

feeding a reactant alcohol into a lower part of the reactive distillation column;

causing an auxiliary alcohol to be present in the reactive distillation column; and optionally replenishing the auxiliary alcohol via a side feed located above the feed of the reactant alcohol and below the top of the column;

withdrawing methanol from the top of the reactive distillation column; and

withdrawing a solution of a product metal alkoxide in the reactant alcohol from the bottom of the reactive distillation column;

wherein the method comprises a process control scheme selected from:

Scheme C:

establishing a signal S 2 which is responsive to a temperature at a point located between the feed of the metal methoxide and the bottom of the reactive distillation column; and

manipulating in response to the signal S 2 the feed amount of the reactant alcohol;

Scheme D:

establishing a signal S 2 which is responsive to a temperature at a point located between the feed of the metal methoxide and the bottom of the reactive distillation column; and

manipulating in response to the signal S 2 the heat supplied to the bottom of the reactive distillation column.

9 . The method according to claim 8 , wherein the method comprises a further process control, which is:

Scheme E:

establishing a signal S 3 which is responsive to a temperature in the rectifying section disposed above the feed of the metal methoxide; and

manipulating in response to the signal S 3 the feed amount of the auxiliary alcohol.

10 . The method according to claim 8 , wherein the reactant alcohol is selected from 3-methyl-3-methoxybutanol, 2-methyl-2-pentanol, 3-methyl-3-pentanol, 3-ethyl-3-pentanol, 2-methyl-2-hexanol, 3-methyl-3-hexanol, and 3,7-dimethyl-3-octanol.

11 . The method according to claim 8 , wherein the boiling point of the auxiliary alcohol is at least 10° C. above the boiling point of methanol at the pressure prevailing in the reactive distillation column.

12 . The method according to claim 8 , wherein the boiling point of the auxiliary alcohol is at least 10° C. below the boiling point of the reactant alcohol at the pressure prevailing in the reactive distillation column.

13 . The method according to claim 8 , wherein the auxiliary alcohol is selected from 1-methoxy-2-propanol, 2-butanol, 2-methyl-2-butanol, 3-methyl-2-butanol, tert-butanol, 3-methyl-3-pentanol and 3-ethyl-3-pentanol.