Distillation method with controlled energy supply

Patent metadata

Field	Value
Publication number	US-11806646-B2
Application number	US-201917285263-A
Country	US
Kind code	B2
Filing date	Oct 21, 2019
Priority date	Oct 24, 2018
Publication date	Nov 7, 2023
Grant date	Nov 7, 2023

Abstract

The present invention relates to a process for thermally separating a mixture comprising a first main component and a second main component, where the boiling point of the first main component is lower than the boiling point of the second main components. The invention further relates to a system for thermal separation comprising a computer for control of the thermal separation which is set up to control the process of the invention. By means of predetermined thermodynamic models, pressure and temperature data are used to ascertain the proportions of first and second main component in bottom product streams.

First claim

The invention claimed is:

1. A process for thermally separating a mixture comprising a first main component and a second main component, where the boiling point of the first main component is lower than the boiling point of the second main component, the process comprising:
A) evaporating a mixture of the first main component and the second main component in an evaporator by supplying thermal energy to obtain a gaseous mixture of the first main component and the second main component and a first bottom product that are in a vapor-liquid equilibrium with one another;
B) transferring the gaseous mixture from A) to a thermal separation apparatus, where the second main component at least partly condenses as a second bottom product in the separation apparatus, the first main component remains at least partly in a gas phase, and there is a vapor-liquid equilibrium between the second bottom product and the gas phase;
C) removing the first bottom product from the evaporator in a first bottom product stream at a mass flow rate F 1 , wherein the first bottom product stream is removed from the evaporator separately from the gaseous mixture;
D) removing the second bottom product from the separation apparatus in a second bottom product stream at a mass flow rate F 2 ;
E) combining the first and second bottom product streams to give a third bottom product stream with a mixing ratio v=F 1 /(F 1 +F 2 ), in which F 1 is a mass flow rate for removing the first bottom product stream and F 2 is a mass flow rate for removing the second bottom product stream;
F) dividing the third bottom product stream into at least one target product stream at a mass flow rate F 3 and a recycle stream at a mass flow rate F rec , where the target product stream is withdrawn and the recycle stream is recycled into the evaporator and where the target product stream has a target value for the proportions of the first and second main components;
the process further including determining the pressure p that exists collectively in the evaporator and/or the separation apparatus,
determining the temperature T 1 that exists in the evaporator,
determining the temperature T 2 that exists in the separation apparatus,
determining according to a first predetermined thermodynamic model, from p and T 1 which are the proportions of the first and second main components in the first bottom product stream, expressed as quality Q 1 ,
determining according to a second predetermined thermodynamic model, p and T 2 which are the proportions of the first and second main components in the second bottom product stream, expressed as quality Q 2 ,
calculating based on the qualities Q 1 and Q 2 and the mixing ratio v, the proportions of the first and second main components in the target product stream, expressed as quality Q 3 , as the actual value and,
altering the supply of thermal energy to the evaporator depending on the deviation of the actual value from the target value for the proportion of the first main component in the third bottom product stream.

2. The process according to claim 1 , wherein the first main component is a haloaromatic and/or the second main component comprises a polyisocyanate.

3. The process according to claim 1 , wherein the evaporator is heated by steam having a mass flow rate F D .

4. The process according to claim 3 , wherein the mass flow rate F 1 is calculated as follows:
F 1 =F Rec −F D ·( h D /h K1 )

wherein h K1 is enthalpy of evaporation of the first main component, h D is enthalpy of evaporation of the steam heating the evaporator, and F D is the mass flow rate of steam into the evaporator.

5. The process according to claim 1 , wherein the temperature T 1 is measured by a sensor disposed in the evaporator and/or wherein the pressure p is measured by a sensor disposed in the evaporator.

6. The process according to claim 1 , further including measuring the mass flow rate F 3 of the target product stream and the temperature T 3 in the target product stream.

7. The process according to claim 6 , wherein the mass flow rate F 2 is calculated as follows:
F 2 =F 3 +F Rec −F 1 .

8. The process according to claim 7 , wherein the temperature T 2 is calculated as follows:
T 2 =[c p,3 ·T 3 ·( F 3 +F Rec )− c p,1 ·T 1 ·F 1 ]/[ cp,2 ·F 2 ]

wherein c p,1 is heat capacity of the first bottom product stream, c p,2 is heat capacity of the second bottom product stream and c p,3 is heat capacity of a target product stream.

9. The process according to claim 8 , wherein quality Q 3 is calculated by a mixing ratio v or v′ as follows:
Q 3 =v·Q 1 +(1− v )· Q 2

or
Q 3 =v′·Q 1 +(1− v ′)· Q 2

wherein v′ is calculated as follows:
v ′=( T 3 −T 2 )/( T 1 −T 2 ).

10. The process according to claim 1 , further including determining the proportions of the first and second main components in the target product stream experimentally at least once and correcting the calculation of the quality Q 3 with the experimentally determined proportions.

11. The process according to claim 1 , wherein a correction value is added onto p.

12. The process according to claim 11 , wherein the correction value added onto p is calculated from a value determined experimentally.

13. The process according to claim 10 , further including estimating coefficients of activity of the partial pressures of the first main component and/or the second main component with p, T 1 and/or T 2 and the value determined experimentally, =in an estimation of state based on a Kalman filter or a least-squares parameter estimate on a moving horizon.

14. The process according to claim 1 , further including monitoring operating status of sensors and, switching operation to an alternative process when predetermined criteria are fulfilled.

Assignees

• Covestro Intellectual Property Gmbh & Co Kg

Inventors

• Kuepper Achim
• Frenzel Philipp
• Kobylka Manfred

Classifications

• B01D3/322 Primary

  Reboiler specifications · CPC title

• B01D3/148

  in combination with at least one evaporator · CPC title

• B01D3/42

  Regulation; Control · CPC title

• B01D3/4283

  Bottom stream · CPC title

• B01D2259/65

  Employing advanced heat integration, e.g. Pinch technology · CPC title