MANUFACTURING OF COLUMN INTERNALS NO. 3 (INT 3) AND ...

MANUFACTURING OF COLUMN INTERNALS NO. 3 (INT 3)
AND THEIR MODIFICATION (MATERIALS)
Deliverable 54
Workpackage 9
Technical Report
Authors:
T.A. Nijhuis, F. Kapteijn, J.A. Moulijn
Date:
19/05/00
Distribution:
Frédéric Gouardères, European Commission,
Andrzej Górak, University of Dortmund
Eugeny Kenig, University of Dortmund
Oliver Bailer, SULZER
Harald Baeder, BASF
Remko Bakker, DSM
Willem Levering, SULZER
Jacob Moulijn, University of Delft
Hans Hasse, University of Stuttgart
Wieslaw Salacki, PLOCK
Jiri Klemes, UMIST
Andrzej Kraslawski, Lappeenranta University of Technology
Joerg Zellmer, MONTZ
Florian Menter, AEA
Maria Majchrzak, ICSO
Andrzej Kolodziej, IIC
Ion Ivanescu, PETROM
Valentin Plesu, University „Politehnica” of Bucharest
PROGRAMME GROWTH
Intelligent Column Internals for Reactive Separations (INTINT)
Project No. GRD1 CT1999 10596
Contract No. G1RD CT1999 00048

Intelligent Column Internals for Reactive Separations Page 2 of 3
Deliverable No. 54 Issued: 19.05.00
INT 3 will be Sulzer KATAPAK-S Laboratory packing.
Technical data:
Gauze:
Material: SS 1.4401
Mesh size: 0.25 mm
Wire thickness: 0.5 mm
Catalyst:
Particle diameter between 0.63 – 1.5 mm,
optimal 80% between 0.8 – 1.0 mm
Element height:
Labor: 100 mm and 200 mm
Unit Laboratory
Specific surface area m²/m³ 270
Catalyst fraction Vol.% 21
Layer height mm 4
"Sandwich thickness" mm 8
Corrugation angle ° 45
Corrugation stepsize mm 12
NTSM 1/m 3
Pictures:
KATAPAK-S packing in a 1.2 m reactor KATAPAK-S
Delivery time for packing: 1 month.

Separation efficieny [NTSM]
Pressure drop [mbar/m]
REACTIVE DISTILLATION USING
KATAPAK-S – Technical Data
Intelligent Column Internals for Reactive Separations Page 3 of 3
Deliverable No. 54 Issued: 19.05.00
Measurements of the separation efficiency
and pressure drop of KATAPAK-S laboratory
packing were carried out in a 70 mm diameter
distillation column for the test system chlorobenzene
/ ethylbenzene at total reflux. The
separation efficiency is almost constant
(NTSM = 3) up to F-factors of about 1.5 Pa 0.5 .
At F-factors above 1.5 Pa 0.5 , NTSM rapidly
increases due to better gas/liquid mass
transfer as more liquid runs on the outside of
the sandwiches. Flooding of the packing occurred
at F-factors around 1.9 Pa 0.5 .
6
5
4
3
2
1
0
100
10
1
0.1
0.1 1 10
F-factor [Pa0.5 ]
Separation efficiency and pressure drop
KATAPAK-S laboratory (70 mm)
Test system: CB/EB
The dynamic hold-up is shown in the next
diagram. Water was used as test system.
Dynamic hold-up [m 3 /m 3 ]
Function of residence time
distribution E (q)
0.18
0.16
0.14
0.12
0.1
0.08
0.06
0 5 10 15 20 25 30 35
Liquid load [m 3 /m 2 h]
Hold-up KATAPAK-S laboratory (70mm)
Test system: water
The figure below shows measured residence
time distributions. At low liquid loads, the
residence time distribution is narrow, showing
slight tailing due to stagnant zones which
are observed at small liquid loads when the
sandwiches are not sufficiently filled with
liquid. At optimal liquid loads, the residence
time distribution is still narrow and the tailing
almost disappears, as the sandwiches are
now completely filled with flowing liquid. At
high liquid loads, the residence time distribution
becomes broader. This is due to the fact
that the excess liquid flows as bypass on the
outside of the sandwiches.
4
3.5
3
2.5
2
1.5
1
0.5
0
0 0.5 1 1.5 2
Dimensionless time q
low liquid load
optimal liquid load
high liquid load
Residence time behaviour
KATAPAK-S laboratory (70 mm)
Test system: water/NaCl