DIVIDED WALL COLUMN
DISTILLATION PROCESS
FOR PIPERAZINE CRUDE
Team 1: Catapharma Chemicals
• Dr. Shrikant Karwa (MD)
• Dr Shweta Karwa (Management)
• Shruti Karwa (Management)
• Anand Karwa (Management)
• Shrinivas Jahagirdar (Project)
Team 2 IIT Bombay
• Prof. Sunil Potale
• Prof. Sujit Jogwar
• Pravin Bharar Dalve
• Smrati Rathaur
• Yash Niraj Shah
Conventionally used distillation configurations for the separation of three or
more components

Columns in series

Multicomponent Distillation
(3 or more components present in the
feed)

Petlyuk Configuaration
 Distillation columns in series

• At least two columns are required to for separation of minimum three components

Figure (a) Direct Sequence, Figure (b) Indirect Sequence

 Petlyuk configuration

• A reboiler and a condenser are

effectively replaced by thermal
coupling.
• Can separate three or more
components provided reflux is
above a certain value.
• The avoidance of remixing
enhances energy efficiency.
• Reduces mixing losses because of
the greater freedom available to
match the feed composition with
the tray in the column.

Figure: Petlyuk Configuration (A-light, B-middle

C-Heavy boiling component)
Divided Wall Column Distillation Process (DWC)

• The two columns of the

Petlyuk configuration
are integrated into one
shell.
• DWC can deliver high
purity side product, and
thus is able to produce
three pure products in
just a single shell.
• Unlike conventional
columns with a side
draw, a DWC can
deliver high purity side
product, and thus is
able to produce three
pure products in just a
single shell.
DWC Configurations

(a) Wright Configuration (b) Split-shell column with common

overhead and divided bottom section (c) Split-shell column with
common bottom section and divided overhead
DWC Configurations
DWC configurations (Different positions and shape of the divided wall)
DWC Configurations
• In fig (a) two middle
boiling products are
accumulated at the right
hand side of the divided
wall, and this
combination is thermally
less efficient.
• In fig (b) The thermal
efficiency is improved by
addition of additional
dividing walls. This kind
of arrangement is also
known as Sargent
arrangement.
DWC Configurations (Agarwal Arrangement)

In this configuration, the feed enters the middle partition of the

DWC.
DWC Configurations (Agarwal arrangement cont..)
DWC Configurations (Agarwal arrangements cont..)
 A case study on designing a packed divided wall distillation column for Aromatic
Plants (Based on INA refinery distillation columns)

 The research group at the University of Zagreb and the University of Delft
investigated the design of a packed divided wall column distillation for
aromatic chemicals.
 For this purpose, a distillation process at INA refinery was used for reference.
 It consisted of direct sequence with two columns with a platformate splitter and
a benzene recovery column connected in series.
 These columns were used to separate platformate with 40 chemical
components.
1. C5-C6 Gasoline with benzene not greater than 1.5 mass%.
2. Benzene rich cut with 68 mass% benzene.
3. A heavy reformate with toluene, xylene, and other heavier components with
benzene less than 1.5 mass%.
4. Authors grouped 40 components to a 15-component mixture for this purpose.
Columns used at the INA refinery
INA REFINERY CASE STUDY
(CONTINUED..)
• The use of DWC allows a greater
degree of freedom for simulation
than the conventional distillation
method.
• Authors for this study used method
suggested by Halvorsen and
Skogestad ( Vmin method).
• The method required the use of
pure components. Therefore, they
used 2-methyl pentane, benzene,
and toluene to represent the 15-
component system.
• Vmin diagram was calculated by
simulating all binary splits. The
stage number was kept fourfold the
minimum number of stages
required.
HALVORSEN AND SKOGESTAD Vmin Method

 Halvorsen and Skogestad developed a method to determine minimum vapour and liquid
flows needed for binary separation occurring in particular columns with infinite number of
stages. The postulates proposed by them are discussed below
1. Minimum vapour flow required for separation of n components into n pure products
corresponds with that required for the most difficult binary split.
2. As mentioned in the previous slide 15-component system was converted into a three key
component system.
3. These three components were 2-Methyl Pentane (60 0C), Benzene (80 0C), and Toluene
(110 0C).
4. Subsequently, Vmin diagram was constructed by rigorous simulation of possible binary
splits with the stage number being at least 4 times the minimum number of stages.
5. The mass recovery of key components was set to 0.99.
6. From this diagram initial design parameters can be obtained by rigorous simulation with
infinite number of stages.
 Rigorous performance of DWC simulation

 Commercial process simulators such as Chemcad, ASPEN or HYSYS allows

DWC to be modelled as a sequence of simple columns.
 The authors used four-column models for the simulation of DWC in Chemcad.
The procedure used by authors is given below
1. First, the feed composition was restored to 15 full components.
2. Benzene mass fraction in the distillate and side-draw flow rate were set to be
the same.
3. Initial value of reboiler flow rate was set to give the minimal vapour flow.
4. Liquid and vapour flow rates were adjusted until minimum benzene in
bottoms was achieved.
INA REFINERY CASE STUDY

For the purpose of simulation, DWC was converted into a four-column

model (A= 2-Methyl Pentane, B= Benzene, and C= Toluene).
INA REFINERY (CONT..)
INA REFINERY
• Min N(R+1) versus N
was studied.
• The minimum number
of stages was 64.
 INA REFINERY

 The minimum rule of thumb for designing packed column

is that the number a single bed height should not exceed
20 equivalent stages.
 The bed arrangements, liquid collection, and distribution
is crucial in packed divided wall column distillation.
 In this study, the required number of equivalent stages in
the upper part was 26 while that in the lower part was 13.
Therefore, the recommended number of beds for the upper
part was 2, and that for the lower part was 1.
 • Authors suggested that the
plate should be adjusted
INA REFINERY slightly off-centre.
• This was because the load in
the pre-fractionator was 5-
fold the load in the main
column in the bottom
section.

• Liquid flow rate in the

bottom section of the
pre-fractionator

Liquid flow rate in the

bottom section of the
main column in
packed DWC.
INA REFINERY
SUMMARY OF THE APPROACH USED BY THE AUTHORS

15-component system
40-component mixture was represented by 3-
Vmin diagram with all
was lumped into a 15- key-component system
possible binary splits.
component mixture (2-Methyl pentane,
benzene, and toluene)

Detailed simulations
Column dimensioning were then performed
using 4-column model
CATAPHARMA PIPERAZINE
CRUDE DATA
Sr no Chemical Specification (wt %)

1 Ethylenediamine 4.85

2 Monoethanolamine 7.96

3 PIP+EDA+DETA 61.29

4 Piperazine 48

5 Triethylenediamine 2.62

6 Water Content 28.11

Properties of ethylenediamine
Properties of ethylenediamine
Ethylenediamine Properties
Diethylenetriamine (CAS # 111-40-0)
Diethylenetriamine Properties
Piperazine chemical properties (CAS 110-85-0)
Piperazine chemical properties
Triethylenediamine chemical properties
(CAS No.280-57-9)
Triethylenediamine chemical properties
Monoethanolamine (CAS-No-141-43-5)
Monoethanolamine chemical properties
(CAS-No-141-43-5)
Water properties