Design of Distillation Column to separate the

1, 3 butadiene from ethanol mixture

Presented by:
K. Uma Sai Mahesh
CH16MTECH11009
16MTECH11009

Department of Chemical Engineering

Indian Institute of Technology - Hyderabad

Table of Contents
Introduction: ...................................................................................................... 3
FLOW SHEET AND PROBLEM STATEMENT ......................................................... 4
Design Objective: ............................................................................................... 5
Compounds mention: ........................................................................................ 5
Method used: .................................................................................................... 6
Binary Interactions:............................................................................................ 6
Process conditions: ............................................................................................ 7
No. of Stages Vs Reflux ratio: ............................................................................. 9
Distillation tower data: .................................................................................... 10
Light component results: ................................................................................. 12
Distillate results: .............................................................................................. 13
Bottom results: ................................................................................................ 14
Column Dynamics: ........................................................................................... 15
Dynamic control diagram: ................................................................................ 16
Servo problem ................................................................................................. 17
Regulatory control: .......................................................................................... 17
Conclusion: ...................................................................................................... 18
References: ...................................................................................................... 18

Introduction:
1, 3-butadiene is a chemical compound that is frequently used as a monomer in
the production of synthetic styrene-butadiene rubber (SBR). It is also used to
make adiponitrile, an intermediate of nylon, as well as acrylonitrile-butadienestyrene (ABS), vinylcyclohexene, cyclooctadiene, cyclododecatriene,
cycloalkanes, cycloalkenes, polybutadiene, hexamethylene diamine, styrenebutadiene latex, chloroprene, and nitrile rubbers.
A common method of producing butadiene was the two-step Ostromislensky
process, in which ethanol is oxidized to acetaldehyde which then reacts with
additional ethanol over a tantala-promoted silica catalyst to yield butadiene.
CH3CH2OH CH3CHO + H2
CH3CH2OH + CH3CHO CH2CHCHCH2 + 2H2O
The chief function of distillation column is to separate the product, butadiene,
along with ethylene, from the heavy products, including ethanol, acetaldehyde,
and water. The column has 18 stages, a height of 86 feet, and a diameter of 12
ft. The tray efficiency was calculated to be 40%, requiring a total of 37 trays.
For our application, sieve trays of 24-inch spacing are used. The feed stage is at
tray 12, and the column operates at a molar reflux ratio of 6 and a pressure of
125 psi.
A distillation train is used to recover the butadiene. Before the product stream
can enter the distillation train, however, its pressure must be increased to 125
psi and its temperature decreased to 200F. The pressure was set so that the feed
stream to the first distillation column matched the condenser pressure, and the
temperature was set so that it was between the temperatures of the bottoms and
distillate streams. To achieve the required pressure and temperature change, two
heat exchangers, a compressor, two pumps, and two pressurized vessels, were
used.
So the product from second reactor splits into two fractions hence the feed
to the distillation column are feed1 and fee2.

FLOW SHEET AND PROBLEM STATEMENT

A plant utilizing a two-step reaction process, which takes a 95% ethanol
stream (by mass) and produces a 98% 1, 3 butadiene stream, was designed.
The production goal for this plant was 200,000 tonnes of butadiene with the
main motivation behind the project being the recent rise in butadiene prices.
The process first passes ethanol through a catalytic dehydrogenation reactor to
convert ethanol to acetaldehyde and hydrogen. The acetaldehyde
Intermediate is further reacted with ethanol in a catalytic reactor to form
butadiene.

Design Objective:
Removal of butadiene and
nd light components from the ethanol and
acetaldehyde mixture using Aspen Simulation.

Compounds mention:
The compounds include ethanol, acetaldehyde, hydrogen, methane,
carbon dioxide, carbon monoxide, acetic acid, diethyl ether, water,
ethylene, hexamine, butene, and butadiene.
butadiene

Method used:
NRTL (non random two liquid) because of involving of liquid phase
reactions.
Binary Interactions:

Process conditions:
Feed1 (from reactor)
Temperature: 200oF
Pressure
: 126 psi
Total Flow rate: 99893 lb/hr
Butadiene Flow rate: 47300 lb/hr

Feed 2 (from mixer)

Temperature : 221oF
Pressure : 125 psi
Total Flow rate : 187733 lb/hr
Butadiene Flow rate : 8871 lb/hr
Total butadiene Feed : 56171 lb/hr

Flow sheet:

Feed 1 data:
Feed enters the distillation at 200oF and pressure of 126 psi.

Feed 2 data:
Feed 2 enters the distillation column at 221oF and pressure at 125
psi.

No. of Stages Vs Reflux ratio:

The column was optimized to find the best combination of number
of stages to molar reflux ratio. To do so, a reflux ratio was set and
then a design specification was used in ASPEN to find the minimum
number of stages needed to achieve the desired separation. The
reflux ratio was changed, and the process was repeated.
repeated. Three
combinations were found that achieved the desired separation. The
points were plotted in Excel and a 45 line was plotted against the
line of best fit. The point of intersection determined the optimal
operating conditions.
Note, that this procedure was done assuming 100% tray efficiency.
Therefore, the final tray efficiency was taken as 40%,, which resulted
in a new tray number. It was assumed that the optimal reflux ratio
remained the same once the efficiency was changed.

Distillation tower data:

Number of stages are 37 with partial condenser with rate of 1262.54
lbmol/hr.
The reflux ratio is 6.

Condenser is maintained at 125 psi and pressure drop across the

each stage is 0.1 psi.

Feed entering data:

Feed 1 and Feed 2 enter the column at 12 stages.

Light component results:

Distillate results:
Butadiene in feed: 56171 lb/hr
Butadiene in distillate: 54977.9 lb/hr.
So, fractional removal of butadiene from feed is given by
(54977.9)*(100)/ (56171) = 97.875%

Bottom results:
Bottom contains only small portion of butadiene. It can be removed
in the next distillation column to recover the butadiene.

Column Dynamics:
Reflux Drum:
Head type Elliptical
Length 25 ft
Diameter 8 ft

Hydraulics:
Diameter of column 12 ft
Spacing 2 ft

Dynamic control diagram:

Controllers:
PC controller for controlling top stage pressure.
LC controller for controlling reflux drum level.
LC controller for controlling re
re-boiler drum level.
Manually added controllers:
CCT controller for controlling butadiene composition in distillate.

Servo problem: (composition control of top distillate)

Set point (0.1883 lbmol/lbmol) of mole fraction of
butadiene in distillate was changed to 0.189 lbmol/lbmol
at 12hrs.
The process variable reaches the set point at 13hrs.i.e it
reaches the steady state value after 1hr.
The gain and integral time used are 1
10% and 20 min.

Regulatory control:
For regulatory control feed pressure was changed from 126 psi to
130 psi at 3hrs and steady state reached at 9hrs.

Conclusion:
Distillation design for removal of butadiene from ethanol mixture is done using
ASPEN plus. The results of separation are satisfactory. In the dynamic
simulation the servo and regulatory changes for composition controller is
satisfactory.

References:
Outlines of Chemical Technology-Dryden.
Website: University of Pennsylvania, Dept. of Chemical &
Bimolecular Engineering.