Documente Academic
Documente Profesional
Documente Cultură
Vol. 25, No. 04, pp. 765 - 776, October - December, 2008
Abstract - A mathematical model has been developed for describing the dynamic operation of the N-
formylmorpholine extractive distillation column and the corresponding solvent recovery column in the
benzene extraction plant. The NRTL equation was used to calculate the equilibrium and thermodynamic
properties of the mixtures. The validity of the model in terms of temperature, pressure and split fraction was
examined using actual plant data at steady-state conditions. Comparison between model results and plant data
shows good consistency. In order to improve the control of the process and selection of the optimal control
strategy, the model was used to find the optimum values of the constants of the controllers with Nelder-Mead
algorithm during unsteady-state operation by minimizing the deviation from steady-state conditions. The
outcome of this study could be used by operators and engineers to increase the productivity of the unit.
Keywords: Benzene extractive distillation; Process modeling; Dynamic optimization; N-formylmorpholine
(NFM).
extractive distillation using NFM as the solvent. In aromatics. The vapors at the overhead of the
some dynamic cases, the product may become off- extractive distillation column, containing non-
spec where the disposal would be rather costly aromatics and a small amount of benzene and
(Wozny and Li, 2004). Such a drawback could be solvent, are fed into the solvent recovery column,
overcome by optimization if the process reaches where solvent and non-aromatics are separated. The
steady-state as fast as possible. bottom product of the extractive distillation column,
Dynamic optimization is an increasingly consisting of solvent, benzene and a small amount of
important aspect in energy and chemical industries. non-aromatics, is conveyed to the stripper column, in
Start-up, shut-down and feed changeovers are which pure benzene is obtained as the overhead
frequent operations in chemical industries and the product by vacuum distillation (solvent regeneration
demand for more flexible processes that can better unit). The stripped hot solvent from the bottom of
handle such operations is increasing. These dynamic the stripper column is pumped through several heat
events could be subject to optimization in order to exchangers to the top of the extractive distillation
find the optimum trajectories. Optimization attempts column. In this research, the extractive distillation
have been reported for extractive distillation section was the subject of the dynamic optimization.
processes by Langston et al (2005), Low and
Sorensen (2002) and Munoz et al (2006). However, Extractive Distillation Section
none deals with extractive distillation of benzene by
NFM. In the present study, a dynamic model has The extractive distillation section itself consists
been developed for the extractive distillation of of two units: extractive distillation column and
benzene by the NFM solvent. The dynamic solvent recovery column, as shown in Figure 2. In
optimization techniques were applied for the purpose the extractive distillation column, non-aromatics are
of reaching fast steady state conditions where the separated from benzene. This separation is
calculation of the control parameters becomes impossible under normal conditions by means of
possible in the event of feed disturbances. distillation. NFM, the solvent, which is fed to the
top of the extraction distillation column, makes it
possible to selectively absorb and separate non-
PROCESS DESCRIPTION aromatics and benzene. The solvent recovery
column is used for separation of the non-aromatics
The industrial benzene extraction plant, shown in present at the top of the extractive distillation column
Figure 1, consists of three main sections, which are from the residual solvent. A portion of the bottom is
pre-distillation, extractive distillation and solvent fed to the solvent separator in order to recover NFM.
regeneration. In the pre-distillation section, the feed The solvent separator splits the liquid into two liquid
(consisting of benzene and non-aromatics) is phases. The non-aromatic-rich phase is returned to
separated to toluene and benzene fractions. The the Solvent Recovery Column; while the NFM-rich
benzene fraction enters the extractive distillation phase is directed to the ED Column (lean solvent
column, being recovered using the NFM solvent. In circuit). The solvent recovery column in
fact, adding NFM as solvent alters the vapor combination with the solvent separator reduces the
pressure, facilitating paraffins and naphthenes (i.e., use of NFM. This section is controlled by pressure,
non-aromatics) removal by distillation from temperature and level controllers.
Automatic control of the extractive distillation in the extractive distillation column. Since the vapor
column includes the operation of the solvent flow is very small compared to the bottom product
recovery column, the function of which always has flow, slight changes in solvent temperature cause
to be considered in conjunction with the extractive significant changes in the vapor flow. The extractive
distillation column. Reliable operation of the distillation column is very sensitive to the heat
extractive distillation column is achieved by balance, i.e., vapor flow rates could change
employing the following three controllers: remarkably when the net heat to the column changes.
a) Overhead pressure controller: This controller Higher temperature of NFM or hydrocarbon feed
influences the overhead pressure of the extractive stock in extractive distillation causes higher vapor
distillation column. Input signal to this controller is flow at constant reboiler duty. Close controlling of
the overhead pressure signal, which changes the flow heating duty of the reboiler is an essential
rate of the overhead vapor exiting the column in prerequisite for normal operation of the column.
order to maintain the pressure at set point. In fact, an Therefore, this controller maintains the overhead
increase in the overhead pressure is a result of temperature by influencing the duty of the reboiler
accumulation of vapor at the top of the column. reversely through changing the flow of the steam.
Therefore, the valve should be opened in this case, c) Bottom level controller: This controller maintains
allowing the vapors to leave the column, reaching the liquid level in the bottom section of the column.
the pressure determined by the set point. If the When the liquid level is low, the control valve on the
pressure decreases, the valve would become close liquid output of the column would be closed in order
and the vapors accumulate in the column, resulting to keep the liquid inside the column until the level
in an increase in pressure. reaches the desired point.
b) Overhead temperature controller: Flow of the Safe operation of the solvent recovery column is
overhead vapors is influenced by the thermal balance also ensured by the following controllers:
Brazilian Journal of Chemical Engineering Vol. 25, No. 04, pp. 765 - 776, October - December, 2008
768 Azadeh Ghaee, Rahmat Sotudeh-Gharebagh and Navid Mostoufi
a) Overhead pressure controller: Overhead pressure systems containing NFM, Ko et al. (2002 a) have
of the column is controlled by direct change in the shown that the NRTL model correlates these data
duty of the condenser. If the pressure is increased, properly. Therefore, the NRTL activity model was
this would lead to an increase in the air flow rate of used in the present study for the liquid phase with the
the air cooler and the duty of the condenser, so vapor binary interaction coefficient reported by Ko et al.
is condensed and vapor accumulation on the top of (2002 a). Moreover, the Peng-Robinson equation of
the column and top pressure are decreased state was used to predict the fugacity coefficient of the
accordingly. vapor because of the absence of NFM in this phase.
b) Overhead level controller: Liquid level in the
reflux drum is controlled by the flow rate of the Hypotheses
overhead product of the column. Liquid level
changes directly with the flow rate of the product. Modeling of the extractive distillation section in
This controller with the flow controller of overhead this study was done based on the following
product forms a cascade control structure. assumptions:
c) Bottom level controller: liquid level in the bottom a) Vapor and liquid are completely mixed in each
of the column is controlled directly by the flow rate stage and assumed to be at equilibrium.
of the bottom product. When the level decreases, the b) Heat of mixing can be neglected.
valve would be close and let the liquid accumulate in c) Condenser and reboiler were considered as
the column. equilibrium stages.
d) Vapor holdup is negligible compared to the total
holdup on each tray; therefore, variation of pressure
MODEL DEVELOPMENT could be neglected on each tray.
1 t
Temperature controller of the CTCED (t) Kc (T0 T(t))
extractive distillation column WI (T T(t))dt T
0
0 0
dM ' j
V ' j1 V ' j L' j1 L' j F' j S'Vj S'Lj Total mass balance at stage j
dt
dM' jx 'i, j
V' j1y'i, j1 V' j y'i, j L' j1x 'i, j1 Component mass balance at
dt
Solvent recovery column at stage j
stage j L'J x 'i, j F' jz'i S'Vj y'i, j S'Lj x 'i, j
dM' jH'i, j
V' j1H'V j1 V' jH'V j L' j1H'L j1
dt Energy balance at stage j
' 'L 'F '
L jH j F jH j S'Vj H'V j S'Lj H'L j Q j '
1 t
Pressure controller of the CPCSR (t) Kc (P '
(t) P'0 ) ' ' '
solvent recovery column WI 0 (P (t) P 0 )dt P 0
COLCSR (t) Kc (Le'Ov (t) Le'Ov0 )
Overhead level controller of the
1 t
solvent recovery column ' ' '
WI (Le
0
Ov (t) Le Ov0 )dt Le Ov0
dM
FR E Total mass balance
dt
dM i
Fzi Rx i Eyi Component mass balance
dt
n n
Energy balance
n n
R x Cp (T T
i 1
i i O) E y Cp (T T
i 1
i i O)
Brazilian Journal of Chemical Engineering Vol. 25, No. 04, pp. 765 - 776, October - December, 2008
770 Azadeh Ghaee, Rahmat Sotudeh-Gharebagh and Navid Mostoufi
T(Qx , Q, u, t) 0 (2)
Minimize
i 1
ISE (6)
definition in Eq. (1) reveals that, in the present RESULTS AND DISCUSSION
2
problem, = 0 and = PV SP
SP The results of steady state and dynamic modeling
and optimization are detailed in the following
Optimization Problem Solution sections:
Brazilian Journal of Chemical Engineering Vol. 25, No. 04, pp. 765 - 776, October - December, 2008
772 Azadeh Ghaee, Rahmat Sotudeh-Gharebagh and Navid Mostoufi
Table 4: Comparison between calculated and actual value in the extractive distillation and solvent
recovery columns
of the solvent. However, since the overhead were determined by minimizing the deviation of key
temperature is decreased (see Figure 6c), duty of the operating variables from their corresponding set
reboiler is increased, resulting in a decrease in the points [Eq. (7)]. In order to estimate the optimized
benzene recovery, as illustrated in Figure 6d. constants, each controller was optimized separately
It should also be mentioned that the optimization with constants of the other controllers assumed to be
was carried out for some other parameters such as unchanged. Final optimized constants of all
feed temperature or any other changes in feed flow controllers were found by applying the optimization
rate. With different disturbances like pulse function algorithm, taking these estimates as initial guess and
rather than a step function, different results may be letting the constants of all controllers be changed
obtained with similar trends. The model was, of during the optimization.
course, solved for different disturbances and only Optimized constants of the controllers as well as
part of the results presented here in order to keep the the corresponding constants before optimization are
paper clear and concise since other disturbances did listed in Table 5. Figures 7a-d illustrate the changes
not add new information because the trends are in the extractive distillation conditions with
rather similar. When a pulsed disturbance is optimized constants of the controllers when the flow
imposed on the process, one can better monitor the rate of the solvent to the extractive distillation
actions of the controllers in the return path too. column is increased by 15% for 30 minutes.
Since experimental data were not available for the Comparing these figures with Figures 6a-d (dynamic
new steady state that resulted from the step input for changes of the same parameters using constants of the
the validation purposes, the pulse function is used controllers before optimization) clearly reveals that the
since the end point validation of the system was controllers with optimized constants respond much
possible. faster and the process reaches steady-state almost
immediately. In fact, optimized controllers of the
Dynamic Optimization extractive distillation column are so very fast that the
solvent recovery column does not sense such a small
In this section the time dependent profiles of the deviation from steady-state. This procedure could be
parameters of the controllers (i.e., Kc and I) during applied in the advanced process control of the unit in
transition from one steady-state condition to another order to reduce off-spec products of the unit.
0.956 0.956
0.954 0.954
Benzene recovery in bottom flow
Benzene recovery in bottom flow
0.952 0.952
0.95 0.95
0.948 0.948
0.946 0.946
0.944 0.944
0.942 0.942
0.94 0.94
0 20 40 60 80 100 120 0 1 2 3 4 5
Temperature (C) Solvent to Feed ratio
Figure 4: Effect of NFM feed temperature on benzene Figure 5: The effect of solvent to feed ratio on
recovery benzene recovery
Brazilian Journal of Chemical Engineering Vol. 25, No. 04, pp. 765 - 776, October - December, 2008
774 Azadeh Ghaee, Rahmat Sotudeh-Gharebagh and Navid Mostoufi
1.82 1.82
Extractive distillation overhead pressure (bar)
1.76
1.81
1.74
1.72 1.805
1.7
1.8
1.68
1.66
1.795
1.64
1.62 1.79
0 50 100 150 0 50 100 150
Time (min) Time (min)
(a) (b)
112 0.995
Extractive distillation overhead temperature (C)
0.99
110
0.985
108 0.98
Benzene recovery
0.975
106
0.97
104 0.965
0.96
102
0.955
100 0.95
0 50 100 150 0 50 100 150
Time (min) Time (min)
(c) (d)
Figure 6: effect of increasing the flow rate of solvent on (a) Extractive distillation overhead pressure.
(b) Extractive distillation bottom liquid level. (c) Extractive distillation overhead temperature.
(d) Benzene recovery, using non-optimized controllers' constants.
Initial Optimized
Controller
KC I KC I
Pressure controller of the
100 2.25 20.42 2.03
extractive distillation column
Temperature controller of the
85 3 9.89 1
extractive distillation column
Bottom level controller of the
30 0.02 15.39 2.05
extractive distillation column
Pressure controller of the solvent
100 2.25 20.07 12.06
recovery column
Overhead level controller of the
30 0.02 8.45 2.07
solvent recovery column
Bottom level controller of the
30 0.02 10.13 55.88
solvent recovery column
2 2
1.6 1.85
1.5
1.8
1.4
1.75
1.3
1.2 1.7
0 50 100 150 0 50 100 150
Time (min) Time (min)
(a) (b)
112 1
Extractive distillation overhead temperature(C)
0.99
110
0.97
108
0.96
106 0.95
0.94
104
0.93
0.92
102
0.91
100 0.9
0 50 100 150 0 50 100 150
Time (min) Time (min)
(c) (d)
Figure 7: effect of increasing the flow rate of solvent on (a) Extractive distillation overhead pressure. (b)
Extractive distillation bottom liquid level. (c) Extractive distillation overhead temperature with optimized
controllers' constant. (d) Benzene recovery, using optimized controllers' constants.
Brazilian Journal of Chemical Engineering Vol. 25, No. 04, pp. 765 - 776, October - December, 2008
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