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Volume 4, Issue 1 2009 Article 14
Recommended Citation:
Aryana, Shahla; Ahmadi, Mitra; Gomes, Vincent G.; Romagnoli, Jose A.; and Ngian, Kian
(2009) "Modelling and Optimisation of an Industrial Ethylene Oxide Reactor," Chemical
Product and Process Modeling: Vol. 4: Iss. 1, Article 14.
DOI: 10.2202/1934-2659.1231
Available at: http://www.bepress.com/cppm/vol4/iss1/14
©2009 Berkeley Electronic Press. All rights reserved.
Modelling and Optimisation of an Industrial
Ethylene Oxide Reactor
Shahla Aryana, Mitra Ahmadi, Vincent G. Gomes, Jose A. Romagnoli, and Kian
Ngian
Abstract
A dynamic model of an industrial packed-bed multi-tubular reactor was developed to
investigate performance of an industrial ethylene oxide (EO) reactor, conducting epoxidation of
ethylene over a silver-based catalyst. The set of nonlinear kinetic rate equations for the catalytic
oxidation process in the presence of ethylene dichloride (EDC) as a moderator was coupled with
the governing heat and mass transfer equations along the packed bed. Catalyst deactivation was
modelled as a nonlinear function of operating time and the equation was benchmarked against
plant data for the period of operation. Our process model was compared with experimental data
obtained from an industrial EO reactor. The model predictions were found to agree well with the
plant data. The influences of operating parameters such as EDC level, reactant concentrations,
reactor pressure, coolant temperature and the feed temperature on reactor performance were
investigated. The variables having significant impact on work rate and selectivity were identified.
The model was used to optimise the performance of ethylene oxide reactor for maximising work
rate and selectivity.
Introduction
Ethylene oxide (EO) is a major chemical, and the global demand for ethylene
oxide continues to increase because of its importance as an intermediate in
producing antifreeze, polyester fibres and other petrochemical products. The
production of EO is a critical process because the reactor can generate eleven
times as much heat in a runaway condition as under normal operation conditions
[Rebsdat 1987; Kishor 2003]. From 0.03 to 1 mole fraction, a mixture of EO in air
is explosive at room temperature. As result, EO is normally stored at 5oC under
4.5 kg/cm2 pressure [Rebsdat, 1987]. Therefore, the safety issues for an EO
reactor are of paramount importance.
Commercial processes for producing EO are based on direct oxidation of
ethylene with pure oxygen. Complete combustion of ethylene, as well as further
oxidation of ethylene oxide to carbon dioxide and water, also occurs during the
reaction. Silver catalyst, packed in tubes with promoters, is the state-of-the-art
catalyst for ethylene oxidation, because of its high activity and selectivity for EO.
Organohalide inhibitors such as 1,2-dichloroethane or ethylene dichloride (EDC)
are added to control the reaction rate and improve the selectivity of the catalyst
and its concentration is usually 1-3 ppm. The complete oxidation of ethylene is
inhibited to a great extent by EDC than partial oxidation; hence the selectivity for
ethylene oxide is promoted. Thus, EDC is termed an “inhibitor” and a “promoter”
due to its promoting effect on selectivity and inhibiting effect on oxidation.
Since the reactions involved are highly exothermic, heat transfer
efficiency is critical. Multi-tubular fixed bed reactors are widely used in industrial
EO production. Heat is removed by a coolant circulating through the shell side.
Failure to remove the heat adequately may lead to thermal runaway. With time,
the silver based catalysts for EO production exhibit a continuous loss of activity
and selectivity, which is accelerated if the reactor is run at higher than necessary
temperatures. Run-away conditions and burn-out of the catalyst and equipment
may transpire at elevated temperatures. These considerations are particularly
important in industrial EO manufacture, where maximising production and
minimising risks under variable conditions are imperative.
Several authors investigated the modelling and simulation of ethylene
epoxidation [Azevedo, 1990; Cornelio, 2006; Zhou & Yuan, 2005] however, the
published information is insufficient. Zhou and Yuan [2005] studied the steady-
state and dynamic optimisation of an ethylene epoxidation process. They
investigated the effect of inlet ethylene, O2 and CO2 concentrations, and operating
pressure on productivity but did not consider the effect of ethylene oxide
oxidation, which has significant consequences. The current work considered all
relevant reactions for analysis and optimization of the EO reactor over the period
of catalyst life time.
Reaction Kinetics
(1)
½ O2
C2H4 C2H4O
3O2 5/2 O2
(2) (3)
2CO2 + 2H2O
Ri = f i (T , p j ) × ai (t, T , pk ) × Ci Eq.1
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main reactions with effects of EDC as inhibitor, were adapted from elsewhere
[Petrov et al., 1984, 1986, 1988, Eliyas et al., 1988] as given below:
f (3) = − × − 0 .5 2
× ρ cat Eq.4
2 (1 + K 9 P0 xy + K 10 P. 0oxy. 5 + K 11 PEO + K 12 PEO P. oxy )
where Eth, Oxy, EO, and EDC stand for ethylene, oxygen, ethylene oxide and
dichloroethane, respectively. The kinetic rate constants k1 –k12 have an Arrhenius
dependency on temperature and can be expressed as:
− E a ,i
K i =1 − 4 , 7 − 8 = K 0 , i e ( )
RT S
E a ,i
K i = 5 , 6 , 9 −12 = K 0 , i e ( )
RT S
The equation parameters are given elsewhere [Petrov et al, 1986]. The
correction factors (Ci) were calculated based on the information provided by the
catalyst vendor. The catalyst density of 1260 kg/m3 is calculated from catalyst
pellet packing data received from plant.
Process Description
The product gas from the outlet of the reactor preheats the inlet gas in a
separate heat exchanger. The product gas is then stripped off ethylene oxide in 2
scrubbers. The stripped gas is thereafter de-carbonated before being recycled
back to the reactor. The outlet cooling oil is cooled in a kettle boiler to produce
saturated steam.
The raw feed materials including pure oxygen and ethylene mixed with
recycle gas stream (from the scrubbers), are heated and fed to the reactor. The
reactor feed consists of 7 main components including: ethylene, oxygen, ethylene
oxide (usually less than 0.01%), carbon dioxide, water (reaction’s by-products),
argon (built up in the system by adding oxygen) and nitrogen (used as ballast).
Also, a small concentration of 1,2-dichloroethane (EDC) and ethane are
intentionally added to the feed to improve reactor selectivity and to moderate the
oxidation. A typical reactor feed and product composition is shown in Table 1.
Table 2 shows the reactor typical operating conditions. We note that a
difference in oil inlet temperature between start of run (SOR) and end of run
(EOR) exists due to catalyst deactivation.
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Model Development
Mass Balance
The species mass balance for the gas phase is given by:
∂F j ∂F j ∂ 2 Fj
= Vgas × ( ∑ν j / ν BASE ( i ) × Ri ) × AC ,T × (1 − e) − Vgas × + Dax × Eq.5
∂t i =1−3 ∂Z ∂Z 2
∂FC2 H 4
= V gas × (2 × R1 + 1 / 3 × R2 ) × AC ,T × (1 − e) −
∂t Eq.6
∂FC2 H 4 ∂ 2 FC2 H 4
V gas × + Dax ×
∂Z ∂Z 2
∂FEO ∂F
= −V gas × (2 × R1 − 2 / 5 × R3 ) × AC ,T × (1 − e) − V gas × EO +
∂t ∂Z
Eq.8
∂ FEO
2
Dax ×
∂Z 2
∂FCO2 ∂FCO2
= −V gas × (2 / 3 × R2 + 4 / 5 × R3 ) × AC ,T × (1 − e) − V gas × +
∂t ∂Z
Eq.9
∂ 2 FCO2
Dax ×
∂Z 2
∂FH 2O ∂FH 2O
= −V gas × (2 / 3 × R2 + 4 / 5 × R3 ) × AC ,T × (1 − e) − V gas × +
∂t ∂Z
Eq.10
∂ 2 FH 2O
Dax ×
∂Z 2
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∂ Twall ,O
ρ wall × Cp wall × = α s × (4 × DO ) ( DO2 − DI2 ) × (Toil − Twall ,O )
∂t Eq.13
− α wall × (4 × DO ) ( DO2 − DI2 ) × (Twall ,O − Twall , I )
The inner sides of the tube wall exchange heat with the outer side of tube wall as
well as the gas, where α wall the tube side heat transfer coefficient is:
∂ Twall , I
ρ wall × Cp wall × = α wall × (4 × DO ) ( DO2 − DI2 ) × (Twall ,O − Twall , I )
∂t Eq.14
− α T × (4 × DI ) ( D − D ) × (Twall , I − Tgas )
2
O
2
I
∂ Toil ∂T
ρ oil × Cp oil × Ac ,c × = −Goil × Cp oil × oil + α s × (π × N T × DO )
∂t ∂Z Eq.15
× (Twall ,O − Toil ) + U loss × (π × DS ) × (Tamb − Toil )
Catalyst Deactivation
The main mechanisms of catalyst deactivation can be grouped into six types: (i)
poisoning, (ii) fouling, (iii) thermal degradation, (iv) 1,2-dichloroethane vapor
formation accompanied by transport, (v) vapor–solid and/or solid–solid reactions,
and (vi) attrition/crushing [Bartholomew, 2001].
The catalyst deactivation model used in this study is derived from
Boskovic et al. [2004a] for a commercial Ag/Ag2O3 catalyst. The equation
describes catalyst activity decline as a function of time with a term of steady-state
activity, ass, reached at infinite time [Fuentes, 1985]:
da
− = K d POα2 ( a − a ss ) d
dt Eq.16
Ea
a = a ss + (1 − a ss ) exp( − K d0 ( − ) POα2 t ) Eq.17
RT
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0.8
0.7
Deact 2
0.6
0.5
0 200 400 600 800 1000
Time (day)
The catalyst temperature has a major effect on the reactor performance, catalyst
aging and safety. Since no plant data are available for the catalyst temperature,
data for the oil and gas outlet temperature were used to validate our model. Figure
4 and Figure 5 show the oil and gas outlet temperatures of the model predictions
against plant data during 3 years of reactor operation. The model predictions are
in reasonable agreement with plant operating data. However, some discrepancies
exist due to error in measurement related to model input data. We observe that the
oil inlet temperature increases with time to compensate for the loss in catalyst
activity and maintain desired production rate and selectivity.
270
Plant Data
265
Model Prediction
260
Temp (C) 255
250
245
240
235
230
0 200 400 600 800 1000
Time (day)
Figure 4- Comparison of outlet oil temperature predictions with plant data during
3 years operation
270
Plant Data
265
Model Prediction
260
255
Temp (C)
250
245
240
235
230
0 200 400 600 800 1000
Time (day)
Figure 5- Comparison of outlet gas temperature predictions with plant data during
3 years operation
The other important parameters are selectivity and work-rate. These two
parameters represent the EO reactor efficiency and product rate, respectively. The
selectivity (Sel%) and the work-rate (WR) definitions we used are given as
follows:
EO produced
Sel % = × 100 Eq.18
Total ethylene consumed
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90%
Plant Data
Model Prediction
85%
Selectivity (%)
80%
75%
70%
0 200 400 600 800 1000
Time (day)
Overall, the model predictions for the selectivity and the work-rate against
the plant data are satisfactory. Whenever the plant data for the input variables
were available, the model predictions were very close to plant data. However,
when accurate plant data are unavailable, we noticed disagreements between
model predictions and plant data. For example, EDC concentration has significant
effect on the selectivity and work-rate; however, accurate data on EDC
concentration (ppm levels) were not always available. Despite the uncertainties in
plant data and unknown disturbances, our model prediction show reasonable
agreement with the plant data.
160
Plant Data
Model Prediction
Work Rate (T/Day)
140
120
100
80
0 200 400 600 800 1000
Time (Day)
Sensitivity Analysis
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280
270
Time = 100 Sec
260
220
210
200
190
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7 7.5
Distance along the reactor (m)
We note that the first and the last half meter of the 7.35 meter long tubes
have no catalyst which means no reaction, so, just heat exchange between the oil
and gas take place. During the first half meter of tubes and the last half meter,
respectively, the model shows a significant rise and small decline in the gas
temperature due to heat exchanger between gas and oil.
Figure 9 shows the effect of step increasing (+5%) the oil inlet temperature
(@ t = 0 s) on the work-rate and selectivity. With increasing oil temperature, the
work-rate increases by about 12% while selectivity decreases by 2.5% as be
expected, since the reaction rates of all the three reactions increase with
temperature and the work-rate increases with increasing oil temperature.
However, a decrease on selectivity is expected due to stronger effect of
temperature on the undesired reaction (the total ethylene and EO oxidation) than
the desired one (partial oxidation of ethylene).
130 81.5
81
125
80.5
Selectivity (%)
Work-rate
Work Rate (Ton/day)
Selectivity 80
120
79.5
79
115
78.5
110 78
0 40 80 120 160 200
Time (s)
Figure 9- Selectivity and work-rate with +5% step-changes in oil inlet temperature
For further investigation, the amount of heat transferred between the tube
wall and the coolant oil is shown in Figure 10. This graph shows that in the
beginning, the amount of transferred heat drops dramatically due to the step
increase of shell side temperature (oil inlet temperature) which results in
decreasing the temperature difference between the shell side and the gas phase.
Consequently, the bedside temperature starts to increase enhancing the reactions
thereby increasing the released heat by reactions and the reactor inside
temperature. Thus, heat transfer starts to increase. The dramatic decrease in heat
transfer rate could lead to a thermal runaway condition and catalyst damage.
248 3000
246 2500
2000
242
Oil Inlet temp 1500
240 Heat Transferred
1000
238
Possible
236 Runaway 500
Condition
234 0
0 10 20 30 40 50 60 70 80 90 100
Time (s)
Figure 10- The oil inlet temperature and transferred heat between oil and tube wall
in response to a +5% step-change in oil inlet temperature
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250 2700
2500
246
230 1500
0 10 20 30 40 50
Time (min)
Figure 11- Oil inlet temperature and heat transferred between oil and tube wall
with +5% linear change in oil inlet temperature
130 81.5
Work-rate
81
Selectivity
125
80.5 Selectivity (%)
Work Rate (Ton/day)
80
120
79.5
79
115
78.5
110 78
0 10 20 30 40 50
Time (min)
EDC level
Selectivity (%)
Work Rate (Ton/day)
85
84
105
83
82
95 81
80
79
85 78
1 1.4 1.8 2.2 2.6 3
EDC Level (ppm)
110
100
90
80
Mole Flow (mol/s)
70 EO Mole Flow
50
40
30
20
10
1 1.4 1.8 2.2 2.6 3
EDC Level (ppm)
Figure 14- The influence of EDC level on product mole flow (EO and CO2)
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Reactant
150 83
82.5
140 Work-rate
Selectivity 82
130 81.5
Selectivity (%)
Work Rate (Ton/day)
81
120
80.5
110
80
100 79.5
79
90
78.5
80 78
5 5.5 6 6.5 7 7.5 8
Oxygen Mole %
Figure 15- The influence of inlet oxygen concentration on work-rate and selectivity
150 81.5
140
81.1
130
Work-rate
Selectivity (%)
Work Rate (Ton/day)
Selectivity 80.7
120
110
80.3
100
79.9
90
80 79.5
15 16 17 18 19
Ethylene Mole %
Figure 16- The influence of inlet ethylene concentration on work-rate and selectivity
Optimisation
For the EO reactor, higher temperature leads to excessive carbon dioxide and
water formation which results in loss of selectivity. Lower temperatures result in
lower conversion and loss of productivity. Thus optimisation is to maximise
conversion of ethylene to EO (selectivity) within the flammability limit for safe
operation. The objective function is defined to maximise selectivity for desired
production rate (work rate).
Flammability is a major constraint of the EO reactor. The flammability
limit gives the proportion of combustible gases in a mixture, between which limits
this mixture is flammable. It is known that in actual practice in order to remain
outside the flammability limit of the gas mixture the concentration of oxygen has
to be lowered as the concentration of ethylene is raised. The actual safe operating
ranges depend, along with the gas composition (reactants and balance gases), also
on individual plant conditions such as temperature and pressure. Therefore in each
individual plant a flammability equation is used to determine the concentration of
oxygen which may be used with any given concentration of ethylene. The
flammability equation can be expressed via a flammability curve.
The flammability limit is calculated based on the maximum allowable
oxygen limit using equation provided by industry patent. Based on our sensitivity
analysis, the coolant temperature, reactant concentration and EDC level in the
feed, which significantly affect the reactor performance, can be manipulated for
maximal profit. EO has a significantly negative effect on selectivity and work-
rate. In practice, its concentration is kept as low as possible. The inlet feed
temperature has insignificant effect on productivity and is unsuited as a
manipulated variable. Steady state optimisation was carried out for 2 cases:
¾ Case 1: Low production rate (110 Ton/day EO)
¾ Case 2: High production rate (130 Ton/day EO)
The constraints and the final values for first and second case studies are shown in
Tables 3 and 4, respectively.
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The control variables and their optimum values the first and second case
studies are shown in Table 5 and 6, respectively. The EDC level, ethylene and
oxygen concentration in the feed and oil inlet temperature are chosen as control
variables. At the start of the operation, the results show that in both low and high
production cases, ethylene and EDC concentrations act as active bounds.
Furthermore, in high production rate (second case), the oxygen concentration acts
as lower active bound according to the flammability point.
selectivity. Also the results show that the optimum selectivity in the first case
(low work-rate) is higher than the second case (high work-rate). To increase the
work-rate, the oil inlet temperature should be increased to enhance the reactions,
although the selectivity would be decreased. Nevertheless, the result shows that
the selectivity could be improved by keeping the control variable close to the
optimal point.
Dynamic Optimisation
t min
f ≤ t f ≤ t max
f Eq.23
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according to the functionality u (t ) over the span of the time horizon [0, t f ] . The
latter indicates parametric variables that are fixed at a value.
Equation 21 denotes the set of differential-algebraic equations (DAEs)
representing the process model, while equation 22 symbolises a set of additional
equations (initial conditions) that must be satisfied at the beginning of the
optimisation horizon. In these equations x and y denote differential and algebraic
variables respectively, and indicates the time derivatives of x. Equations 23, 24
and 25 denote lower and upper bounds on the decision variables, indicated by the
superscripts min and max, respectively.
There are also other types of constraints and importantly those which
bound the decision variables and in some cases the time horizon of the process.
Further constraints are in the form of interior point constraints, path constraints
and end-point constraint. The end product concentration must be greater than
99%, a purity demand. This constraint can be formulated as an inequality where
the constrained condition must be less than a desired value (Equation 26), greater
than a desired value or within a desired region or may be an equality constraint
where the final value must equal a desired value (Equation 27).
Equation 28 denotes interior-point constraint variables, which are used to
enforce process variables to lie within the defined upper and lower bounds at any
other time except the end of the optimisation horizon. By definition, these are
inequality constraints. Although the inclusion of these constraints is not strictly
essential, research [Vassiliadis et al., 1994] demonstrated that adopting them may
increase the robustness and efficiency of algorithms handling inequality
constraints. Eq. 29 symbolises the inequality path constraints mentioned above.
Two case studies were considered:
¾ Case 1: Optimal coolant temperature profile during 3 years operating
time.
¾ Case 2: The optimal profiles for coolant temperature and oxygen inlet
concentration with transition between low production (110 Ton/day) and
high production rate (127 Ton/day).
Results from steady state optimisation were used as initial conditions for
the dynamic optimisation. Since the catalyst decays continuously, the production
process is dynamic and a dynamic optimisation strategy was used. However, it is
infeasible to simultaneously change all the variables dynamically. Experience
shows that the improvement of the optimisation performance with more than one
variable in dynamic optimisation is minor over that when only one variable is
varied dynamically while others are fixed to constant sub-optimal values [Bonvin,
1998]. The variable that is most sensitive to dynamic behavior is bed temperature,
which is responsible for thermal sintering and catalyst decay.Activity losses are
attributed to a decrease of the catalyst surface area, by poisoning or sintering, and
Case 1
Figure 17 shows the oil inlet temperature optimal profile to obtain the desired
work-rate (127 Ton/day) over the 3 year operation which maximises selectivity.
As observed, the oil inlet temperature needs to be increased by 15 ºC to
compensate for catalyst deactivation. By increasing oil inlet temperature, it is
expected that the selectivity will decrease gradually. The loss of selectivity
according to the optimal condition is shown Figure 17.
250 81.2
T_Oil
TOil_In
In
81
247 Selectivity
Selectivity 80.8
Selectivity (%)
80.6
244
80.4
Temp (°C)
80.2
241
80
238 79.8
79.6
235 79.4
0 6 12 18 24 30 36
Time (month)
Figure 17- Optimal oil inlet and selectivity losses profile for 3 years operating time
Case 2
Oil inlet temperature and oxygen inlet concentration were used as control
variables to shift work-rate from 110 (Ton/day) to 127 (Ton/day) and objective
function was to maximise selectivity. The ethylene inlet concentration and the
EDC levels are kept constant at 17.5 mol% and 1.5 ppm, respectively. It was
assumed that the transition operation takes place in 2 hours. To avoid a runaway
condition, linear increase was suggested. Therefore, piecewise-linear control was
used for the oxygen inlet concentration and oil inlet temperature.
Figure 18 shows the optimal transition profiles for the oil inlet temperature
and the optimal transition profiles for the oxygen concentration. The results show
that to increase the work-rate from 110 (Ton/day) to 127 (Ton/day), the oil inlet
temperature and the oxygen concentration require to increase by 4 ºC and 0.5
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mol%, respectively. Also, Figure 18 shows the change in work-rate during the
transition period. By increasing oil inlet temperature, the selectivity decreases by
1.2% due to increasing oil inlet temperature.
7 238
6.8 237
(Ton/day)
(%)
Temp (°C)
6.6 236
Percent
6.4 235
Rate
O2 Mole Percent
O2 Mole Frac %
O2 Mole
T_Oil
Toil-In
In
Work
6.2 234
6 233
0 2000 4000 6000 8000
Time (s)
Conclusions
Nomenclature
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NT number of tubes
Pi partial pressure of component i [in bar unless noted otherwise]
S and SV specific surface area [m2/m3]
Sel Selectivity (%)
Ri overall reaction rate [kmol O2/m3 (cat) s]
t time [s]
T temperature [°C unless noted otherwise]
U heat tranfer (overall unless stated) [kW/m2 °C]
WR workrate (ton/day)
Vgas velocity [m/s]
Z length in tube direction
Greek letters
Subscripts
0 inlet condition
1 reaction 1 (C2H4 + 1/2O2 ⇒ C2H4O)
2 reaction 2 (C2H4 + 3O2 ⇒ 2CO2 + 2H2O)
3 reaction 3 (C2H40 + 5/2O2 ⇒ 2CO2 + 2H2O)
amb ambient
b catalyst bed
c cross (e.g. area)
cat catalyst
Eth ethylene
EO ethylene oxide
Oxy oxygen
EDC ethylene Dichloride
gas gas phase
H2O water
I inside tube
in inlet
Loss heat loss
O outside tube
oil cooling oil
out outlet
p particle
S shell
T tube or total
wall tube wall
References
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