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Production of ethylene and cyclohexane in a catalytic membrane reactor

Article  in  Chemical Engineering and Processing · November 2005

DOI: 10.1016/j.cep.2005.02.004

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 Chemical Engineering and Processing 44 (2005) 1188–1196

Production of ethylene and cyclohexane in a catalytic

membrane reactor
M.E.E. Abashar ∗ , A.A. Al-Rabiah
Department of Chemical Engineering, King Saud University, P.O. Box 800, Riyadh 11421, Saudi Arabia

Received 27 July 2004; received in revised form 4 October 2004; accepted 21 February 2005
Available online 31 May 2005

Abstract

A rigorous two-dimensional mathematical model is used to simulate a bench-scale membrane reactor for ethane dehydrogenation to ethylene
using a palladium-based membrane. Since the reaction is equilibrium limited the removal of the product hydrogen by the membrane shifts
the thermodynamic equilibrium. For further displacement of the thermodynamic equilibrium, auxiliary hydrogenation reaction of benzene
to cyclohexane over nickel catalyst is used to remove part of hydrogen. The two catalysts are loaded together in a well-mixed pattern
configuration. Optimal conditions are observed and explanations offered. An effective length criterion for the optimal conditions is presented.
The results show that the well-mixed pattern strategy has substantial improvement in the reactor performance in terms of high conversions,
low temperatures and reduced mass of the catalyst used. The investigation, although is restricted to two catalyst, has uncovered a part of the
rich characteristics of this system.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Cyclohexane; Ethylene; Membrane reactor; Mathematical modeling

1. Introduction Ethylene is commercially produced by thermal cracking

Ethylene is one of the most important basic chemicals.
The importance of ethylene is derived from the double bond
in its molecular structure. The double bond makes ethylene
very reactive to a variety of intermediate and end products [1].
The major use of ethylene is to produce low and high-density
polyethylenes, which are used in many industrial and domes-
tic products. Other significant uses of ethylene include chlo-
rination to ethylene dichloride, used in the manufacture of
polyvinyl chloride (PVC), oxidation to ethylene oxide, which
is an intermediate in the manufacture of polyester fibers and
films, and the conversion to ethylbenzene, an intermediate in
the manufacture of polystyrene [2].
Abbreviations: CT, contact time; FBR, fixed bed reactor; FBMR, fixed
bed membrane reactor; FBRA, fixed bed reactor with auxiliary reaction;
FBMRA, fixed bed membrane reactor with auxiliary reaction; SR, sweep
ratio
∗ Corresponding author. Tel.: +966 1 4675843; fax: +966 1 4678770.
E-mail address: mabashar@ksu.edu.sa (M.E.E. Abashar).
of natural gas liquids (NGLs) or crude oil fractions in the
presence of steam. Thermal cracking employs elevated tem-
peratures and the cost of separation and purification of the
products is very high [3]. This provides a strong economic
incentive for reexamining the impact of new technologies
such as catalytic dehydrogenation reactions in catalytic mem-
brane reactors to overcome high temperature requirements,
separation and purification problems in the existing ethylene
production technology.
In the last few years the research interest has been focused
on catalytic membrane reactors as multi-functional reactors
[4–15]. The main advantages of the membrane reactors are:
shift of the thermodynamic equilibrium, simultaneous reac-
tion and separation of products, enhancement of yield and
selectivity, control of reactants distribution and low costs.
Despite the significant advantages of the membrane catalytic
reactors, still the membrane reactor is not fully understood
and the technology is limited to certain kind of reactions and
is not commercially utilized.

0255-2701/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2005.02.004
 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196 1189

Recently, several studies have shown that the performance where I at temperature (T0 ) is given by
of the fixed bed catalytic reactors (FBRs) and fixed bed cat-
H ◦ a b c 2 d 3
alytic membrane reactors (FBMRs) has improved signifi- I= − ln T0 − T0 − T − T
cantly by introduction of the dual-functionality via structured RT0 R 2R 6R 0 12R 0
pattern (either mixed or layered configuration) of the catalyst e 4 G◦
− T − (5)
bed [5–7,16]. The purpose of these patterns is to couple the 20R 0 RT0
reactions in different ways to achieve certain degree of inte-
gration of heat, further shift of thermodynamic equilibrium 2.2. Auxiliary reaction
and simultaneous production of more than one product.
Ethane dehydrogenation to ethylene is endothermic and The purpose of the auxiliary reaction is to remove hy-
thermodynamically limited reaction. The membrane reactor drogen for further displacement of the dehydrogenation ther-
technology is very attractive field to be implemented in this modynamic equilibrium. This may be accomplished through
respect, however very little research work has been done so hydrogenation of benzene on nickel catalysts to cyclohexane.
far [9,10,12]. The authors [9,10,12] have shown experimen- The kinetics is given by [19]:
tally that the conversion of ethane to ethylene has improved
C6 H6 + 3H2 → C6 H12 (6)
substantially by implementing the membrane reactors, how-
ever high conversions still require high temperatures. The P C 6 H6 P H2
R2 = k2 KB (7)
objective of this investigation is to explore the potential ap- (1 + KB PC6 H6 )(PC6 H6 + PH2 )
plication of integrated catalytic membrane reactors for simul-
taneous production of ethylene and cyclohexane at relatively the rate constant is given by
 
low temperatures. The concept of the dual-functionality of the 6038.65
catalyst bed is implemented in an experimental co-current k2 = 121.11 × exp − (8)
T
composite membrane reactor. The thermodynamic equilib-
rium is shifted by the membrane and auxiliary reaction. A and the adsorption equilibrium constant of benzene is given
rigorous mathematical model is utilized to study the influ- by
ence of various parameters and to identify the key parame-  
3019.32
ters that are likely to affect the catalyst pattern strategies and KB = 788.0 × exp − (9)
T
the performance of the membrane reactors. This preliminary
investigation is restricted to two types of catalysts.
3. Hydrogen permeation rate

2. Reaction kinetics The composite membrane used in this study is made of a

very thin layer of palladium–silver alloy. The membrane is
2.1. Primary reaction deposited as a continuous layer on the outer surface of ther-
mostable support. The details of the membrane are given by
The rate expression for dehydrogenation of ethane: Gobina et al. [11]. The permeation rate of hydrogen through
the composite membrane is assumed to obey the half power
C2 H6
C2 H4 + H2 (1) pressure law [20,21]:
    
is given by [10]: A
QH2 = Q0 PHt 2 − PHs 2 (10)

 δ
P C H PH
R1 = k1 PC2 H6 − 2 4 2 (2) where QH2 is the hydrogen permeation rate, A the membrane
K1
area available for flow, δ the Pd–Ag alloy film thickness, and
the rate constant is given by (PHt 2 ) and (PHs 2 ) are the hydrogen partial pressures in the
  tube and shell sides, respectively. The permeability constant
9090.69
k1 = 4.39 exp − (3) of hydrogen (Q0 ) has been determined experimentally by
T Gobina et al. [11], as follows:
 
and the equilibrium constant (K1 ) as a function of tempera- −12 767.38
ture (T) is calculated from the standard heat of reaction and Q0 = 1.0061 × 10 exp − (11)
T
standard Gibbs free-energy as follows [17,18]:
H ◦ a b c 2 d 3
ln K1 = − + ln T + T+ T + T 4. Model development
RT R 2R 6R 12R
e 4 A rigorous two-dimensional model is developed for the
+ T +I (4)
20R dehydrogenation of ethane and hydrogenation of benzene in
1190 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196

a co-current packed bed membrane reactor. A schematic di- The boundary conditions are
agram of the composite Pd–Ag membrane reactor is given
in Fig. 1. The following simplifying assumptions are used in ∂Cit
L = 0, Cit = Cift ; r1 = 0, = 0;
the derivation of the conservation equations of the model: ∂r1

1. The reactor operates at steady state conditions and isother- r1 = R1 , Cit = Cic ; i = 1–5 (13)
mally with negligible pressure drop.
2. The membrane has exclusive selectivity for hydrogen. The effective diffusivity coefficient is calculated from [22]:
This assumption is justified by the experimental evidence 1 − yi
of Gobina et al. [11]. Dei = (14)

n
3. The reactions are considered to take place only in the tube (yi /Dij )
side. j=1
j = i
4. Negligible diffusion resistances within the catalyst parti-
cles.
5. Axial diffusion is negligible. 4.2. Ceramic support
6. The ideal gas law is obeyed.
The differential mass balance equations on component i
is given by
4.1. Tube side


Deci ε2 ∂ ∂Cc
The differential mass balance equations on component i r2 i = 0, R1 < r2 < R2 , i = 1–5
r2 ∂r2 ∂r2
is given by (15)


∂Cit Det i ε1 L0 1 ∂ ∂Cit (1 − ε1 )L0
= r1 + The boundary conditions are
∂L ul r1 ∂r1 ∂r1 ul

n=2 ∂Cit

 r2 = R1 , Cit = Cic , Dei ε1

t
× θj γij Rj ρj , 0 < r1 < R1 , i = 1–5 (12) ∂r1
r1 =R1
j=1

∂Cic

= Dei ε2
c
, i = 1–5;
where i = 1, 2, 3, 4 and 5 for C2 H6 , C2 H4 , H2 , C6 H6 and ∂r2
r2 =R1
C6 H12 , respectively, γ ij the stiochiometric coefficient of com-

∂Cic

ponent i in the jth reaction (negative for reactants) and θ j is r 2 = R2 , = 0, i = 1, 2, 4, 5 (16)

the volume fraction of catalyst j. ∂r2
r2 =R2

Fig. 1. Schematic representation of the co-current catalytic membrane reactor.

 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196 1191

for H2 are ignored due to the small particle used. Abashar [24] has

  given special attention in his published article to the total dif-
∂C3c
Q   

=
0
PHt 2 − PHs 2 (17) fusive fluxes in the catalyst pellet in the pilot plant reactor.

∂r2 r2 =R2 δDe3 ε2

c
These are described by implementing the dusty gas model
to gain an insight into various mass transfer processes that
4.3. Shell side take place inside the catalyst pellet through the effectiveness
factor concept.
The differential mass balance on hydrogen gives:
6.1. Single catalyst pattern
dFHs 2
= Q H2 (18)
dL In this case, the fixed bed reactor (FBR) and the fixed bed
membrane reactor (FBMR) are packed with catalyst 1 only,
i.e. the dehydrogenation reaction of ethane (the primary re-
5. Solution of the model equations action) proceeds alone. A comparison is made for identical
feed conditions and catalyst. Since this reaction is highly en-
The global orthogonal collocation technique [23] is imple- dothermic, the comparison is made at isothermal conditions.
mented to change the set of the partial differential equations Fig. 2 compares the performance of the fixed bed reactor
(Eqs. (12) and (15)) into a set of ordinary equations. The radial (FBR) and fixed bed membrane reactor (FBMR) at high tem-
derivatives are discretized using six orthogonal collocation perature (T = 1000.0 K). The contact time (CT) is defined as
points. Then, the new set of ordinary differential equations the mass of the catalyst in the reactor divided by the feed mo-
and the shell side equation (18) are integrated by an IMSL lar flow rate of ethane. The sweep ratio (SR) is defined as the
subroutine (DGEAR) based on a Runge–Kutta–Verner fifth- ratio of the sweep gas rate to that of the feed rate. Fig. 2(a)
and sixth-order method with automatic step size and double shows that the fixed bed reactor (FBR) attains the thermo-
precision to ensure accuracy. dynamic equilibrium and only a small part of the reactor is
utilized. The poor performance shown by the fixed bed reactor
indicates that the fixed bed reactor is not suitable for ethane
6. Results and discussion dehydrogenation at these operating conditions. Substantial
improvement in the ethane conversion is achieved by the fixed
The catalyst used for the dehydrogenation of ethane (the bed membrane reactor (FBMR). The reactor achieves about
primary reaction) is considered to be catalyst 1 and that used 80.16% exit ethane conversion. As shown in Fig. 2(b) that
for the hydrogenation of benzene (the auxiliary reaction) is the driving force for hydrogen permeation decreases along
catalyst 2. Two cases are investigated. The first case involves the length of the reactor and approaches zero and hence com-
only catalyst 1 and the second case involves two types of cat- plete conversion of ethane cannot be achieved. In fact, about
alysts, which are well mixed. Co-current mode of operation 40% of the reactor has very little contribution.
is considered in this study. The data used for mathematical Fig. 3 shows how the exit ethane conversion varies as a
simulation in this investigation are presented in Table 1. In function of temperature for different contact times (CTs).
fact, this hydrogenation–dehydrogenation study differs con- The influence of the contact time in the temperature range of
siderably from the recent published one by Abashar [24]. 800–1000 K is pronounced.
The main differences are: In this study we are dealing with a The effect of the sweep ratio (SR) on the exit ethane con-
different system carried out in a bench scale reactor. The mod- version for various temperatures is shown in Fig. 4. It is
eling level here is very sophisticated using a rigorous two- clearly shown that the increase of the sweep ratio has an
dimensional model. The intraparticle diffusion resistances overall positive effect on the conversion by enhancing the
hydrogen permeation driving force due to the reduction of
Table 1
Data for the membrane reactor [10,19]
the partial pressure of hydrogen in the shell side. In fact, the
complete conversion of ethane occurs at high temperatures
Reactor length (m) 0.15
Radius of catalyst bed (m) 0.39 × 10−2
(T > 1100.0 K) for all sweep ratios.
Palladium–silver alloy film thickness (␮m) 6.0 Sensitivity analysis for the effect of membrane thickness
Thickness of ceramic support (m) 0.11 × 10−2 on the exit ethane conversion is shown in Fig. 5. As it can
Diameter of catalyst pellets (m) (0.15–0.2) × 10−2 be seen, the membrane thickness has little effect on the exit
ρ1 (kg/m3 ) 355.8 ethane conversion. This interesting result reflects the com-
ρ2 (kg/m3 ) 1200.0
ε1 0.5
plex interaction of many factors. According to Eq. (10), the
ε2 0.28 decrease of the membrane thickness has a substantial effect
Catalyst weight (kg) 2.55 × 10−3 on the hydrogen permeation rate. However, the performance
Pressure in tube side (kPa) 150.0 of the membrane reactor does not depend only on the perme-
Pressure of sweep gas (kPa) 100.0 ation rate of the hydrogen. It depends on a complex interac-
Flow rate of sweep gas stream (m3 (STP)/s) 5.000 × 10−6
tion of the feed rate, reaction rate and permeation rate. The
1192 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196
Fig. 2. Comparison of fixed bed (FBR) and fixed bed membrane (FBMR) re-
actors: (a) ethane conversion vs. dimensionless reactor length; (b) hydrogen
partial pressure vs. dimensionless reactor length.
decrease of the membrane thickness increases the hydrogen
permeation rate, then equilibration of the partial pressures
on each side of the membrane occurs and the permeation
rate drops accordingly. On the other hand, if the equilibrium
is approached too slowly the removal of hydrogen will not
affect the conversion in this small reaction volume. In fact,
the amount of hydrogen permeating per unit time through a
specific membrane area must match the amount of hydrogen
produced by the reaction in the given volume of the reactor
per unit time at the existing driving force. The hydrogen pro-
duction and removal should be at comparable rates. Neither
the production rate nor removal rate of hydrogen are constant
within this small reaction volume. This may explain the little
Fig. 3. Exit ethane conversion as a function of temperature for various con-
tact time (CT).
Fig. 4. Effect of sweep ratio (SR) on the exit ethane conversion for various
temperatures.
effect of the decrease of the membrane thickness on the exit
ethane conversion.
Fig. 6 shows the effect of tube side total pressure (Pt )
on the exit ethane conversion. The dehydrogenation reac-
tion of ethane (Eq. (1)) shows that the total number of moles
increases. Therefore, the reaction is thermodynamically fa-
vored at low pressure according to Le Châtelier’s [5] principle
and at the same time the high pressure favors the hydrogen
permeation driving force. As one can see clearly that the
decrease of pressure has positive effect on the exit ethane
conversion. This could be due to the fact that under these
operating conditions the effect of decrease of pressure on
the displacement of the thermodynamic equilibrium is more
 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196
Fig. 5. Effect of membrane thickness (δ) on exit ethane conversion.
Fig. 6. Effect of pressure in the tube side on the exit ethane conversion.
pronounced than increase of pressure, i.e. the hydrogen per-
meation driving force. It is interesting to note that there exists
a temperature (T = 970 K) beyond which the ethane conver-
sion becomes insensitive to the pressure.
6.2. Two catalysts pattern
This case represents the well-mixed pattern in which two
catalysts are involved in the reactions. The well-mixed cata-
lyst pattern can be made of composite pellets, i.e. the two cat-
alysts are co-extruded into composite pellets or two discrete
type of pellets that are physically well mixed [5,6]. Here, the
well-mixed pattern involves loading the reactor with catalysts
1 and 2 after physically well mixed as shown in Fig. 1.
1193
Fig. 7. Comparison of fixed bed reactor (FBR), fixed bed membrane reactor
(FBMR), fixed bed reactor with auxiliary reaction (FBRA) and fixed bed
membrane reactor with auxiliary reaction (FBMRA).
Fig. 7 compares the fixed bed reactor (FBR), fixed bed
membrane reactor (FBMR), fixed bed reactor with auxil-
iary reaction (FBRA) and fixed bed membrane reactor with
auxiliary reaction (FBMRA) at relatively low temperature
(T = 800 K). It is clearly shown that substantial improvement
in the ethane conversion is achieved in the FBRA by addi-
tion of small amount of catalyst 2 (θ 2 = 0.01). Further im-
provement occurs when the membrane is implemented in the
FBMRA. It is interesting to note that the membrane alone is
not sufficient to shift the thermodynamic equilibrium to high
ethane conversions. It seems that under the prevailing oper-
ating conditions the effect of the auxiliary reaction is more
pronounced on the displacement of the thermodynamic equi-
librium than the membrane. This could be due to the limited
membrane area used in this study. Therefore, in the following
analyses, we focused on the fixed bed membrane reactor with
auxiliary reaction (FBMRA).
Fig. 8 shows how the exit ethane conversion varies as a
function of the bed composition for different temperatures.
It seems the influence of the temperature is pronounced. It
can be seen that the exit ethane conversion passes through a
maximum with the increase of catalyst 2 (θ 2 ) in the bed. The
occurrence of the maximum could be due to the interaction
of the equilibrium, hydrogen permeation driving force and
composition of the catalyst bed. The maxima at temperatures
of 750 and 800 K are presented in a form of plateau. The
results show that, it is possible to achieve complete conversion
of ethane at relatively low temperature as shown by the profile
at T = 750 K. This is an important result because it is known
that high temperatures affect the useful life of the membrane
and the catalyst.
Fig. 9 shows the conversion profiles along the length of the
reactor at T = 800 K for different catalyst bed compositions.
1194 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196
Fig. 8. Exit ethane conversion vs. catalyst 2 concentration for various tem-
peratures.
It can be seen that the complete conversion of ethane is
attained at different reactor lengths depending on the bed
compositions. Also, the exit ethane conversion increases and
decreases as the amount of catalyst 2 increases, i.e. there ex-
ist optimal conditions under which the complete conversion
of ethane is achievable. In order to investigate the optimum
conditions, we define an effective reactor length (Leff ) as the
reactor length that gives 99.8% conversion of ethane. This
criterion is fair enough to find the optimum conditions.
Fig. 10 shows the dimensionless effective reactor length
versus the bed composition for different temperatures. It is
Fig. 9. Ethane conversion along the reactor for different concentrations of
catalyst 2.
Fig. 10. Effect of temperature on the dimensionless effective reactor
length.
shown that the profile at all temperatures present a minimum
value at which the effective reactor length is optimal. The
minima steadily decrease as the temperature increases and
the effective length regions shrink with the decrease of tem-
perature. It appears that the temperature has a pronounced
effect on the effective reactor length and the position of the
optimal conditions.
The effect of the tube side pressure on the dimen-
sionless effective reactor length is shown in Fig. 11. The
increase of the pressure has two opposing effects on the
thermodynamic equilibrium. The increase of the pressure
Fig. 11. Effect of tube side pressure on the dimensionless effective reactor
length.
 M.E.E. Abashar, A.A. Al-Rabiah / Chemical Engineering and Processing 44 (2005) 1188–1196 1195

has positive effect on the hydrogen permeation driving force k2 reaction rate constant of hydrogenation reaction
and the hydrogenation reaction of benzene due to the de- (kg mol/kg s)
crease in number of moles and negative effect on the de- KB adsorption constant for benzene (Pa−1 )
hydrogenation reaction of ethane due to the increase of the K1 equilibrium constant of dehydrogenation reaction
number of moles. The increase of the pressure has an over- (Pa)
all positive effect on the optimal value of the dimension- L dimensionless reactor length
less effective reactor length and its position. This result is L0 reactor length (m)
opposite to the negative result of increasing the pressure Pi partial pressure of component i (Pa)
in the fixed bed membrane reactor (FBMR) as shown in Pt pressure in tube side (Pa)
Fig. 6. Ps pressure of sweep gas (Pa)
QH2 hydrogen permeation rate (kg mol/s)
Q0 permeability constant (kg mol m/m2 s Pa0.5 )
7. Conclusions r1 radial dimension in catalyst bed (m)
r2 radial dimension in ceramic support (m)
The results presented in this paper show that the inte- R universal gas constant (kJ/kg mol K)
grated catalytic membrane reactor with catalyst pattern strat- R1 inner tube radius (m)
egy is an attractive application for production of ethylene R2 outer radius of composite tube (m)
and cyclohexane. The introduction of the concept of dual- R1 rate of dehydrogenation reaction (kg mol/kg s)
functionality of the well-mixed catalyst bed has appreciable R2 rate of hydrogenation reaction (kg mol/kg s)
improvement of the reactor performance in terms of high con- T temperature (K)
versions, low temperatures and reduced total reactor lengths. ul axial velocity (m2 /s)
The combined effect of the membrane and reaction cou- yi mole fraction of component i
pling is believed to enhance the ethane conversion to com-
pletion at relatively low temperatures (720–800 K). These Greeks symbols
are important results, since it is known that excessive tem- γ ij stiochiometric coefficient of component i in the jth
peratures have destructive effects on the catalysts, the me- reaction
chanical and chemical stability of the membranes and the δ membrane thickness (m)
reactors. ε1 porosity of catalyst bed
Effective operating regions with optimal conditions are ε2 porosity of ceramic support
observed and an effective reactor length criterion is used to θj volume fraction of catalyst j
evaluate the performance of the reactor. In light of the results ρj density of catalyst j (kg/m3 )
presented the optimal effective reactor length is favored by
high temperature and tube side pressure. It seems that the po- Subscript
tential application of coupling ethane and benzene reactions f feed
in fixed bed membrane reactors is promising. Future research
should focus on different catalyst layer configurations and Superscripts
rigorous optimization studies. Further improvements are still c ceramic support
to be expected both in scientific knowledge and industrial s shell side
practice in ethylene industry. t tube side

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