Journal of Energy Chemistry 22(2013)726–732

Kinetic study of propane dehydrogenation and catalyst

deactivation over Pt-Sn/Al2O3 catalyst
Farnaz Tahriri Zangeneha∗ , Abbas Taeba , Khodayar Gholivanda, Saeed Sahebdelfarb
a. Department of Chemistry, Science and Research Branch, Islamic Azad University, Tehran, Iran;
b. Catalyst Research Group, Petrochemical Research and Technology Company, National Petrochemical Company, P. O. Box 14358 84711, Tehran, Iran
[ Manuscript received February 3, 2013; revised May 14, 2013 ]

Abstract
The kinetics of propane dehydrogenation and catalyst deactivation over Pt-Sn/Al2 O3 catalyst were studied. Performance test runs were carried
out in a fixed-bed integral reactor. Using a power-law rate expression for the surface reaction kinetics and independent law for deactivation
kinetics, the experimental data were analyzed both by integral and a novel differential method of analysis and the results were compared. To
avoid fluctuation of time-derivatives of conversion required for differential analysis, the conversion-time data were first fitted with appropriate
functions. While the time-zero and rate constant of reaction were largely insensitive to the function employed, the rate constant of deactivation
was much more sensitive to the function form. The advantage of the proposed differential method, however, is that the integration of the rate
expression is not necessary which otherwise could be complicated or impossible. It was also found that the reaction is not limited by external
and internal mass transfer limitations, implying that the employed kinetics could be considered as intrinsic ones.
Key words
propane dehydrogenation; Pt-Sn/Al2O3 ; kinetics; catalyst deactivation; mass transfer limitation

1. Introduction ysis reactions [6−8]. The acidity of the support is suppressed

Propylene is the building block for many important petro-
chemicals such as polypropylene and acrylonitrile. Catalytic
dehydrogenation of propane to propylene is much sought
as a complementary supply to the conventional processes
such as steam cracking or FCC units to satisfy the growing
demand [1]:
C3 H8 ⇐⇒ C3 H6 + H2 ∆H298
0
= 124 kJ/mol
The reaction is reversible, endothermic and accompanied
by volume expansion. Therefore, higher temperatures and
lower pressures shift it to completion. Higher temperatures,
on the other hand, promote side reactions, coke formation and
catalyst deactivation.
Commercially, chromia and platinum-based catalysts are
used for dehydrogenation of light alkanes [2−5]. Platinum ex-
hibits a good activity in the dehydrogenation of paraffins, but
the olefin yield is poor because the platinum particles catalyze
C–C bond rupture as well. Platinum-based catalysts are often
promoted with tin and alkali metals (mostly potassium) to in-
crease the selectivity and lifetime. Incorporation of tin into
platinum-based catalysts has a positive effect on the selectiv-
ity toward dehydrogenation, at the expense of the hydrogenol-
∗
Corresponding author. Tel: +98-21-44580519; Fax: +98-21-44580501; E-mail: tahriri zangeneh@yahoo.com
by the addition of an alkaline metal [7,8].
Due to thermodynamic limitations, dehydrogenation of
light alkanes is operated at temperatures around 600 ◦ C to
achieve reasonable commercial yields. Under these condi-
tions, catalyst deactivation is rapid and frequent catalyst re-
generation is necessary [9]. Some technologies operate under
vacuum or in the presence of diluents such as steam or even
hydrogen to lower alkane partial pressure and to shift the re-
(1) action to olefin formation. The utilization of a coke remov-
ing diluent inhibits coke formation and catalyst deactivation
as well [10,11]. The UOP Oleflex process [12], for example,
employs Pt-Sn/Al2 O3 catalyst in 3 to 4 adiabatic moving-bed
reactors in series. Hydrogen is used as the diluent and the cat-
alyst is continuously regenerated by coke burning followed by
Pt re-dispersion.
Consequently, despite the simple chemistry, dehydro-
genation processes are very complicated. The availability of
reliable kinetic models for the reactions and catalyst deacti-
vation are, therefore, essential. First-order power-law kinetic
models for the main reaction [13−15] and independent decay
laws for catalyst deactivation [14,16] have been commonly
proposed. Other kinetics can be approximated by power-law
kinetics at high temperatures and low pressures [17], which
are typical of dehydrogenation reactions.

Copyright©2013, Dalian Institute of Chemical Physics, Chinese Academy of Sciences. All rights reserved.
 Journal of Energy Chemistry Vol. 22 No. 5 2013 727

In this work, the kinetics of propane dehydrogenation forward and reverse reactions [17]. As a consequence, the
and that of catalyst deactivation over Pt-Sn/Al2 O3 catalyst are following rate expression can be used for the rate of dehydro-
studied. The kinetics associated with propane dehydrogena- genation reaction [13−15]:
tion and catalyst deactivation are then examined and analyzed. 
CB · CH2

′
A novel method based on differential analysis of integral re- −rA = k1 · a CA − (2)
Keq
actor data is introduced and the results are also compared with
those of the integral method of analysis. The influence of ex- where, A and B represent the paraffin and olefin, respectively.
–rA′ is the rate of reaction per unit mass of catalyst, k is the
ternal and internal mass transfer limitations was also studied. 1
rate constant, Keq is the equilibrium constant and C is the con-
2. Experimental centration. The time-dependent catalyst activity, a, is defined
as [17]:
−rA′ (t) −rA′
Commercial Pt-Sn/Al2 O3 dehydrogenation catalyst was a(t) = = (3)
′
− rA (t = 0) ′
− rA0
provided by a European company, the characteristics of which
are reported elsewhere [18]. The catalyst performance tests For an independent first-order decay law:
were carried out in a fixed-bed quartz reactor (ID = 15 mm)
using a mixture of propane and hydrogen as the feed un- a(t) = exp(−kd · t) (4)
der atmospheric pressure. For each run, 1.5 g of the cata-
where, kd is the deactivation rate constant. Equation 2 can be
lyst was loaded. The reactor effluent was analyzed for C1 –
written in terms of propane conversion, XA , as:
C3 hydrocarbons by an online gas chromatograph (RGA Agi-
lent 6890N), with TCD and FID detectors using 3 ft HayeSep
′ k1 · a · CA0 (XAe − XA )(α + βXA )
Q 80/100, 8 ft HayeSep N 80/100 and 10 ft molecular sieve −rA = =
13×45/60 columns for permanent gases, 4 foot HayeSep (1 + εA · XA )2
(5)
Q+10 ft molecular sieve 13×45/60 columns for hydrogen and
a 50 m, 0.53 mm, 15 µm alumina/Na2 SO4 PLOT column for a(t) · k1 (T ) · f (CA0 , XA , XAe )
hydrocarbons. Test conditions were specified according to
in which
typical conditions of commercial plants, as given in Table 1.
A long-term test run was also conducted to study deactivation 1
α= (6)
kinetics. XAe
Table 1. Levels of operating conditions for performance tests (1 + εA XAe − XAe ) + εA XAe ΘH
β= (7)
Temperature H2 /CH ratio Space velocity XAe (ΘH + XAe )
Factor
(◦ C) (mol/mol) (h−1 )
where, ΘH is hydrogen/propane molar ratio in the feed, XAe
Lower level 580 0.6 1.8
Medium level 600 0.8 2.0 is the equilibrium conversion and εA is the volume expansion
Higher level 620 1.0 2.2 factor. The function f stands for the functionality of the rate
on reacting species concentrations. From a propane mole bal-
ance on the axial element within the reactor bed:
3. Kinetic modeling and analysis dXA dW
′ = (8)
−rA FA0
Dehydrogenation reaction is practiced at relatively high where, FA0 is the molar flow rate of propane in the feed and
temperatures and low pressures due to thermodynamic and W is the mass of catalyst. Integration of Equation 8, us-
kinetic considerations. Under such conditions, the site cov- ing Equation 5 for the rate, following algebraic manipulations
erage is low and power-law expressions could be used for the gives [14]:

(β − εA · α)2 β(1 + εA · XAe )2

   
′ −1 α + β · XA,out
ln(k1 τ ) − kd · t = ln β ln −
β(α + β · XAe ) α (α + β · XAe )
   (9)
XAe − XA,out
ln − ε2A · XA,out = g(XA,out )
XAe

where, XA,out is propane conversion at reactor effluent; τ ′ , Alternatively, upon integrating Equation 8, one obtains
the ratio of catalyst weight per volumetric feed flow rate, is
W dXA
Z
the weight-time. Equation 9 provides a basis for integral anal- = ′ (10)
FA0 −rA
ysis of reactor data, a plot of which (right-hand-side, RHS,
versus time-on-stream) should result in a straight line with the For a catalyst deactivating with time-on-stream, combin-
intercept giving k1 and the slope giving kd . ing Equations 4 and 10 results in:
728 Farnaz Tahriri Zangeneh et al./ Journal of Energy Chemistry Vol. 22 No. 5 2013

partial pressure of hydrogen would not only decrease the ther-

modynamic driving force of the reaction, but also kinetically
W k1 τ ′ dXA
Z
k1 exp(−kd · t) = exp(−kd · t) = reduce the rate of dehydrogenation reaction due to the com-
FA0 CA0 f (XA ) petition of hydrogen with propane for platinum active sites
(11) [4]. Furthermore, higher hydrogen concentrations in the feed
Differentiating with respect to time, using the chain rule, enhance the hydrogenolysis side reaction, as reflected by the
and taking logarithm of both sides yields: decreasing of propylene selectivity with increasing hydrogen
concentration. However, too low levels of H2 /HC ratios are
k1 τ ′
   
dXA,out 1 not desirable due to accelerating catalyst deactivation by coke
ln kd − kd · t = ln −
CA0 dt f (XA,out ) formation.
(12)
A plot of Equation 12 should result in straight lines with
the intercept and slope giving rate constants of the main reac-
tion and deactivation, respectively. The interested reader can
verify Equation 12 by differentiating the integral form (Equa-
tion 9) with respect to time.
Implicit in the above derivations is isothermal reactor as-
sumption, which is well approximated in lab-scale microre-
actors, and also pseudo-steady state assumption for a reac-
tor operating with a deactivating catalyst, which is the case in
sufficiently slow catalyst deactivation.
The occurrence of mass transfer limitation depends on the
relative rates of transport around and within catalyst particles
to that of surface kinetics, as reflected in the Mears (CM ) and
Weisz-Prater (CWP ) numbers for external and internal limita-
tions, respectively [17]:
Figure 1. Influence of temperature on equilibrium propane conversion (dash
′ ·ρ ·d ·n
− rA line) and catalyst performance
b p
CM = (13)
2kc · CAb

′ · ρ · d2
− rA c p
CWP = (14)
4De · CAs
where, ρb is the bulk density of catalyst bed, ρb = (1–φb )ρc ,
(φb : bed porosity), ρc is density of catalyst pellet, dp is cata-
lyst particle diameter, n is reaction order, kc is mass transfer
coefficient, De is effective diffusivity and CAb and CAs are the
bulk and surface concentrations, respectively. Internal mass
transfer effects can be characterized by Thiele modulus and
effectiveness factor as well [17].

4. Results and discussion

4.1. Performance test results
Figure 1 shows the effect of operating temperature on
propane conversion, as well as propylene selectivity and yield.
The propane conversion is close to and parallel to the equilib-
rium conversion. As the reaction is highly endothermic, an in-
crease in temperature enhances the conversion of propane due
to both kinetic and thermodynamic factors. However, higher
temperatures could promote noncatalytic gas-phase reactions
which enhance side reactions such as propane cracking and
coke formation.
Figure 2 illustrates the influence of H2 /HC molar ratio in
the feed on the performance of the catalyst. The propane con-
version decreased with increasing H2 /HC ratio. An increase in
Figure 2. Influence of H2 /HC on equilibrium propane conversion (dash line)
and catalyst performance
Figure 3 shows the effect of space velocity on propane
conversion and propylene selectivity. The conversion of
propane remains rather unaffected, which could be attributed
to thermodynamic limitation of the reaction. Therefore, these
data, though representative of commercial plants, are of lit-
tle application for kinetic study as the kinetics is masked by
equilibrium. However, upon catalyst deactivation, the reaction
shifts from a thermodynamic controlled regime to a kinetic
controlled one. The rate of conversion decline by deactivation
can be used to find the deactivation rate constant as outlined
in the previous section.
 Journal of Energy Chemistry Vol. 22 No. 5 2013 729

Figures 1 to 3 also illustrate that the catalyst exhibits high
propylene selectivities (> 85%) over the rather wide range of
operating conditions tested. As a consequence, the rate and
conversion of propane to propylene are well approximated by
those of overall reactions.
4.2. Modeling results
Figures 5(a) and 5(b) show plots of Equations 9 and
12, respectively, both of which are reasonably straight lines,
confirming the applicability of the kinetic expressions em-
ployed for the main reaction and catalyst decay. Figure 5(b)
is constructed based on the exponential function fit deriva-
tives. The fluctuations of the original experimental data are
smoothened as derivative values were evaluated indirectly
from the fitting function.

Figure 3. Influence of space velocity on equilibrium propane conversion

(dash line) and catalyst performance

Figure 4 shows the effect of time-on-stream on propane

conversion. The observed rapid catalyst deactivation mainly
caused by coke deposition is typical for dehydrogenation cat-
alysts. The fluctuation of data point can cause large er-
rors in numerical time-derivative calculations required for
differential analysis. This can be reduced using an appropri-
ate fitting function. When differentiation of successive exper-
imental data point is under consideration, to avoid fluctuation
effects, they are first fitted and then the differentials are
evaluated from the fitted curve [19]. For the case of the
present experimental data, an exponential function showed
satisfactory fit (Figure 4). The resulting time-zero conversion
of 0.496 is close to the equilibrium conversion of propane,
implying a thermodynamically controlled regime on the
fresh catalyst.

Figure 5. Plots of (a) Eq. 9 and (b) Eq. 12 for long-term test run (T = 620 ◦ C,
H2 /HC = 0.6 and WHSV = 2 h−1 )

Figure 6 shows the parity plots for propane conversion

Figure 4. Long-term propane conversion and the exponential function fit of
the data for numerical differentiation (solid line) (T = 620 ◦ C, H2 /HC = 0.6,
WHSV = 2 h−1 )
using the kinetic parameters obtained by integral method and
those by differential method using the exponential fit. As
it can be seen, the difference between experimental results
and model estimations is predominantly within 20%, which
confirms the accuracy of the results. The results of the integral
method are closer to experimental data, especially for longer
times on-stream. The differential method results approach to
those of integral method as the time approaches zero which
can be explained by thermodynamic limitation of the system
on fresh catalyst as noted above. However, differential method
results in under-estimation of conversion after long times on-
stream which is attributed to the larger resulting deactivation
rate constant (Table 2). Nevertheless, even the elementary ex-
730 Farnaz Tahriri Zangeneh et al./ Journal of Energy Chemistry Vol. 22 No. 5 2013

ponential function gives fair results which can be improved by
using more appropriate fitting functions.
time-zero conversion and rate constant of the reaction are not
very sensitive to the fitting function as can be seen in Table 2.
The magnitude of these parameters is largely governed by
early time-on-stream conversion levels which depend on the
goodness of the fitting of conversion data points. In contrast,
the rate constant of deactivation is much more strongly de-
pendent on the fitting function type. This could be explained
by the fact that this parameter depends on the long-term trend
of time-derivatives of conversion data with time, which might
not be necessarily well fitted by the derivative of a particular
function optimized for fitting data points themselves. In the
case of the aforementioned system, it could be concluded that
a fitting function with low upward curvature should give the
best results.
The pseudo-steady assumption could be verified by not-
ing that deactivation rate was sufficiently slow to allow near-
steady state conditions at any instant of time. The character-
istic time for catalyst stability (say, 1/0.017 h−1 ≈ 2×105 s),
for example, was much longer than the residence time within
the reactor (∼1 s).

4.3. Mass transfer limitations

The observed order and the magnitude of parameters of

the kinetic models could be influenced by mass transfer lim-
itation effects [17,19]. Consequently, analysis of mass trans-
fer limitations is critical in kinetic modeling of heterogonous
catalyst systems. Mass transfer analyses are commonly per-
formed prior to kinetic study, especially when intrinsic kinet-
ics is sought, by changing parameters affecting mass transfer
such as pellet size and flow rate, and observing the effect on
Figure 6. Correlation between experimental data and model predictions for conversion [20]. Alternatively, it can be performed after pre-
propane conversion (a) integral analysis and (b) differential analysis (expo- liminary kinetic study by an iterative procedure using quanti-
nential fit)
tative criteria. The later approach allows more precise analysis
For the sake of comparison, other fitting functions such in the light of estimated kinetic data.
as linear and quadratic equations were also evaluated. Table 2 Equation 2 can be re-written as
shows the kinetic parameters obtained from integral analysis  
and differential analysis using different fitting functions. The ′ CB · CH2
−rA = k1 · a · CA 1 − = k1 · a · CA (1 − η)
tabulated values are reasonably close and consistent. One sur- Keq · CA
prisingly observes that the linear fit gave the best and closest (15)
results to the integral method, although it is obviously not a where, η is the approach to equilibrium. As the reactor prod-
fair fit for long-term conversion versus time data. ucts are close to equilibrium in the case of fresh catalyst (that
is, η ∼1), the highest reaction rate, and mass transfer limi-
Table 2. Kinetic parameters evaluated by different methods at 620 ◦ C
tation, is to be found in the reactor inlet where η is close
Time-zero Rate constant, Decay
Analysis to zero and the rate expression reduces to a first-order irre-
conversion k1 constant,
method
(%) (m3 /(kg·h)) kd (h−1 )
versible one.
Integral 45.8 7.3 0.017 The transport parameters can be estimated from the ap-
Differential (linear) 46.1 7.6 0.015 propriate correlations in the literature under the operating con-
Differential (quadratic) 49.6 7.8 0.028 ditions [21]. The diffusion coefficient, for example, can be
Differential (exponential) 49.6 7.7 0.026 obtained from the kinetic theory and Lennard-Jones expres-
sions for intermolecular forces [22]. The external mass trans-
It is noteworthy that the accuracy of the differential fer coefficient can be estimated by appropriate correlation for
method results depends on the fitting function, which should packed-beds [21]:
fit both propane conversion and its time-derivative with time- Sh = 0.91ΨRe0.49Sc1/3 (16)
on-stream accurately. The fitting functions, however, are often
designed to serve only for the former. As a consequence, the where Ψ is the shape factor ( = 0.91 for spherical particles),
 Journal of Energy Chemistry Vol. 22 No. 5 2013 731

and Sh, Re and Sc are dimensionless Sherwood, Reynolds and propane dehydrogenation and it was found that a power law-
Schmidt numbers, respectively, defined as: based rate expression for the surface reaction kinetics and in-
u · dp dependent deactivation kinetics result in fair fits both for this
Re = (17) method and conventional integral method of analysis. Both
6ν · Ψ(1 − φb)
methods were used to obtain the rate constants. The advantage
kc · dp of the method introduced in this work is that it by pass the in-
Sh = (18)
DAF tegration of the rate expression for integral method of analysis
which could be very time-consuming or impossible for com-
in which u is the superficial velocity, ν kinematic viscosity
and DAF is the diffusivity of propane in feed mixture. The plex rate expressions. Similar advantage is offered compared
latter was approximated by molar-average of diffusivity of to the alternative non-linear regression method which needs
propane in propane and that of propane in hydrogen, which parameter estimation and solving the model equations.
is reasonable for a gaseous mixture. Table 3 shows typical The analysis of mass transfer effects showed that the reac-
data employed to calculate the mass transfer parameters un- tion is not limited by external and internal transfer limitations,
der reactor inlet conditions of Figure 4. and consequently the kinetic models and their corresponding
parameters could be considered as intrinsic ones.
Table 3. Data used for estimation of mass transfer parameters
Items Data Items Data
dp 1.8 mm −r ′ A0 0.017 mol/(kg·s) Nomenclature
φb 0.42 DAF∗ 1.4 cm2 /s A alkane, propane
Re 0.11 De 0.14 cm2 /s
Sc 0.47 kc 0.017 m/s
a catalyst activity
CA0 8.5 mol/m3 B olefin, propylene
* mole-average diffusivity of propane in propane-hydrogen feed Ci concentration of species i (mol/m3 )
mixture D diffusion coefficient (m2 /s)
dp pellet diameter (m)
Table 4 shows the calculated parameters. From the tab- F feed rate (mol/h or mol/s)
ulated results one obtains CM <0.15 and CWP <<1, showing k1 reaction rate constant (m3 /(kg·h))
that both external and internal mass transfer limitations were kc mass transfer coefficient (m/s)
not significant. Because of low external mass transfer lim- kd rate constant for deactivation of catalyst (h−1 )
itation, CAs is nearly the same as CAb , and the latter was
Keq concentration equilibrium constant (mol/m3 )
used for calculating CWP by Equation 14. Alternatively, the
Re Reynolds number (dimensionless)
Thiele modulus and effectiveness factor were 0.12 and 0.992,
respectively, confirming that internal diffusion limitation was r ′ A rate of disappearance of A per mass of catalyst (mol/(kg·h))
virtually absent. Similar results have been obtained by other Sc Schmidt number (dimensionless)
workers under different operating conditions [23]. As a con- Sh Sherwood number (dimensionless)
sequence, the kinetic model and associated kinetic parameters T temperature (K)
obtained in this work could be considered as intrinsic ones. u superficial velocity (m/s)
W mass of catalyst in the reactor (kg)
Table 4. Calculated parameters based on conditions of
Figure 4 for fresh catalyst X conversion of key component (A)
Parameter Effectiveness factor CM CWP
Value 0.992 0.068 0.13 Subscripts
0 entering or initial condition
b bed or bulk
Higher temperatures can induce mass transfer limitations
c catalyst
due to rapid increase of surface reaction rates. However,
620 ◦ C used in this study is close to the upper temperature p pellet
limit of Pt-Sn/Al2 O3 type catalysts applicability. Higher tem-
peratures increase side reactions, accelerate Pt sintering and Greek symbols
support phase-transformation, and therefore, are unlikely to α parameter defined by Eq. 6
be encountered in practice. β parameter defined by Eq. 7
ε expansion factor, fraction change in volume resulting from
5. Conclusions change in total number of moles
ΘH ratio of hydrogen in H2 /CH mixture
The performance data of an integral reactor can be used ν kinematic viscosity (m2 /s)
to study the kinetics and to obtain the kinetic parameters us- ρc density of catalyst pellet (kg/m3 of pellet)
ing differential method of analysis. This method was used for ρb bulk density of catalyst (kg/m3 of reactor bed)
732 Farnaz Tahriri Zangeneh et al./ Journal of Energy Chemistry Vol. 22 No. 5 2013
τ ′ a capacity factor (catalyst weight per volumetric feed
flow rate) ((kg·h)/m3)
φ void fraction (porosity)
Acknowledgements
Saeed Sahebdelfar would like to thank Professor Farhad Kho-
rasheh, Department of Chemical and Petroleum Engineering, Sharif
University of Technology, for fruitful discussion and invaluable com-
ments.
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