Journal of Membrane Science 253 (2005) 233–242

Propane dehydrogenation using catalytic membrane

Vadim S. Bobrov ∗ , Nikoliy G. Digurov, Valery V. Skudin
Department of Chemical Technology of Carbon Materials, Mendeleev University of Chemical Technology of Russia (MUCTR),
Miusskaya Sq. 9, Moscow, 125047 Russian Federation, Russia

Received 15 April 2004; received in revised form 21 October 2004; accepted 10 November 2004
Available online 7 March 2005

Abstract

The present work is focused on the process of propane dehydrogenation using gas separation inorganic membranes with molybdenum
(Mo) selective layer obtained by chemical vapor deposition (CVD) method. Such membranes could be a valuable substitution for the present
noble metal-coated membranes for dehydrogenation process. Being catalytically active and possessing gas separation properties at the same
time. Mo-coated membranes could prevent from using granulated catalyst bed in membrane reactor. The maximum selectivity to propylene
for Mo-ceramic membranes (Mo coated on ceramic support) was 63% (T = 853 K, conversion to propane 17%). The maximum selectivity to
propylene for Mo–carbon membranes (Mo coated on carbon support) was 84% (T = 853 K, conversion to propane 28%).
© 2005 Elsevier B.V. All rights reserved.

Keywords: Catalytic dehydrogenation; Membrane reactors; Catalytic membranes; Gas separation; Inorganic membranes

1. Introduction a monomer for polypropylene [2]. In these reactions, the ther-

Nowadays olefins are widespread as the raw materials for
a variety of chemical industries. This is the reason for never-
ending interest towards intensification methods of olefins pro-
duction during the last 60 years [1]. Commercially simple
thermal naphtha cracking is not profitable for light olefins
production for the present time because of the low yield to
olefins on the one hand and growing exhaust of natural re-
sources, which requires more thorough naphtha refinery, on
the other hand. That is why among all the present methods cat-
alytic dehydrogenation plays the leading role. Steam crackers
(SC) and fluidized catalytic crackers (FCC) are the predom-
inant source for olefins industrial production [1]. The thing
is that light alkanes dehydrogenation is thermodynamically
limited process, which leads to the well-known problems:
low yield to olefins at low temperatures and coke formation
with following catalyst deactivation at high temperatures. The
dehydrogenation of propane is a typical example of such cat-
alytic reactions, but it is the key step for producing propylene,
∗ Corresponding author. Tel.: +8 10 095 978 8839;
fax: +8 10 095 978 8786.
E-mail address: mendeleevv@yahoo.com (V.S. Bobrov).
modynamic equilibrium conversions are less than 20% even
at 500 ◦ C; therefore, the high temperatures and low pressures
that produce the acceptable olefin yields often create techni-
cal complications and require expensive process equipment
or specialized catalysts.
In fact high temperature catalytic membrane reactors
(CMRs), which combine reaction and separation in a single
unit operation, may solve the yield problems of equilibrium-
limited reactions [2].
Only a few authors have reported on the problem of
propane dehydrogenation in membrane reactors since 1993.
The pioneering work in this field (except Bitter patent [6])
was made by Ziaka et al. [3,4], then a few works of Weyten
et al. [5] and Gobina and co-workers followed [7], and fi-
nally we can find Quicker et al. [8], a few Korean researches
[2] and Hou and Hughes work [9] devoted to propane de-
hydrogenation in membrane reactors. The thing is that only
palladium-coated membranes with Pt-catalysts (of course us-
ing different alloys) were mainly used in these works. Prob-
ably its impossible to avoid exploiting expensive Pd and Pt
metals in light alkanes dehydrogenation reactions at all, but
its necessary to drive forward to more ‘cheap’ catalytically
active metals which will diminish the cost of the membrane

0376-7388/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.memsci.2004.11.037
234 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242
module and make the process less capital intensive. No re-
ports on propane dehydrogenation in a catalytic membrane
reactor were found. Nearly all the papers are devoted to the
packed-bed or fluidized-bed membrane reactors (PBMR or
FBMR according to Marcano and Tsotsis classification [10]).
The catalyst bed increases membrane reactor overall dimen-
sions, increases the resistance of the tubeside or shellside
area and can probably increase the final cost of the pro-
cess. From this point of view membrane with catalytically
active selective layer prevents from using another granulated
catalyst.
In this work, we tried to make the step in another approach
to the membrane catalysis application for alkanes dehydro-
genation reactions.
Propane dehydrogenation in a catalytic membrane reactor
using composite Mo-based membranes is reported in this ar-
ticle. Such membranes could be a valuable substitution for the
present noble metal-coated membranes for dehydrogenation
process. Being catalytically active and possessing gas sep-
aration properties at the same time, Mo-coated membranes
could prevent from using granulated catalyst bed in mem-
brane reactor.
2. Experimental
2.1. Materials
Porous composite membranes with molybdenum se-
lective layer were used in the experiments (Mo-ceramic
Table 1
Mo-selective layer porous properties
Support Specific Mo-layer weight Surface area
(g Mo/g support) (m2 /g)
Ceramic 0.0371 1.30
Carbon 0.0192 85
Fig. 1. SEM-micrographs: (a) surface ×600 and (b) cross-section ×3000 of porous Mo-ceramic membrane.
and Mo–carbon membranes). Ceramic ␣-Al2 O3 microfil-
tration tubes with 7 mm in outer diameter and 7.5 cm in
length and carbon microfiltration tubes with 10 mm in
outer diameter and 7.5 cm in length were used as supports
for membranes. Mo-ceramic and Mo–carbon membranes
were obtained using chemical vapor deposition method
(CVD). This method can be successfully used for the lay-
ers deposition consisted of different compounds, even on
rough or porous surface substrates. Morphology analysis
and direct selective layer thickness measurements were
carried out by scanning electron microscopy (SEM) see
also [11]. Selective layer porous properties for a com-
posite membranes used in the experiments are shown in
Table 1.
Figs. 1 and 2 show the surface and cross-section of ob-
tained membranes. All the inevitable caverns on the support
were covered with Mo layer (see Fig. 2).
The following gases and mixtures were taken for the exper-
iments: hydrogen (99.999 vol.%), propane (99.000 vol.%),
methane (99.950 vol.%), methane–hydrogen mixture (60%
of methane) and propane–hydrogen mixture (80% of
propane).
2.2. Unit for propane conversion experiments
The schematic representation of experimental rig is shown
in Fig. 3. It consists of a feed gas delivery system, a high-
temperature membrane reactor and a gas chromatograph.
Reactor temperature was controlled by two thermocouples
placed in preheating and reaction chambers. Permeate and
Volume porosity Average pore size Thickness
(%) (nm) (␮m)
4 10 5–7
75 12 5–8
 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242 235

Fig. 2. SEM-micrographs: (a) surface ×600 and (b) cross-section ×3000 of porous Mo–carbon membrane.

Fig. 3. Experimental for membrane catalysis. (1) membrane reactor; (2) electric heater; (3 and 4) coolers; (5) gas chromatograph; (6 and 12) needle valves
for fine tuning; (7–11 and 13) throttle valves; (I) feed gas or gas mixture line; (II) permeate line; (III) retentate line. Control devices: FI, flow meters; TI,
thermocouples; PI, pressure indicators.

retentate analysis was made separately using chromato- 2.3. Determination of catalytic activity of Mo-coated
graph 5. membranes and Mo-coated catalyst
Gas permeation and separation properties measurements
for said Mo-coated membranes (see Table 2) were obtained All the catalytic measurements were detected only
and discussed in [12,13]. when the permanent reaction products concentrations were
achieved under isothermal conditions. Values used in the
present work:
Table 2
Gas separation properties for Mo-ceramic membranes [13] propane propane propane
qf yf − q r yr − q p yp
Gas index Kn CH4 –H2 permselectivity Xpropane = propane (1)
Knudsen diffusion Ideal Binary gas mixture qf yf
(theoretical) (T = 650 ◦ C) (T = 650 ◦ C)
propylene propylene
He 67 2.8 6.1 4.9 qr yr + q p yp
CH4 32 Spropylene = propylene
(2)
H2 130 q f yf Xpropane
236 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242

Table 3 tions, the following reactions can proceed in reactor module:

Propane conversion mass balance (T = 853 K)
IN OUT C3 H 8 ↔ C3 H 6 + H 2 (R1)
Reagents C (mol/s) H (mol/s) Products C (mol/s) H (mol/s)
C3 H8 → CH4 + C2 H4 (R2)
C 3 H8 0.000302 0.000403 C 3 H8 0.000261 0.000348
H2 0.000023 C 3 H6 0.000026 0.000026 C2 H4 + H2 ↔ C2 H6 (R3)
C2 H 6 0.000004 0.000006 C 2 H6 0.000005 0.000007
C2 H 4 0.000009 0.000009 Reactions (R1)–(R3) are possible both in gas phase volume
CH4 0.000005 0.000010
(thermal conversion) and on the surface of composite Mo
H2 0.000034
membrane (catalytic conversion). Decreasing the tempera-
Total 0.000306 0.000432 0.000306 0.000434 ture will lead to reaction (R1) domination over reactions (R2)
and (R3).
Table 4 Catalytic properties of the support were evaluated using
Example of products analysis in CMR (T = 853 K, feed flow rate 170 ml/min) the standard method. The ground membrane sample (coated
Flow index Product mol% on ceramic or carbon support) with 0.8 mm average diameter
Permeate (flow rate = 146 ml/min) H2 29.1 and total mass 1.6 g was loaded in reactor. Then the sample
CH4 1.6 was heated up to 800 K with 2 K/min rate in the presence of
C2 H4 2.4 methane–hydrogen mixture flow (flow rate 90 ml/min). After
C2 H6 1.4
that the temperature was increased up to 900 K and ground
C3 H6 5.2
C3 H8 60.3 membrane sample was kept for 60 min in the presence of
100 hydrogen flow. This operation was made to obtain the Mo-
Retentate (flow rate = 43 ml/min) H2 22.2
carbides as reported in [14].
CH4 4.1 Gas phase propane conversion temperature dependence
C2 H4 3.6 (gas-phase conversion) was studied in hollow reactor.
C2 H6 1.8 All experiments in catalytic membrane reactor were car-
C3 H6 6.5 ried out at total feed shellside pressure 1.8 atm, while the tube-
C3 H8 61.8
100
side pressure was maintained at 1 atm. Propane–hydrogen
mixture (with 20 vol.% of hydrogen) was used as a feed for
propane dehydrogenation experimental modeling. The res-
Vr idence time (3 s) and dehydrogenation temperature interval
τ= (3)
qf (880–960 K) were taking from [3].
Results of propane conversion achieved in CMR (conver-
λi sion to propane X, selectivity to propylene S) were compared
α0i,j = (4)
λj to reactor with ground membrane bed (conventional reactor).

Before X and S determination the mass balance was fixed.
Mi Example of such balance is shown in Table 3.
αKn
i,j = (5)
Mj

P2 3. Results and discussion

Pr =
P1
yp,i [(1 − yr,i ) − Pr (1 − yp,i )]
αi,j = (7)
(1 − yp,i )[yr − Pr yp ]
qp
θ=
qr
Gas products were analyzed using chromatograph Tzvet-
500 with thermo conductive detector. Carrier gas—helium;
adsorbent—Porapak-Q (USA). Components were detected
by coincidence of their retention time in chromatograph and
retention time data components. Table 4 shows example of
the conversion products identification. Carbon and acetylene
were not detected.
Judging our product analysis, mass balance (one example
for T = 853 K is presented on Table 3), thermodynamic data
analysis for the possible reactions under the working condi-
(6)
In membrane reactor reaction chamber two processes can
take place simultaneously: chemical reaction and separation
of products on the membrane. One can assume that the closer
the catalyst is situated to the membrane, the more effective
(8) will be chemical reaction processes, taken place on the cata-
lyst, as the products mass transfer through the catalyst bed is
eliminated. In this way the case when the catalyst is fixed just
on membrane will be more effective. The possible modes of
this catalytic membrane can be illustrated by Fig. 4. One can
see that carrying out both processes on the single surface can
be achieved only when the catalyst plays selective layer role
as well.
Recently we have realized that not only Mo, but the sup-
port origin can take part in light alkanes conversion process.
Though the role of each above-mentioned constituent parts
of composite membrane has not been practically determined.
 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242 237

Fig. 4. Catalytic membrane modes: (a) support + selective layer + catalyst layer; (b) catalyst layer + support + selective layer; (c) support-catalyst + selective
layer; (d) support + selective layer-catalyst; (e) support + membrane impregnated with catalyst.

Needless to say that gas phase hydrocarbon conversion (with-
out catalyst) can bring significant contribution to the total
conversion process under high temperatures.
3.1. The influence of support and Mo selective layer
material on conversion to propane and selectivity to
propylene
As we have obtained Mo-ceramic membranes for the first
time we had to prove the catalytic activity of Mo selective
layer, deposited on the support.
Fig. 5 shows that conversion to propane increases
with temperature rise. Maximum propane conversion was
achieved in the experiments with Mo-ceramic catalyst
(ground membrane) in comparison to propane conversion
with the presence of ground ceramic support.
Conversion on the ceramic support practically can be de-
fined as the sum of two processes—gas phase conversion in
the hollow reactor volume and on the ground support sur-
face. Conversion on Mo-ceramic catalyst will be a result of
gas phase, ceramic surface and Mo surface conversions. Thus,
Mo layer contribution to the propane conversion can be cal-
culated by subtracting X or S parameters for the conversion

Fig. 5. Conversion to propane vs. temperature. Reactor residence time 3 s; feed rate 170 ml/min; tubeside pressure 1.8 bar; shellside pressure atmospheric.
238 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242

Fig. 6. Selectivity to propylene vs. temperature. Reactor residence time 3 s; feed rate 170 ml/min; tubeside pressure 1.8 bar; shellside pressure atmospheric.

on the ceramic support from X of S obtained when using Mo-
ceramic catalyst (as both experiments were carried out under
the same conditions: temperature, pressure, granules size and
loading mass, etc.)
Fig. 6 shows that obtained selectivity to propylene on Mo-
ceramic catalyst exceeds selectivity obtained on the ceramic
support.
Fig. 7 shows that selectivity to propylene for Mo
layer remains practically constant in the temperature in-
terval 880–920 K with the following decrease under the
higher temperatures. Conversion is steadily increasing in
studied temperature interval. Data comparison depicted in
Figs. 6 and 7 indicates that coating ceramic support with
Mo layer increase conversion to propane up to 30–50% and
selectivity to propylene to 30–70% depending on process
temperature.
Above-mentioned data can be the evidence of Mo catalytic
activity, coated on the ceramic support.
3.2. Propane dehydrogenation in CMR
Different works pay much attention to permselectivity. It
is supposed that the greater is permselectivity the more ef-
fective will be membrane in catalytic process. The principle
of widespread method of permselectiviy increase is to de-
crease an average pore size in the selective layer. But the
other side of this method can be subsequent decreasing of
membrane permeability (under the same pressure) or tube-
side resistance increase (under the same permeate flow rate).
It is worth mentioning that none of researchers gave any com-
ments on this parameter selection in membrane catalysis pro-
cess. Judging the main deductions from the thermodynamic
analysis (for example, the necessity of carrying out light alka-
nes dehydrogenation under low pressures) one can predict
the importance of using membranes with high permeability.
That is why before the Mo membrane efficiency reveal, us-
ing different temperature regimes, we defined the flow ratio,

Fig. 7. Propane conversion and propylene selectivity of Mo layer (deposited on ceramic support) vs. temperature; specific Mo weight 0.0371 g Mo/g support.
Reactor residence time 3 s; feed rate 170 ml/min; tubeside pressure 1.8 bar; shellside pressure atmospheric.
 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242 239

Fig. 8. The effect of flow ratio on catalytic activity of Mo-ceramic membrane; T = 913 K.

under which the S and X could achieve the maximum val-
ues.
Fig. 8 shows that X and S achieve the maximum values
when flow ratio equals approximately 0.3. This figure, ob-
tained for chemical reaction and membrane separation cou-
pling process, coincides with the optimum flow ratio taken
for membrane separation (0.2–0.3). It is worth mentioning
that during the study of separation properties of Mo-ceramic
membranes using the binary mixture methane–hydrogen the
maximum permselectivity occurred only when the flow ratio
equaled 0.28. This fact also coincides with abovementioned
data.
When the flow ratio equaled 0 (the permeate line was
closed) the gas mainly contacted with Mo layer; selectiv-
ity and conversion were very closed to S, X calculated for Mo
layer (see Fig. 7). When the flow ratio equaled 1 these values
were close to S, X for Mo-ceramic catalyst (see Figs. 5 and 6).
It is difficult to predict membrane effect on the reaction se-
lectivity and conversion using only gas permselectivity. That
is why we additionally used Figs. 9 and 10 to demonstrate
Mo-membrane reactor advantage in comparison to conven-
tional reactor with Mo catalyst.
Figs. 9 and 10 give the comparison of S and X for Mo-
ceramic catalyst and Mo-ceramic CMR. The CMR S and X
values exceeds there of for conventional reactor. The reason
is the effect of shifting the equilibrium for propane dehydro-
genatiom reaction by selective hydrogen permeance through
the membrane (removing from the reaction volume). Fig. 11
shows that hydrogen concentration in permeate (including
feed hydrogen concentration) increased more than 1.3 times.
Propylene (having larger molecular mass) almost was not
separating (for Mo-ceramic membrane and T = 853 K). When
raising the temperature to 913 K, propylene concentration in
retentate increases 1.75 times in comparison to permeate.
These membrane separation properties can be explained us-
ing the reaction products permselectivity.
Fig. 12 shows Mo-ceramic membrane separation activity
towards propane dehydrogenation products. The calculated
Knudsen permselectivity is given for compare. Conversion
products permselectivity and Knudsen permseiectivity are
calculated using formulas (6) and (7).
It is worth mentioning that propane conversion prod-
ucts permselectivity for methane–hydrogen pare (4.43)
practically coincided with binary mixture permselectivity

Fig. 9. Conversion to propane for Mo-ceramic CMR and packed-bed reactor. Reactor residence time 3 s; feed rate 170 ml/min; tubeside pressure 1.8 bar;
shellside pressure atmospheric.
240 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242

Fig. 10. Propylene selectivity vs. temperature for packed-bed reactor and Mo-ceramic CMR. Reactor residence time 3 s; feed rate 170 ml/min; tubeside pressure
1.8 bar; shellside pressure atmospheric.

Fig. 11. Hydrogen and propylene concentrations in permeate and retentate for Mo-ceramic CMR (left) and Mo–carbon CMR (right)—hydrogen feed concen-
tration is included; T = 853 K. Reactor residence time 3 s; feed rate 170 ml/min; tubeside pressure 1.8 bar; shellside pressure atmospheric.

Fig. 12. Mo-ceramic membrane permselectivity for different propane dehydrogenation products, T = 913 K.
 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242
Fig. 13. Conversion to propane and selectivity to propylene vs. temperature for Mo-ceramic and Mo–carbon CMR. Reactor residence time 3 s; feed rate
170 ml/min; tubeside pressure 1.8 bar; shellside pressure atmospheric.
(4.90) (methane–hydrogen) calculated earlier (see Table 2).
Conversion products permselectivity for methane–hydrogen
(4.43) exceeds calculated Knudsen permselectivity
(2.83). For other couples (hydrogen/ethane–ethylen,
hydrogen/propane–propylene fractions) conversion products
permselectivities were lower, than calculated Knudsen
permselectivity. One can suppose that the reaction products
transport (except hydrogen) is the result of coupled Knudsen
and surface diffusion. In this way the lower conversion
products permselectivities can be explained by the sur-
face diffusion influence prevail, which contributes to the
component flow increase along the pore walls. This fact
finally decreases permselectivity. The surface diffusion
influence prevails for the components with large molecular
masses, lowering their permselectivity as a result. Judging
Fig. 12 permselectivities for propane conversion products
(hydrogen/ethane–ethylen and hydrogen/propane–propylene
fractions) are lower than calculated permselectivities for Kn
diffusion for above-mentioned fractions.
3.3. Mo–carbon membranes
Ceramic support, being catalytically active for propane de-
hydrogenation process (as it was discussed earlier), possesses
acid catalytic centers (Lewis acids), which can promote the
hydrocarbon cracking process producing by-products and
lowering selectivity to propylene. This was the main rea-
son for changing the ceramic to carbon support (which does
not posses such centers). Fig. 6 shows that the selectivity
for carbon support exceeded ceramic in the entire studied
temperature interval. Porous properties for Mo layer, coated
on carbon support were much better than for Mo layer on
ceramic support (porosity 75%, surface area 85 m2 /g, see
Table 1). The SEM study of Mo–carbon membrane before
and after high temperature treatment (T = 953 K, propane de-
241
hydrogenation) showed no significant changes in the selec-
tive layer structure, while dramatic changes (caverns, cracks,
etc.) for Mo-ceramic membrane were found. One can sup-
pose that Mo layer coated on carbon support will be more
stable. Fig. 11 shows that separation values to hydrogen and
propylene for Mo–carbon membrane have obvious improve-
ment over Mo-ceramic membranes.
These three advantages of Mo–carbon membranes (ab-
sence of acid centers, selective layer thermal stability, porous
properties advantages) must result in integral process values
X and S. Fig. 13 shows comparison of S and X for Mo-ceramic
and Mo–carbon CMR. Obtained selectivity and conversion
for Mo–carbon membrane exceed Mo-ceramic thereof val-
ues.
Thus, one can see how just the change of support can
influence the membrane catalysis efficiency.
4. Conclusions
The importance of obtained results is not only in ab-
solute values, which characterize dehydrogenation process
in membrane reactor. The thing is that to influence the
chemical reaction effectively, it is not necessary to achieve
the perfect membrane permselectivity (using noble met-
als like Pd). Probably giving catalytic activity to the se-
lective layer of membrane, achieving its maximum values
(conversion and yields to the main products, high thermal
stability, operating temperature decrease, etc.) will be the
main trend in catalytic membranes technology development
in the nearest future. Up-to-date development of methods,
which can improve membrane separation properties pro-
vide its optimization in a way to obtain high productivity of
composition catalytic membranes and membrane reactors.
The optimum combination of gas and catalytic properties
242 V.S. Bobrov et al. / Journal of Membrane Science 253 (2005) 233–242

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