Rev Chem Eng 2019; 35(3): 377–392

Majid Taghizadeh* and Fatemeh Aghili

Recent advances in membrane reactors

for hydrogen production by steam reforming
of ethanol as a renewable resource
https://doi.org/10.1515/revce-2017-0083 energy used is supplied from fossil fuels as the depleting
Received September 5, 2017; accepted January 24, 2018; previously conventional energy sources that produce large amounts
­published online March 27, 2018
of gas emissions such as NOx, SOx, and CO2 (James et al.
2011, Gonçalves et  al. 2017). Producing new and renew-
Abstract: During the last decade, hydrogen has attracted
able energy sources that can replace existing fossil fuels
lots of interest due to its potential as an energy carrier.
is one of the most significant concerns of many works
Ethanol is one of the renewable resources that can be
(Mehri and Taghizadeh 2012, Dehkordi et al. 2016). In this
considered as a sustainable candidate for hydrogen gen-
context, hydrogen has been identified as a powerful alter-
eration. In this regard, producing hydrogen from etha-
native energy source and an environmentally clean energy
nol steam reforming (ESR) would be an environmentally
carrier, which can be used as a transportation fuel and
friendly process. Commonly, ESR is performed in packed
safely converted to thermal and electrical energy with a
bed reactors; however, this process needs several stages
higher efficiency (El Hawa et al. 2016, Song et al. 2016). As
for hydrogen separation with desired purity. Recently,
hydrogen is an energy carrier but not an energy resource,
the concept of a membrane reactor, an attractive device
some methods are implemented to produce it (Angeli et al.
integrating catalytic reactions and separation processes
2014). All over the world, about half of the feedstocks are
in a single unit, has allowed obtaining a smaller reactor
natural gases that produce hydrogen through the steam
volume, higher conversion degrees, and higher hydro-
reforming process as a high-performance and cost-effec-
gen yield in comparison to conventional reactors. This
tive method (Haryanto et al. 2005, Authayanun et al. 2015,
paper deals with recent advances in ESR in terms of cata-
Sharma et al. 2017). Natural gas is a fossil fuel that emits
lyst utilization and the fundamental of membranes. The
a considerable volume of CO2 annually (Sohn and Ozkan
main part of this paper discusses the performance of dif-
2016). Hence, by an increase in power demand and envi-
ferent membrane reactor configurations, mainly packed
ronmental concerns, it is necessary to develop a sustain-
bed membrane reactors, fluidized bed membrane reac-
able feedstock for hydrogen production to have a closed
tors, and micro-membrane reactors. In addition, a short
carbon loop cycle (Authayanun et al. 2015, Roldán 2015).
overview is given about the impact of ESR via different
Among the candidates for hydrogen production,
catalysts such as noble metal, non-noble metal, and bi-
ethanol has gained great attention as it offers some
metallic catalysts.
upsides compared to fossil fuels (Trane-Restrup et al. 2014,
Keywords: ethanol steam reforming; fluidized bed; mem- Dehkordi et al. 2016, Jin et al. 2016). For instance, ethanol
brane reactor; micro-reactor; packed bed. is a renewable source; i.e. it can be produced from envi-
ronmental processes and be transformed to eco-friendly
material. Further, it has a high H/C ratio, lower toxicity
1 Introduction than methanol, and easy transportation (Contreras et al.
2016, Dehkordi et al. 2016, Jin et al. 2016).
The rapid increase in the world population and indus- Hydrogen can be produced from ethanol by steam
trialization has led to a significant rise in energy con- reforming (Morales and Segarra 2015, Gonçalves et  al.
sumption demands (Sohn and Ozkan 2016). Most of the 2017), partial oxidation (Koehle and Mhadeshwar 2012,
Pirez et al. 2016), and oxidative steam reforming (Pereira
et al. 2010, Baruah et al. 2017, Espitia-Sibaja et al. 2017).
*Corresponding author: Majid Taghizadeh, Chemical Engineering In addition, the production of hydrogen through the elec-
Department, Babol Noshirvani University of Technology, P. O. Box
trolysis of ethanol can be considered in terms of energy
484, Babol 4714871167, Iran, e-mail: m_taghizadehfr@yahoo.com
Fatemeh Aghili: Chemical Engineering Department, Babol
efficiency and environmental friendliness if bio-ethanol
Noshirvani University of Technology, P. O. Box 484, Babol is used as the fuel (Yan et al. 2008, Ehteshami et al. 2016).
4714871167, Iran Furthermore, photocatalytic hydrogen production over

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378      M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors
semiconductor photocatalysts is a promising technology
in which solar energy is harnessed for hydrogen genera-
tion from renewable sources such as ethanol. However,
hydrogen production by means of this method remains
economically and technically challenging (Nadeem
et al. 2012, Jovic et al. 2013a,b). Among these methods,
ethanol steam reforming (ESR) using an appropriate cat-
alyst is the most economical way of renewable hydrogen
production (Silveira et al. 2009). The main advantages of
the ESR method are its non-use of oxygen supply, a high
H2/CO ratio for hydrogen production, and the possibil-
ity for regulation of the process condition by preventing
coking (Dehkordi et al. 2016, Sohn and Ozkan 2016). ESR
is represented by the following general stoichiometric
reaction:
C2H5OH + 3H2O → 6H2 + 2CO2 (∆H = 174 kJ mol −1 at 25°C). (1)

The enthalpy change value of 174  kJ mol−1 is consid-
ered when the reactants are in the gas phase (Palma et al.
2014, Mulewa et al. 2017, Sidhu et al. 2017), while the value
of 347.4 kJ mol−1 for enthalpy change at 25°C is applied to
the liquid phase (Haryanto et al. 2005, Carrero et al. 2010).
Many efforts have been made to develop catalysts for
ESR in different reactor configurations (Hedayati et  al.
2016, Pirez et  al. 2016, Sharma et  al. 2017) to overcome
by-product formation and catalytic deactivation, which
are the major barriers to the ESR method. The catalysts
are based on noble or non-noble metals as well as the
combinations of both, which are supported on alumina
or other different materials (Gallucci et al. 2010, Muñoz
et al. 2013, Roldán 2015). Noble metal catalysts such as
Pd, Pt, Rh, Au, and Ru exhibit high catalytic activity
and stability. Among these metals, Rh is considered as
the catalyst with the best activity (Palma et al. 2014, da
Silva et al. 2015, Roldán 2015, Miyamoto et al. 2016, Sohn
and Ozkan 2016, Touri and Taghizadeh 2016, Sharma
et  al. 2017). Although inexpensive catalysts such as Ni,
Cu, and Co as non-noble metals are more attractive for
commercial applications (Sharifi Pajaie and Taghizadeh
2012, Trane-Restrup et  al. 2014, Miyamoto et  al. 2016,
Pirez et  al. 2016, Sharma et  al. 2017), non-noble cata-
lysts become deactivated due to carbonaceous deposits
formed as the by-product of the ESR reaction (Jeong and
Lee 2008, Carrero et al. 2010).
ESR is an endothermic process that requires high tem-
peratures with effective heat management, which also
favors high intrinsic reaction rates (Sohn and Ozkan 2016,
Sidhu et al. 2017). Packed bed reactors have so far been the
most common reactors for producing hydrogen through
steam. To improve the heat and mass transfer rates as the
vital factors for the effective performance of the reactor,
smaller catalyst particles are demanded. However, using
such particles is associated with higher pressure drops.
Thus, fluidized bed systems and micro-channel reactors
have been developed to reach a trade-off between these
two opposing requirements (Sidhu et  al. 2017). On the
other hand, the major disadvantages of the conventional
ethanol reforming reactors include equilibrium restric-
tions and a hydrogen-rich gas stream that contains carbon
oxides and other by-products as well as unreacted rea-
gents (Meng and Tsuru 2015). In this connection, hydro-
gen production processes have traditionally been carried
out in reaction units in series with one or more separa-
tion units because of incomplete reactions induced by
thermodynamic and/or kinetic obstacles. Nowadays,
many researchers have demonstrated that an integrated
system in which the reaction and the separation are oper-
ated simultaneously (rather than sequentially) is able to
accelerate the reactions both kinetically and thermody-
namically (Basile 2008, Iulianelli et  al. 2016b). Among
different techniques, membrane technology seems appro-
priate for the production and purification of H2 consider-
ing its attractive possibility of process miniaturization,
continuous operation, and energy saving (Basile 2008,
Di Marcoberardino et al. 2017). Therefore, the idea of the
simultaneous production and removal of hydrogen, which
is realized by using a membrane reactor, has received a
great deal of attention in the past few decades because it
would allow for a significant reduction in capital costs.
The application of the membrane reactor creates the pos-
sibility to overcome the thermodynamic limitations of
the reforming reactions and to perform these reactions at
milder operating conditions (Gallucci et al. 2013, Anzelmo
et al. 2017). Also, when a reactor is integrated with a mem-
brane, removing hydrogen through a membrane results
in a shift in the equilibrium reaction toward the product
of interest; however, it is normally limited by the mem-
brane’s surface area, hydrogen partial pressure driving
force, membrane’s permeance, reactor design, and reac-
tion kinetics (Gallucci et  al. 2013, El Hawa et  al. 2016,
Jiwanuruk et al. 2016).
Recently, some authors have focused on the catalyst
of ethanol reforming (Contreras et al. 2014, Baruah et al.
2015, Sohn and Ozkan 2016, Sharma et al. 2017). To the
best of our knowledge, however, no review paper has
discussed various membrane reactor configurations for
hydrogen production using ESR. Hence, in this review,
we will first provide an overview of the recent attempts
concerning the catalysts of ESR. Subsequently, new
concepts in membrane and membrane reactor designs
are highlighted, and the applications of these con-
figurations for hydrogen production from ethanol are
discussed.
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 M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors      379

2 E
 SR process and kinetic 2.1 Catalysts
mechanism description Catalysts play a crucial role in completing ethanol con-
version and maximizing the hydrogen yield (Hou et  al.
Steam reforming is recognized as the first step of the
2015). As mentioned in Section 1, the catalysts can be
H2 production process. In this stage, C2H5OH is fed into
divided into noble-metal-based, non-noble-metal based,
a reformer or reactor, where the liquid is broken down
and bi-metallic catalysts (Baruah et  al. 2015). Besides
into carbonaceous species that would react with steam
the active metals, the support by the effect on the cata-
over the catalyst to produce a mixture of H2 and other
lyst activity can accelerate ethanol transformation (Hou
compounds, such as methane, carbon monoxide, acetic
et  al. 2015). During the last decade, various catalytic
acid, acetaldehyde, ethylene, acetone, diethyl-ether,
systems, such as single active metals, a combination of
and coke (Haryanto et  al. 2005, Mulewa et  al. 2017).
several active metals, single supports, and mixed oxide
Many reactions occur in the process of steam reform-
supports, have been tested (Bshish et  al. 2011). Noble
ing of ethanol (Table  1). Three significant reactions,
metal catalysts are well known because of their high con-
namely ESR, water gas shift (WGS) reaction, and ethanol
version efficiency and high H2 selectivity.
decomposition, are the principal reactions in the kinetic
However, the high cost of noble metals is a major lim-
schemes and design purposes (George and Suresh 2016,
iting factor in their use for hydrogen production via steam
Sidhu et al. 2017). Among these reactions, ESR and WGS
reforming. As a matter of fact, few works have been con-
are thermodynamically and kinetically favored at high
ducted to develop novel catalysts with composite phases
temperatures (Sidhu et  al. 2017). However, high tem-
and nanostructures (Baruah et al. 2015). In addition, it is
perature is favorable for the formation of CO as a result
seen that the direction of recent literature is shifted toward
of the reverse WGS reaction. Thus, converting CO–CO2,
the development of non-noble metal catalysts as a succes-
as an exothermic reaction, occurs appreciably at low
sor to the conventional noble metal catalysts (Zhang et al.
temperatures.
2014, Baruah et al. 2015).
Kinetically undesired by-products may be related
Table 2 shows the basic results of selected studies on
to the operation conditions (complex reaction mecha-
ESR using noble metal catalysts. As can be seen, among
nisms) and the type of catalysts. Nevertheless, catalysts
the noble metals on various supports, Rh-based catalysts
designed to maximize the hydrogen production should
usually present superior performance in terms of activity,
efficiently break the C–C bond, as well as eliminate the
selectivity, and stability in the ESR reactions, as Rh has
side reactions (Chen et  al. 2009, Guil-López et  al. 2011,
the highest capacity to break the C–C bond and the high
Muñoz et al. 2013).
hydrogen yield (Ferencz et al. 2014, Zhang et al. 2014, Hou
et al. 2015).
Table 1: Possible reaction pathways of ESR (Palma et al. 2014, Non-noble metals, especially Ni and Co, have been
Trane-Restrup et al. 2014, Roldán 2015, Sohn and Ozkan 2016, widely investigated for ethanol reforming essentially
Sharma et al. 2017, Sidhu et al. 2017). because of their lower cost as compared to noble metals.
Table 3 summarizes the main non-noble catalysts used in
Name of reaction Formula of reaction ESR. Despite the challenges in using Ni-based catalysts
Ethanol decomposition CH3CH2OH→CH4 + CO + H2 (e.g. rapid deactivation due to heavy coke formation and
Incomplete reforming CH3CH2OH + H2O→2CO + 4H2 Ni particle sintering), Ni-based catalysts have been widely
(insufficient steam) investigated in ESR on different supports considering their
Dehydrogenation CH3CH2OH→CH3CHO + H2
high activity and relatively low cost. Also, several strat-
Dehydration CH3CH2OH→C2H4 + H2O
Coke formation C2H4→coke
egies such as modifying the support or Ni species have
Diethyl ether formation 2CH3CH2OH→(C2H5)2O + H2O been developed to improve the catalyst stability (Bshish
Methanation CO + 3H2→CH4 + H2O et  al. 2011, Hou et  al. 2015, Viviente et  al. 2017). Cobalt
Methane decomposition CH4→C + 2H2 has also been investigated because of its aptitude to C–C
Methane steam reforming CH4 + 2H2O→4H2 + CO2 bond rupture (Soykal et al. 2012, Kumar et al. 2017). In this
Acetaldehyde decomposition CH3CHO→CH4 + CO
regard, several studies have shown significantly different
Acetaldehyde steam reforming CH3CHO + 3H2O→2CO2 + 5H2
Acetone formation 2CH3CHO→CH3COCH3 + CO + H2 properties of the catalysts in bimetallic systems than either
Acetic acid formation C2H5OH + H2O→CH3COOH + 2H2 of the parent metals. As a result, bimetallic systems can be
Water-gas shift, reverse water- CO + H2O ↔ CO2 + H2 promising approaches to promote the synergistic effect of
gas shift two active species (He et al. 2017, Shejale and Yadav 2017).
Boudouard reaction 2CO→CO2 + C
Table 4 reports the performances of the bi-metallic systems.
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 Table 2: Noble catalysts of ESR.

Catalyst Support Preparation method Temperature Ethanol Hydrogen Comment Reference

conversion selectivity

Rh La2O3-SiO2 Incipient wetness 773 K 100% 68% A slight difference in the hydrogen permeated/feed ethanol (da Silva et al. 2015)
Rh CeO2 impregnation 773 K 100% 70% ratio was observed at higher sweep gas flow rates being higher
Incipient wetness for Rh supported on CeO2 in comparison with the Rh/La2O3-SiO2
impregnation catalyst
Rh La2O3-Al2O3-CeO2 Wet impregnation 723 K 80% 65% The modification of γ-Al2O3 with La2O3 and CeO2 improves the (Osorio-Vargas et al.
stability of the catalyst by decreasing the carbon deposition rate 2015)
Rh Al2O3 Over Rh/alumina, the steam reforming reaction was maintained (Bilal and Jackson
and the carbon deposition showed no trend relative to the 2017)
impurities
Pt ZrO2 773 K 75% 55% H2 and CO formation was favored over Pt/CeO2 and Pt/CeZrO2 (de Lima et al. 2008)
Pt CeO2 773 K 100% 58% catalysts, whereas Pt/ZrO2 catalyst exhibited the highest
Pt CeZrO2 773 K 65% 65% production of acetaldehyde and ethene
Pt HBS Pt/HBS not only exhibited excellent catalytic performance but (Zheng et al. 2016)
also maintained the catalytic reaction for >28 h without losing
its activity
Pt Al2O3 The Pt/alumina catalyst was rapidly poisoned when propanal, (Bilal and Jackson
propylamine, and acetone were present as impurities and the 2017)
high conversion related to ethanol decomposition resulted in
380      M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors

lower hydrogen yields and higher methane yields

Pd SBA-15 Impregnation 500°C 67.32% 87.42% A Pd/SBA-15 catalyst was prepared with 1% Pd (Matei et al. 2016)
Ir CeO2 Deposition- 800 K 100% The Ir/CeO2 catalyst demonstrated rather high stability for the (Cai et al. 2008)
precipitation reactions at 800 K with no apparent deactivation for 60 h on
stream
Ir Ce-La Impregnation 400°C 100% The Ce1xLaxO2ᵟ solid solution supported Ir catalysts (Han et al. 2017)
Ir TiO2 Impregnation 473 K 5.9% (after 10 h) (Nozawa et al. 2015)
Ru TiO2 Impregnation 473 K 30.1% (after 10 h) (Nozawa et al. 2015)

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 Table 3: Non-noble catalysts of ESR.

Catalyst Support Preparation method Temperature Ethanol Hydrogen Comment Reference

conversion selectivity

Ni TiO2 Sol-gel assisted 500°C 89% 55% The Ni/TiO2 nano-composite catalyst possessed excellent stability at (Mulewa et al. 2017)
impregnation the optimum temperature, over a 20-h reaction time
Ni CeO2 Solution combustion 400°C 98% 65% (Iulianelli et al. 2016a)
Ni SBA-15 Incipient wetness 550°C 100% 90% (He et al. 2017)
impregnation
Ni Al2O3-La2O3-CeO2 773 K 100% 73% The γ-Al2O3 modification with CeO2 and La2O3 improves catalyst (Osorio-Vargas et al.
stability by decreasing the carbon deposition rate 2016)
Ni CNT-SiO2 The Ni/CNTs-SiO2 catalyst was used for the ESR at different reaction (Prasongthum et al.
temperatures (300–550°C) 2017)
Ni CeO2-MgO 600°C 100% 75% Ni/CeO2-MgO catalysts were prepared on powder form and (Santander et al.
supported on stainless-steel plates 2017)
Ni SiO2 Incipient wetness 500°C ESR was studied in a fluidized bed reactor. Ni and Co were (Vicente et al. 2014)
Co Al2O3 impregnation deactivated at 500°C because of coke deposition
Co Carbon nano- 723 K 100% 96.5% This approach showed significant results in terms of hydrogen (Kumar et al. 2017)
filament generation and method of Co carbon nano-filament for further
utilization in different prospects
Co ZrO2 Impregnation 450°C 75% The reaction pathway of ESR on Co-ZrO2 was identified. It means (Sun et al. 2015)
ethanol was firstly dehydrogenated to form acetaldehyde, which
was then converted into acetone via a condensation/ketonization
process. Then, acetone was reformed to H2
Co Cordierite pieces Co-precipitation 873 K 65% ESR was carried out in a catalytic membrane reactor consisting of (Espinal et al. 2014)
(Al3Mg2AlSi5O18) cobalt hydrotalcite-derived catalyst doped with potassium

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M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors      381
 Table 4: Bi-metallic catalysts of ESR.

Catalyst Support Preparation method Temperature Ethanol Hydrogen Comment Reference

conversion selectivity

Ni-Pt CeO2-SiO2 Wet impregnation 520°C 95% The catalyst was tested under fluidization conditions and the results (Ruocco et al. 2016)
showed good attrition resistance of the catalyst and no chemical
interaction with the membrane material
Ni-Cu SiO2 600°C 99% 69.9% Mg-promoted catalysts achieved the highest hydrogen selectivity (Carrero et al. 2010)
Ni-Cu Mg-SiO2 600°C 100% 84.8% because of smaller Ni crystallite size, which is one of the main
Ni-Cu Ca-SiO2 600°C 99.9% 78.1% factors affecting catalytic activity. Ca-modified catalysts produced
the lowest carbon deposition
Ni-Ti-Al Impregnation 80% One-pot synthesis of nanostructured ternary oxides of Ni, Al, and Ti (Gonçalves et al. 2017)
was designed and performed via evaporation-induced self-assembly
Ni-Cu Al2O3-ZrO2 Single-step epoxide- 450°C 100% (Greluk et al. 2016)
driven sol-gel
Ni-Au SBA-15 550°C 100% 98% Au promoted the Ni/SBA-15 catalyst in terms of high activity and (He et al. 2017)
excellent long-term stability for ESR
La-Ni-Al Impregnation 873 K 100% 80% The least amount of coke was accumulated on meso-3LaNiAl catalyst (Ma et al. 2016a)
Cu-Ni-Co HTc Incipient wetness 98% 83.3% The presence of Cu, Ni, and Co assisted in the low formation of (Shejale and Yadav 2017)
impregnation intermediates and coke with higher concentration of hydrogen
(93.6 mol%)
Rh-Ni Al2O3 700°C 100% 70% (González-Gil et al. 2016)
Rh-Pt CeO2-SiO2 680°C 100% (Cifuentes et al. 2016)
Rh-Re TiO2 Impregnation 473 K 36.1 (after By adding Re to the Rh/TiO2 catalyst, the initial rates of H2, CH4, and (Nozawa et al. 2015)
10 h) CO2 formation increased 3–4 times
Rh-Fe Ca-Al2O3 On Rh-Fe/Ca-Al2O3, a good balance of the interaction between Rh, (Choong et al. 2017)
Fe2O3, and Ca-Al2O3 prevented strong metal support interaction
382      M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors

between Rh and Fe2O3 and thus promoted CO elimination via a WGS

reaction
Rh-Pd CeO2 Impregnation 772 K 100% 63% (Scott et al. 2008)
Rh-Pd CeO2 Incipient wetness 823 K CeO2 exerted a quenching effect on the metal nanoparticles and (Divins and Llorca 2016)
impregnation limited atomic rearrangement under the different atmospheres
tested for ESR
Pt-Co CeO2 Impregnation 540°C 100% The presence of oxygen in the feed decreased the deactivation (Greluk et al. 2016)
rate of the catalyst but also decreased the selectivity of ethanol
conversion to hydrogen
Cu-Co Mg-Al Impregnation 450°C 99% The Cu-Co/Mg-Al catalyst showed a much lower quantity of coke (Homsi et al. 2017)
deposition with no deactivation due to the basic character conferred
by the magnesium oxide phase

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Ir-Re TiO2 Impregnation 473 K 14.7 (after By adding Re to the Ir/TiO2 catalyst, the initial rates of H2, CH4, and (Nozawa et al. 2015)
10 h) CO2 formation increased 3–4 times
 M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors      383
Furthermore, there are other nano-catalysts such as
nano-diamonds (Xiaoyan et al. 2013), which were used by
Mironova et al. (2013) for ESR. Nano-diamonds are not only
used as catalyst supports, but they can also demonstrate
intrinsic catalytic activity. Hydrogen selectivity depends
highly on the treatment conditions of nano-diamonds.
In other words, change in catalytic activity is caused by
changes in the nature and quantity of functional groups
on its surface.
Incipient wetness impregnation is a common tech-
nique used for the synthesis of heterogeneous catalysts. In
this procedure, the active metal precursor is dissolved in
an organic or aqueous solution. Then, the metal-contain-
ing solution is added to a catalyst support containing the
same pore volume as that of the added solution. The solu-
tion is drawn into the pores by capillary action, and then
the catalyst is dried and calcined to drive off the volatile
components of the solution (Baruah et al. 2015).
3 Membrane
Membranes are basically barriers that allow the flow of
some components of a feed stream. The feed stream is sep-
arated by a membrane into permeate and retentate related
to the passed components and rejected components,
respectively (Gallucci et al. 2013). Regarding the types of
materials, hydrogen separation membranes may be classi-
fied into dense membranes, porous membranes, and pro-
ton-conducting membranes (Figure 1) (Gallucci et al. 2013,
Wang et al. 2014). Among these types of materials, dense
metal membranes (mainly palladium alloys) and dense
ceramic membrane (having a sufficient permeability
Figure 1: Types of hydrogen separation membranes.
toward hydrogen, an extremely high selectivity for hydro-
gen separation, and stability over a long period) meet the
industrial standards (Viviente et al. 2017). However, cost
remains a challenge that hinders their practical applica-
tion. Microporous membranes are promising materials
employed in membrane reactors because of their low-cost
manufacturing and the high-purity separation of hydro-
gen. As size exclusion is the main mechanism of hydrogen
separation in this membrane, selectivity is still limited
compared to dense inorganic membranes (Meng and Tsuru
2015) such as unsupported palladium membranes, which
are generally thick self-standing films (>50 µm thick) with
high mechanical stability (Conde et  al. 2017, Fernandez
et  al. 2017). The sharp increase in the costs involved in
membrane separation, on the one hand, and decreasing
of the permeation flux, on the other hand, are the main
drawbacks of increasing the membrane thickness. Thus,
in order to minimize the cost and maximize the membrane
performance, supported membrane consisting of a selec-
tive layer was proposed. Selecting the support is crucial to
prepare thin (<5 µm) and defect-free layers (Viviente et al.
2017). Porous ceramics with excellent chemical stability
and good surface quality are the most common substrate
materials used as support. To deposit the dense metal
layer on a support, the following techniques are applied:
physical vapor deposition (PVD), chemical vapor deposi-
tion, electroless plating (ELP), electro-plating, and diffu-
sion welding (Hatlevik et al. 2010, Shi et al. 2010, Peters
et al. 2011, Coulter et al. 2012).
Medrano et  al. (2016) presented a 4–5-μm metallic
supported Pd-Ag membrane synthesized by the aid of
the ELP method. They reported ideal perm-selectivities
and hydrogen permeances at 600°C above 200,000 and
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384      M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors
1.3 × 10−6 mol m−2 s−1 Pa−1, respectively. Medrano et al. (2016)
tested the prepared membrane configuration for >800 h.
After this period, however, some defects appeared on the
membrane surface, leading to an increase in the N2 perme-
ance with the consequence of a pronounced decrease in
the perm-selectivity.
A 5-μm Pd-Ru membrane supported on a porous yttria-
stabilized-zirconia/stainless steel substrate was used by El
Hawa et al. (2015) for H2 separation. It was also demonstrated
that the hydrogen permeance (0.0027 mol m−2 s−1 Pa−1) was
highly stable at 580°C, for 1000 h of testing.
Recently, Zhang and Way (2017) summarized the key
elements and details of Pd-Cu alloy membranes for H2 sep-
aration. These authors used the Pd-Cu phase diagram and
its implications for membrane permeability and stability,
and demonstrated that there are still challenges in apply-
ing Pd-Cu membranes in large-scale H2 separation, such
as membrane thermal and chemical stability, precise com-
position control, and the development of alloy annealing
procedures.
Supported composite Pd-Au alloy membranes on
alumina substrate were developed using the ELP tech-
nique by Shi et al. (2010), who obtained a hydrogen per-
meability of 1.3 × 10−8 mol m−2 s−1 Pa−0.5 at 400°C by using
5-μm Pd-Au alloy membranes. Also, Shi et  al. (2010)
reported that the H2/N2 ideal selectivity was around 1400
under 350 h of a test run.
4 Membrane reactor
The development of a membrane reactor is a good example
of process intensification in which hydrogen production
and hydrogen purity are simultaneously performed in a
unit. Hence, both the separation/purification and product
selectivity are improved. The application of membrane
Catalyst
Membrane
Feed (CH5OH, H2O)
Retentate (H2, CH4, H2O, CO2, CO)
Figure 2: Schematic of the PBMR configuration for ESR.
Reproduced from Ma et al. (2016b). With permission from Elsevier (copyright 2016).
reactors has been proposed for pure hydrogen production
using ethanol reforming (Deshmukh et al. 2007, Fernandez
et al. 2015, Silva and de Abreu 2016, Serra et al. 2017). As
mentioned in Section 1, there are different types of mem-
brane reactors that have been considered for hydrogen
production. Although most previous works have been per-
formed in packed bed membrane reactors (PBMRs) (Figure
2), there is a current growing interest in novel configura-
tions such as fluidized bed membrane reactors (FBMRs)
and micro-membrane reactors (MMRs). In the following,
these reactor configurations are discussed in detail.
4.1 PBMR
PBMR is the first and most studied configuration for
hydrogen production. Generally, for those reactions men-
tioned in Section 1, ESR, partial oxidation, etc. (Tosti et al.
2009) were carried out in a Pd-based tubular membrane
reactor. Indeed, the tubular membrane reactor is the most
commonly used packed bed configuration, using which
the catalyst may be packed either in the membrane tube
(Figure 3A) or on the shell side (Figure 3B), and the per-
meation stream is collected on the other side of the hydro-
gen-selective membrane. However, Tosti et  al. (2009)
employed a configuration (Figure 3A) in which the feed
stream (the water/ethanol mixture) was sent to the cata-
lyst bed via a stainless-steel tube placed inside the Pd-Ag
thin wall tube. They also added N2 as a sweep gas to keep
the N2 partial pressure on the permeation side of the mem-
brane reactor as low as possible for minimizing the mem-
brane area required for the hydrogen separation.
Domínguez et al. (2012) investigated ESR at a low tem-
perature in a PBMR using a reactor consisting of cobalt
talc [Co3(Si2O5)2(OH)2] supported over cordierite and a
Pd-Ag membrane. They set the configuration using the
catalyst bed packed around the membrane (Figure 3B). By
Permeate (H2)
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 M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors      385
Figure 3: Schematic of two configurations of the tubular membrane
reactor.
Catalyst in tube (A) and catalyst in shell (B).
evaluating the influence of temperature (598–673 K) and
pressure (5–15 bar) on PBMR performance, Domínguez
et  al. (2012) reported that at complete ethanol conver-
sion, the temperature had little effect on selectivity and
hydrogen separation. In contrast, a higher hydrogen flow
was obtained by increasing the pressure while the total
hydrogen production was decreased. Basile et  al. (2011)
investigated a porous stainless-steel-supported palla-
dium membrane reactor for ESR. The palladium layer
(around 25  mm) was deposited onto a stainless-steel
tubular macroporous support, which was prepared by an
ELP technique. A commercial Co/Al2O3 catalyst was used
as a packing material in the PBMR with ethanol conver-
sion varying from 85.0% to 100% in the reaction pressure
range of 3.0–8.0 bar. The optimum result was obtained
at 400°C and 8 bar in terms of hydrogen recovery (>50%)
and hydrogen purity (around 65%). However, by compar-
ing the membrane reactor performances after the reaction
tests, a decrease was observed in the permeation capac-
ity and the overall efficiency of the membrane reactor.
Energy-dispersive X-ray spectroscopy micro-analysis
detected iron, alumina, and cobalt in correspondence of
some deposits on the palladium layer of the membrane.
da Silva et  al. (2015) compared the performance of
the membrane reactor and the conventional packed bed
reactor for ESR by employing Rh/La2O3-SiO2 and Rh/CeO2
as the catalysts and the self-supported Pd-Ag as the mem-
brane in a double tubular membrane reactor. The research-
ers reported that ethanol conversion was kept at 100% in
the PBMR. In fact, the higher total hydrogen production in
the PBMR compared to the conventional reactor suggests
the overall ethanol reforming reaction without the forma-
tion of carbon deposits. The optimum results were related
to the H2 recovery (about 70%) and the hydrogen produced
for each mole of ethanol (close to 2.8) that were obtained
with an H2O/ethanol molar ratio equal to 10.
Espinal et al. (2014) carried out ESR in a PBMR con-
sisting of cobalt hydrotalcite (Co2Mg4Al2(OH)16)CO3 · 4H2O-
derived catalyst doped with potassium supported over
cordierite and a composite Pd-Ag selective membrane.
As these researchers used no sweep gas, they obtained
pure hydrogen at atmospheric pressure. They also inves-
tigated the effects of different temperatures, pressures,
and steam-to-carbon values. As explained above, a higher
hydrogen permeating flux was obtained at higher pres-
sures while at the same time, a decrease in the total pro-
duction of hydrogen was observed due to the Le Chatelier
principle and thermodynamics of the reaction. For this
reason, Espinal et al. (2014) reported that high hydrogen
recovery values of about 80% are achieved at 873 K and 16
bar. For the PBMR at 873 K, a remarkable value of 5.1 was
obtained for the hydrogen yield. Such a high yield might
be attributed to the enhancement of the shift effect in the
membrane reactor design as hydrogen permeated through
the membrane in the reaction zone. These authors also
evaluated different steam-to-carbon ratios from 1.8 up
to 3 and concluded that this ratio, the partial pressure of
hydrogen, and the driving force all decrease, leading to a
lower recovery of hydrogen. Yu et al. (2009) studied ESR in
PBMR with the WGS reaction on the permeate side.
Also, Rh/SiO2 and modified porous stainless steel were
used as the catalyst and the support, respectively. This
modified membrane with Knudsen permeation properties
shows remarkably high gas permeance. To induce the WGS
reaction inside the membrane, the Knudsen membrane
was impregnated with an aqueous solution of tetra-amine
platinum(II) hydroxide. According to their study, with a
sweeping gas flow rate of 70 ml min−1, water flow rate of
0.03 ml min−1, and temperature range of 300–600°C, the
PBMR showed an increase in ethanol conversion of 11.9%–
19% and extremely high hydrogen recovery of 78%–87%
compared to the conventional reactor. Moreover, the CO
concentration was reduced by 1% via the WGS reaction at
300–500°C. ESR was performed over a Pd-Rh/CeO2 cata-
lyst in a PBMR as a reformer unit for the production of fuel
cell grade pure hydrogen by Hedayati et al. (2016). They
employed four Pd-Ag membrane tubes inside the reactor
that was selective to hydrogen and fully covered using the
catalysts. The experiments were performed at 923 K, 6–10
bar, and fuel flow rates of 50–200 ml min−1 using a mixture
of ethanol and distilled water with a steam-to-carbon ratio
of 3. For the modeling task, the PBMR was divided into two
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386      M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors
sections, i.e. the catalytic zone and the permeation zone
(the membrane). Hedayati et al. (2016) used the Arrhenius
law as a static model for the catalytic zone to calculate the
total molar production rates of the ESR products inside the
reactor. They also simulated the pure hydrogen production
rate at steady-state conditions by means of Sieverts’ law
model. Finally, applying the ideal gas law assumptions at
isothermal conditions, Hedayati et al. (2016) successfully
simulated the dynamics of pure hydrogen production rate
(permeation zone) in the case of the operating fuel flow
rate or pressure set point adjustment.
4.2 FBMR
As discussed earlier, there are considerable efforts in the
application of the PBMRs, while these kinds of reactors
have been very limited because of technical and economic
drawbacks in commercial processes. A recent trend in
membrane reactor design has been guided in the direc-
tion of introducing membranes into fluidized beds. It
helps overcome the limitations often prevailing in PBMRs
because FBMR can successfully combine the perm-selec-
tive abilities of the membrane with excellent gas-solid
contact and heat transfer ability of fluidized beds (Desh-
mukh et al. 2007). Figure 4 shows a schematic of an FBMR
for the selective removal of hydrogen. Here, the membrane
area can be minimized because of the more flexible struc-
ture of the FBMR, and (virtual) isothermal operation (even
in the case of highly endothermic/exothermic reactions)
can be performed in an FBMR. As an FBMR can greatly
reduce pressure drops, catalyst particles can be much
smaller, meaning that the catalyst effectiveness factors
are greatly improved (Lu and Xie 2016, Ruocco et al. 2016).
Ruocco et  al. (2016) investigated one of the most
crucial issues in FBMR, i.e. catalyst-membrane interac-
tion. They synthesized the Pt-Ni/CeO2-SiO2 catalyst (with
a CeO2-SiO2 weight ratio of 20%) via the wet impregnation
method and demonstrated good attrition resistance of the
catalyst and no chemical interaction with the membrane
material. Through these experiments, they applied an
ultra-thin (~1-mm-thick) Pd-based membrane supported
on a ceramic porous tube prepared by a combination of
PVD magnetron sputtering and ELP techniques. They also
showed that the catalyst in the fluidized bed configuration
does not affect the permeation rate and the membrane
reaches the same H2 flux as in the case of an empty bed.
Ruocco et al. (2016) also illustrated a uniform temperature
profile along the bed. In other words, the membranes do
not experience any thermal stress in the axial direction.
Therefore, such a configuration will be used to design the
H2, CH4, H2O, CO2, CO
H2 H2
Membranes
Catalyst
Heat exchangers
Feed (CH5OH, H2O)
Figure 4: Schematic of an FBMR for selective removal of hydrogen.
Reproduced from Gallucci et al. (2013). With permission from
­Elsevier (copyright 2013).
pilot plant. Advanced micro-combined heat and power
based on an FBMR was studied recently by Viviente et al.
(2017). They designed a membrane reactor for an output of
3.2 Nm3 h−1 with a hydrogen recovery factor of 76.8%. The
reactor design consisted of 37 tubular membranes synthe-
sized by an ultra-thin film of Pd-Ag membrane supported
on ceramic porous tubes. The reactor was operated at a
partial feed load down to 40% of its nominal value, 12 bar,
500°C, and two different series of conditions: a water-to-
ethanol ratio (molar) of 3.6 and oxygen-to-ethanol ratio
of 0.43. Viviente et al. (2017) demonstrated an increase in
H2 separation at higher temperatures mostly due to the
fuel conversion with obtaining a higher permeation rate.
According to these results, a prototype with 37 longer
membranes was designed and built.
Gallucci et al. (2010) studied the production of ultra-
pure hydrogen via ethanol reforming in an FBMR (Figure 5).
The heat needed for the ESR was supplied by the burning
part of the hydrogen recovered, thereby integrating CO2
capture. The produced hydrogen was directly recovered
as an ultra-pure stream via perm-selective dead-end Pd-
based membranes. Indeed, the dead-end membrane con-
figuration allows connecting the membrane from one end
only to the reactor housing, thus minimizing the effects
of stresses due to both thermal and hydrogenation cycles
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 M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors      387
H2
CO + CO2 + H2O
N2 + O2
N2 + H2O
C2H5OH + H2O
Figure 5: Schematic of an FBMR for reforming of ethanol.
Reprinted from Gallucci et al. (2010). With permission from Elsevier
(copyright 2010).
and simplifying the manifold of the reactor. Gallucci et al.
(2010) also illustrated the effect of bubble-to-emulsion
phase mass transfer limitations on FBMR performance
using computational fluid dynamic (CFD) simulation. The
CFD simulation showed that a critical point in the FBMR
was the extent of bubble-to-emulsion phase mass transfer
limitations.
4.3 MMR
Micro-reactors are micro-structured reactors with sub-
millimeter dimensions that are gaining increasing atten-
tion for in situ and on-demand chemical processing in
the chemical industry. Micro-reactors have characteristic
properties, like a high surface-to-volume ratio, use of small
amounts of chemicals, high heat and mass transfer rates,
and short residence times that make them an interesting
research topic (Cai et  al. 2010, Uriz et  al. 2011, de-Souza
et  al. 2013, Touri and Taghizadeh 2016, Chen et  al. 2017,
Zhang et al. 2017). Hou et al. (2014) investigated ESR in a
micro-channel structured reactor and successfully depos-
ited a supported Ir/CeO2 catalyst. The stable performance
of this configuration during long time runs may be related
to the excellent adherence to the stainless-steel platelets.
Hou et al. (2014) demonstrated that the hydrogen selectiv-
ity in the micro-structured reactor was higher than that in
a conventional packed bed reactor due to the rapid heat
and mass transfer. Micro-reactors also have other advan-
tages, such as simpler process optimization, rapid design
implementation, easier scale-up through replication,
and better safety, which make them highly promising for
hydrogen production in micro-fuel cell application (Peela
and Kunzru 2011a,b, Peela et al. 2011, Rahman et al. 2011,
Uriz et al. 2011, Hou et al. 2014, Lu and Xie 2016).
A micro-structured membrane reactor combines the
advantages of both a membrane reactor and a micro-
reactor, exhibiting great potential for process intensifica-
tion and suitable for small-scale applications because of
a large membrane area in a small compact unit. Also, it
involves excellent advantages such as avoiding membrane
deformation and cracks, realizing greatly intensified pro-
duction processes, and allowing lower operating tem-
peratures due to the rapid heat and mass transfer rates.
Accordingly, hydrogen production via the MMR has been
an interesting subject in recent years (Rahman et al. 2012,
Boeltken et  al. 2014, García-García et  al. 2014, Vigneault
and Grace 2015, Lu and Xie 2016, Ebrahimi and Rahmani
2017). However, still, only few works on MMRs for hydro-
gen generation from ethanol have been done.
A microporous silicon membrane with parallel chan-
nels, which is known as an excellent support for catalysts
in microreactors, was used by Llorca et al. (2008) for the
production of hydrogen through ESR at moderate tem-
peratures. Silicon channels were coated with a thin layer
of Co3O4-ZnO. Also, a high selectivity ( >73 vol.% H2) was
reported at 773 K at a contact time of <5 ms per channel.
ESR was carried out in a hollow fiber micro-reactor by
Rahman et al. (2011). They proposed an asymmetric yttria-
stabilized zirconia (YSZ) hollow fiber as a micro-reactor
substrate for the development of catalytic hollow fiber
MMR. They selected Ni/MgO-CeO2 that was impregnated
into the inner surface of YSZ hollow fibers using the sol-gel
technique. The finger-like structure of the YSZ hollow fiber
can be regarded as hundreds of conical micro-channels
that increase the catalytic surface-to-volume ratio and
improve the heat and mass transfer, as well as the mixing
of gases during the reaction (Figure 6A). Excellent cata-
lyst utilization in the hollow fiber micro-reactor enables a
small quantity of catalyst to be used for the ESR reaction.
Using 8 units of the hollow fiber micro-reactor and only
18 mg catalysts, Rahman et al. (2011) produced a relatively
similar amount of H2 compared to a fixed-bed reactor that
used 100 mg catalysts.
Rahman et  al. (2012) developed their previous
study (Rahman et al. 2011) by employing a Pd-Ag mem-
brane on the YSZ hollow fiber (Figure 6B). The use of a
Pd-Ag membrane has some benefits, such as selectively
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388      M. Taghizadeh and F. Aghili: Hydrogen production by ESR in membrane reactors
A reactor, as the efficient selection of the preferable cata-
H2 CO
2
C2H5OH
YSZ hollow
+ fibre
3H2O
Catalyst
CO2 H2
layer
H2 H2 H2
B Pd/Ag membrane
CO2 CO2 CO2
H2 H2 H2 YSZ hellow fibre
H2 + CO2 H2 + CO2 H2 + CO2
Catalyst
CO2
C2H5O + 3H2O
Figure 6: Schematic diagram of a YSZ hollow fiber in which the
finger-like structure can be regarded as conical micro-channels.
The flow distribution of reactants in the conical microchannel (A).
Reprinted from Rahman et al. (2011). With permission from Elsevier
(copyright 2011). Schematic representation that the reactants enter
the conical micro-channels where ESR takes place. Then, H2 will be
separated using the Pd/Ag membrane while CO2 will be retained in
the lumen (B). Reprinted from Rahman et al. (2012).With permission
from Elsevier (copyright 2012).
removing H2 from the reaction zone, shifting the ther-
modynamic equilibria of intermediate reactions toward
product formation, increasing ethanol conversion, and
producing H2 with high purity in the shell side of the
MMR. Ni/Al2O3 and a palladium micro-membrane were
employed as the catalyst and the hydrogen separation
medium, respectively. de-Souza et al. (2013) investigated
ESR by a numerical comparison of an MMR with a mem-
brane-less micro-reactor. They used CFD simulation and
found that thin membranes (<0.5 μm) increased the total
hydrogen yield by up to 105% at a temperature of 773 K
and permitted a hydrogen yield of up to 0.833, which is
2-fold larger than that generated by the membrane-less
reactor. Consequently, MMRs can be successfully applied
to produce high-purity hydrogen for fuel cell systems,
which can generate power for modern multifunctional
portable devices.
5 Conclusions
This review focuses on the generation of hydrogen through
steam reforming of ethanol as a renewable resource.
We reviewed ESR from the perspective of the membrane
lysts and membranes is a crucial challenge for membrane
reactor design.
ESR is performed over a wide range of catalysts such
as noble metals, non-noble metals, and bi-metallic cata-
lysts. Rh (noble metal) and Ni (non-noble) show superior
activity in terms of ethanol conversion, selectivity, and
stability. It has also been observed that non-noble metals
are integrated with noble metals to make bi-metallic
catalysts for capturing the favorable effects of non-noble
metals.
The most studied membranes for hydrogen separa-
tion are dense metal membranes, among which Pd-based
membranes are closest to the market. Extensive experi-
mental studies have shown that the performance of the
Pd-based membranes can be enhanced by alloying the Pd
in binary or ternary alloys.
The membrane reactor plays a significant role in more
environmentally and energy-efficient production method,
because of its attractive possibility of removing thermo-
dynamic impasse, continuous operation, and integrated
production system. PBMR is the easiest to use and most
studied type of reactor. However, the extent of mass trans-
fer limitation and the non-uniform temperature are the
serious drawbacks related to this configuration. FBMRs,
owing to their better gas-solid contact and more flexible
structure, have shown higher potentials in the field of
hydrogen generation. MMRs have been proposed to maxi-
mize ethanol conversion and hydrogen selectivity because
of their great potential for process intensification. In the
FBMRs and MMRs, the mass transfer limitations within
the catalyst bed are circumvented, and thus the required
membrane area is minimized. Accordingly, the industrial-
type reactors for pure hydrogen production will most
likely be based on a fluidized bed configuration and/or
micro-structured reactors.
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Bionotes
Majid Taghizadeh
Chemical Engineering Department, Babol
Noshirvani University of Technology, P. O.
Box 484, Babol 4714871167, Iran,
e-mail: m_taghizadehfr@yahoo.com
Majid Taghizadeh is a professor of Chemical Engineering at Babol
Noshirvani University of Technology (Babol, Iran). He obtained his
BSc (Tehran University, Iran, 1988), MSc (Amirkabir University of
Technology, Iran, 1991), and PhD (University of Claude Bernard Lyon
1, France, 1998) in Chemical Engineering. His research areas focus
on catalysis, kinetics and reactor design, hydrogen production and
purification, and molecularly imprinted polymers. He has pub-
lished 60 journal papers and conducted more than 140 conference
presentations.
Fatemeh Aghili
Chemical Engineering Department, Babol
Noshirvani University of Technology, P. O.
Box 484, Babol 4714871167, Iran
Fatemeh Aghili is currently a PhD candidate at Babol Noshirvani
University of Technology, Iran. She obtained her BSc and MSc in
Chemical Engineering at Babol Noshirvani University of Technology,
Iran, in 2013 and 2015, respectively. Her research interests are in
the areas of separation processes, membrane technology, and
membrane bioreactors.
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