Ali Ebshish

Department of Chemical and Process Engineering,

Faculty of Engineering,
Universiti Kebangsaan Malaysia (UKM),
Bangi, 43600, Selangor, Malaysia
e-mail: aliebshish@gmail.com

Zahira Yaakob
Department of Chemical and Process Engineering,
Faculty of Engineering,
Universiti Kebangsaan Malaysia (UKM),
Bangi, 43600, Selangor, Malaysia;
Fuel Cell Institute,
Universiti Kebangsaan Malaysia,
(UKM), Bangi, Malaysia

Y. H. Taufiq-Yap
Centre of Excellence for Catalysis Science
and Technology,
Faculty of Science,
Universiti Putra Malaysia,
43400 UPM Serdang,
Selangor, Malaysia

Ahmed Bshish
Abdulmajid Shaibani
Department of Chemical and Process Engineering,
Faculty of Engineering,
Universiti Kebangsaan Malaysia (UKM),
Bangi, 43600, Selangor, Malaysia

Catalytic Steam Reforming

of Glycerol Over Cerium and
Palladium-Based Catalysts
for Hydrogen Production
In this work, catalytic steam reforming of glycerol for hydrogen production was performed over Ce/Al2O3 and Pd/Al2O3 catalysts prepared via the impregnation method.
The catalysts were characterized by scanning electron microscopy (SEM-EDX), transmission electron microscopy (TEM), BET surface area, and X-ray diffraction (XRD). Two
sets of catalytic reactions were conducted, one comparing 1% Pd/Al2O3 to 1% Ce/Al2O3
and the second comparing 1% Ce/Al2O3 loading to 10% Ce/Al2O3 loading. All catalytic
reactions were performed using a fixed-bed reactor operated at 600  C and atmospheric
pressure. Aglycerolwater mixture at a molar ratio of 1:6 was fed to the reactor at
0.05 ml/min. In the first set of experiments, Pd/Al2O3 exhibited higher hydrogen productivity than Ce/Al2O3. A maximum hydrogen yield of 56% and a maximum selectivity of
78.7% were achieved over the Pd/Al2O3 catalyst. For the second set of experiments, the
results show that the reaction conversion increased as the cerium loading increased from
1% to 10%. A total average hydrogen yield of 28.0% and a selectivity of 45.5% were
obtained over 1% Ce/Al2O3, while the total average hydrogen yield and selectivity were
42.2% and 52.7%, respectively, for 10% Ce/Al2O3. [DOI: 10.1115/1.4023687]
Keywords: reforming process, hydrogen production, catalytic system, glycerol

Introduction

Investigating new alternative energy sources has become necessary due to the drastic increase in energy demand and the extreme
reduction of conventional fuel sources. Hydrogen is among the
most promising alternate energy sources [1,2]. The main benefit
of using hydrogen as an energy carrier lies in its ability to provide
energy without negative effects on the environment [3]. In fuel
cell devices, hydrogen energy can be directly converted to reliable
electricity that can be used to power electric machines [47].
Moreover, hydrogen can provide a higher yield of energy than
hydrocarbon fuel [8]. Fossil fuels are the source of nearly 95% of
the feedstocks used for the production of hydrogen [3,9]. However, the challenges of providing sustainable and green energy
systems can only be overcome using renewable sources as feedstocks for hydrogen production [8,10]. Many materials are considered to be desirable substrates for biomass energy generation.
Because of its availability as a biomass by-product and its high
content of hydrogen, glycerol, which can be thermodynamically
used to produce hydrogen [11,12], is one of the biorenewable
materials that can act as a substrate for hydrogen production.
Moreover, glycerol is a nontoxic, nonflammable material and is
thus easy to handle [11,13].

Contributed by the Advanced Energy Systems Division of ASME for publication

in the JOURNAL OF FUEL CELL SCIENCE AND TECHNOLOGY. Manuscript received July 26,
2012; final manuscript received November 2, 2012; published online March 21,
2013. Assoc. Editor: Ken Reifsnider.

Several reforming processes, such as steam reforming [1316],

aqueous phase reforming [17,18], autothermal reforming [19],
partial oxidation [20], supercritical water reforming [21,22], and
photocatalytic reforming [23,24], have been used to produce
hydrogen from glycerol. Among these processes, steam reforming
is the most widely used method for H2 production [25]. In this
process, a glycerol-water mixture reacts at high temperature over
a suitable catalyst to produce H2 and CO2. In the catalytic process
of steam reforming of glycerol, the most interesting catalysts used
are Ni-based catalysts [15,26]. However, Ni-based catalysts suffer
from carbon deposition on the surface of the catalyst [27]. Different metal-based catalysts as well as noble metal catalysts have
also been used in glycerol steam reforming for hydrogen production [28].
In the present work, we aim to study the catalytic activity of a
rare earth metal, Ce, and a noble metal, Pd, both supported on alumina, in glycerol steam reforming for hydrogen production. The
impregnation technique was employed to prepare both of the
catalysts.

Experimental Work

2.1 Catalyst Preparation. Two catalysts were prepared using

the incipient wetness method. c-Al2O3 (SigmaAldrich), which was
treated at 500  C for 1 h to remove impurities, was used as the catalyst support. Cerium nitrate (SigmaAldrich) and palladium nitrate
(SigmaAldrich) were used as metal precursors. The metal loading
of Ce was fixed at 1 wt. % and 10 wt. %, whereas 1 wt. % of Pd was

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used for impregnation. Metals were impregnated in c-Al2O3 under

stirring at 75  C. After the impregnation process was complete, the
catalyst samples were dried overnight in an oven at 100  C and
then calcined at 550  C for 5 h. The catalysts were designated as
1 wt. % Ce/Al2O3, 10 wt. % Ce/Al2O3, and 1 wt. % Pd/Al2O3 corresponding to the Ce and Pd loading used.
2.2 Catalyst Characterization. Different techniques were
employed for catalyst characterization. To identify the crystalline
phases of cerium, palladium and alumina present in the catalysts,
X-ray diffraction (XRD) was performed with a Bruker AXS D8
Advanced diffractometer using a Cuka (k 1.54 deg) radiation
source and a scanning rate of 0.02 deg/s. The XRD patterns were
collected over a 2-h range from 10 deg to 80 deg. Scanning electron microscopy (SEM-EDX) (INCAX-sight (7353), OXFORD
instruments) was employed to show the distribution of Ce and Pd
on the support to study the weight ratio of elements and to investigate surface morphology. The structures and sizes of the particles
inside the catalysts were examined with a CM12 transmission
electron microscope (TEM) from Philips. An ASAP 2020 Micromeritics micropore surface area analyzer was used to determine
the surface area, pore volume and pore size of the prepared catalysts via nitrogen adsorption isotherms collected at 77 K.
2.3 Catalyst Activity Test. All catalytic experiments were
conducted in a fixed-bed stainless steel microreactor (length: 39 mm,
inside diameter: 6.35 mm, wall thickness: 0.9 mm). The catalytic activity of 1 wt. % Ce/Al2O3, 10 wt. % Ce/Al2O3, and 1 wt. %
Pd/Al2O3 catalysts in the steam reforming of glycerol was measured
at operating conditions of 600  C and atmospheric pressure. Glycerol
and water were mixed at a glycerol to water molar ratio of 1:6 and
then fed over 0.5 g of the catalyst, which was placed in the core of
the reactor and supported by glass wool. The feed was injected into
the reactor at a constant flow rate of 0.05 ml/min using an HPLC
pump (PHD 440, Harvard Apparatus). The catalysts were pretreated
at a high temperature of 500  C for 1 h to remove impurities and
then reduced at the same temperature for 2 h under hydrogen gas
flow. Crushed ice was used to cool the reactor output stream to separate the liquid products from the gases. Liquid products were analyzed with HPLC (Johnson Chromatography, 1200 series, Agilent
Technologies), whereas gases were purged into the GC (Clarus 500
Perkin Elmer with FID and TCD detectors) for gas analysis.
The activity performance of catalysts used in this study was
measured in terms of hydrogen yield, selectivity of hydrogen and
other gases, such as CO2, CO, and CH4, and conversion of glycerol into gaseous products. The following equations were used to
calculate these parameters:
hydrogen selectivity; %

H2 moles produced
1

 100
C atoms in the product RR
(1)

where RR is the reforming ratio of H2 to CO2 and its value based

on the glycerol steam reforming equation is 7/3,
selectivity of i; %

C atoms in species i
 100
C atoms in the product

(2)

In Eq. (2), species i CH4, CO2, and CO,

hydrogen yield;%

hydrogen moles produced

 100
maximum moles of hydrogen 7
(3)

glycerol conversion into gaseous product; %

C atoms in the product

 100
Total C atoms in the feedstock

(4)

Fig. 1 XRD analysis for (a) Al2O3, (b) 1 wt. % Pd/Al2O3, (c) 1 wt.
% Ce/Al2O3 and (d) 10 wt. % Ce/Al2O3

Results and Discussion

3.1 Catalyst Characterization. The crystalline phases of Pd/

Al2O3 and Ce/Al2O3 catalysts were analyzed by XRD. The XRD
patterns of prepared catalysts are shown in Fig. 1. For all catalysts,
the crystalline phase of c-Al2O3 is observed at 2h values of 37.3
deg, 47.4 deg, and 67.24 deg. In the 10% Ce/Al2O3 catalyst, the
peaks at 32.9 deg and 59.37 deg correspond to the structure of
CeO2, whereas the presence of CeAlO3 is confirmed by the peaks
at 28.5 deg, 56.33 deg, and 77.11 deg. Moreover, analysis of the
XRD diffraction pattern of a catalyst with a low cerium loading
(1 wt. % Ce/Al2O3) again reveals the presence of CeO2 as indicated by peaks at 32.9 deg and 59.37 deg. No peaks associated
with CeAlO3 are found for the 1 wt. % Ce/Al2O3 catalyst. For the
Pd/Al2O3 sample, weak diffraction lines of PdO are observed at 2h
values of 60.1 deg, 33.8 deg, and 54.9 deg. The XRD peaks of the
1 wt. % Ce/Al2O3 and 1 wt. % Pd/Al2O3 catalysts are almost identical to those of the support, and the presence of Ce and Pd phases
are not detected, which could be attributed to low metal loading.
SEM-EDX was used to determine the morphology, chemical
composition and the distribution of the active metal on the catalyst
surface. Figure 2 shows the morphology of the metal-loaded systems and alumina support. The distribution of Pd and Ce metal on
the support is illustrated with red dots. The analysis for both
metal-incorporated catalysts shows a uniform distribution of Ce or
Pd on the surface of the support. The good dispersion on the support surface indicates the effectiveness of the preparation process.
Table 1 shows the weight percent of Ce and Pd on the catalysts,
which nearly matches to the desired loading.
Approximately spherical morphology of Pd nanoparticles on
the crystalline phase of the support is revealed by TEM as shown
in Fig. 3. The average particle diameter of Pd detected by TEM is
approximately 6 nm. The images indicate a uniform distribution
of the metal, and the TEM analysis is in agreement with SEMEDX results. For 10 wt % Ce/Al2O3, the average particle diameter
of Ce is approximately 8 nm. Only 10 wt. % Ce/Al2O3 and 1 wt. %
Pd/Al2O3 catalysts were analyzed by TEM.
The BET surface area, pore volume and pore size of 1 wt. %
Pd/Al2O3, 1 wt. % Ce/Al2O3, and 10 wt. % Ce/Al2O3 are summarized in Table 2. The reduction of the surface area of 10 wt. % Ce/
Al2O3 could be attributed to the occupation of the Al2O3 pores by
CeO2 [5]. For 1 wt. % Pd/Al2O3, the small decrease in the surface
area after Pd incorporation is due to the small loading of Pd on the
Al2O3 support. The measurements of pore volume and pore size
indicate enough space for the reactants to enter the catalyst pores
and react and for the products to exit the pores.
3.2 Glycerol Steam Reforming. The catalytic activities of
1 wt. % Pd/Al2O3, 1 wt. % Ce/Al2O3, and 10 wt. % Ce/Al2O3 were
evaluated in the steam reforming of glycerol for hydrogen production. The first set of catalytic reforming experiments was
conducted over 1 wt. % Pd/Al2O3 and 1 wt. % Ce/Al2O3. For both

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Fig. 2 SEM for (a) 1 wt. % Ce/Al2O3, (b) 10 wt. % Ce/Al2O3, (c) 1 wt. % Pd/Al2O3, (d) 1 wt. % Ce/Al2O3 with Ce indicated in red,
(e) 10 wt. % Ce/Al2O3 with Ce indicated in red and (f) 1 wt. % Pd/Al2O3 with Pd indicated in red. (See online article for color.)

catalysts, hydrogen yield, moles of hydrogen produced per mole

of glycerol reacted, glycerol conversion into gaseous products and
the selectivity of gases produced were evaluated. As depicted in
Figs. 4(a) and 4(b), the 1 wt. % Pd/Al2O3 catalyst gives a higher
hydrogen yield than the 1 wt. % Ce/Al2O3 catalyst, with a maxiTable 1

Elements
Weight %
Atomic %

The loading of Ce and Pd over prepared catalysts

1 wt. % Pd/Al2O3

Catalysts
O
60.04
72.06

Al
39.02
27.77

mum of 3.92 and 3.12 mol of hydrogen produced per mole of

glycerol reacted for 1 wt. % Pd/Al2O3 and 1 wt. % Ce/Al2O3,
respectively. Figures 4(c) and 4(d) show the conversion of glycerol into gaseous products and the selectivity of hydrogen produced over these catalysts. As indicated in Fig. 4(c), the glycerol

1 wt. % Ce/Al2O3
Pd
0.94
0.17

Journal of Fuel Cell Science and Technology

O
61.02
72.88

Al
38.14
27.01

10 wt. % Ce/Al2O3
Ce
0.84
0.11

O
50.45
67.23

Al
39.55
31.25

Ce
10.00
1.52

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Fig. 3

TEM analysis for (a) 10 wt. % Ce/Al2O3 and (b) 1 wt. % Pd/Al2O3

Table 2
Catalysts
BET surface area, m2/g
Pore volume, cm3/g

Pore size, A

BET characterization of prepared catalysts

1 wt. % Pd/Al2O3

1 wt. % Ce/Al2O3

10 wt. % Ce/Al2O3

163
0.26
63

193
0.33
55

110
0.20
74

Fig. 4 Reforming activity over 1 wt. % Pd/Al2O3 and 1 wt. % Ce/Al2O3 (a) H2 yield, (b) moles of H2 produced, (c) glycerol conversion
into gases, and (d) H2 selectivity

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Fig. 5 Reforming activity over 1 wt. % Ce/Al2O3 and 10 wt. % Ce%Al2O3: (a) H2 yield, (b) moles of H2 produced, (c) glycerol
conversion into gases, and (d) H2 selectivity

conversion increased with time over 1 wt. % Pd/Al2O3 until it

reached its highest value of 78.9% at 2 h. In addition, stable glycerol conversion into gases was observed over 1 wt. % Ce/Al2O3
with a slight decrease after 2 h. Selectivity measurements presented in Fig. 4(d) show that the 1 wt. % Pd/Al2O3 catalyst was
more selective to hydrogen production than the cerium-based catalyst. The good performance of Pd/Al2O3 is because Pd, as a
noble metal, is more effective and gives good thermal stability for
the steam reforming of hydrocarbons, such as methanol [29], and
is more selective to hydrogen production than non-noble metals
[14,27,30]. Moreover, Pd is less susceptible to carbon formation
[14]. In general, catalysts can undergo chemical transformations
that significantly affect their characteristics during reaction. Pd is
more active and more stable than Ce because it has favorable lattice parameters [31]. For the Ce catalyst, there is no previous
study in which cerium is used as a catalyst for glycerol steam
reforming. Only its oxide has been used as a catalyst support, and
it suffered from carbon deposition, as reported elsewhere [32].
In the second set of experiments, the effect of cerium loading
on the glycerol reforming was evaluated over 1 wt. % Ce/Al2O3
and 10 wt. % Ce/Al2O3. As observed in Figs. 5(a) and 5(b), hydrogen yield and the number of moles of hydrogen produced
increased with increasing cerium loading. The maximum moles of
hydrogen produced for both catalysts were 2 and 3.12 for 1 wt. %
and 10 wt. %, respectively. Figures 5(c) and 5(d) show glycerol
conversion into gaseous products and hydrogen selectivity over
Ce-loaded alumina catalysts. Again, increasing the metal loading
enhanced the glycerol conversion into gases and improved the selectivity toward hydrogen production. Given that the synthesis
Journal of Fuel Cell Science and Technology

procedure of both catalysts and their reforming conditions are

same, the enhancement in the catalytic activity over 10 wt. %
Ce-loaded alumina is believed to be due to the increase in the
metal loading. The higher reduction in the hydrogen yield and
glycerol conversion into gases over 10 wt. % Ce/Al2O3 compared
to that over 1 wt. % Ce/Al2O3 after 2 h could be attributed to
higher carbon formation on the 10 wt. %-loaded catalyst.

Conclusions

Hydrogen production via steam reforming of glycerol was performed over two different alumina-supported metal catalysts, Ce
and Pd. All catalysts were prepared by the impregnation method.
To compare Ce and Pd activity as well as Ce loading, the metal
loading over the c-Al2O3 support was fixed at 1 wt. % and 10 wt.
% of cerium and 1 wt. % of palladium, and those three catalyst
systems were tested for glycerol reformation at 600  C and atmospheric pressure. The catalytic activity results showed that the 1 wt.
% Pd/Al2O3 catalyst produces better conversion to gaseous products and better H2 yield than not only 1 wt. % Ce/Al2O3 but also
10 wt. % Ce/Al2O3 under the experimental conditions examined.
The highest hydrogen yields achieved over 1 wt. % Ce/Al2O3,
10 wt. % Ce/Al2O3, and 1 wt. % Pd/Al2O3 were 29%, 44.7%, and
56%, respectively. To our knowledge, this is the first study that
has demonstrated the use of Ce as an alternative catalyst for
hydrogen production by steam reforming of glycerol. Nevertheless, better H2 selectivity with low amounts of carbon oxides
formed was attained over the 10 wt. % Ce/Al2O3 system. The
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good performance of the Pd catalyst is because of its favorable lattice parameters.

Acknowledgment
The authors gratefully acknowledge the financial support provided for this work by the Universiti Kebangsaan Malaysia under
the Grant No. UKM-OUP-NBT-28-124/2010.

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