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j.ijhydene.2018.07.096

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i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
Available online at www.sciencedirect.com
ScienceDirect
journal homepage: www.elsevier.com/locate/he
The stability of PteIr/C bimetallic catalysts in HI
decomposition of the iodineesulfur hydrogen
production process
Yunfei Zhang a,b, Ping Zhang a, Songzhi Hu a, Laijun Wang a,*,
Songzhe Chen a, Baijun Liu b
a
Institute of Nuclear and New Energy Technology, Collaborative Innovation Center of Advanced Nuclear Energy
Technology, Key Laboratory of Advanced Reactor Engineering and Safety of Ministry of Education, Tsinghua
University, Beijing 100084, PR China
b
College of Chemical Engineering, China University of Petroleum, Beijing 102249, PR China
article info
abstract
Article history:
Decomposition of HI is the key reaction of hydrogen production in the iodineesulfur
Received 30 November 2017
thermochemical water splitting cycle, so studies about the catalysts for HI decomposi-
Received in revised form
tion have drawn increasing attention. In this study, a series of monometallic Pt/C((Pt/C-400,
19 June 2018
Pt/C-500, Pt/C-600, Pt/C-700 and Pt/C-800), Ir/C(Ir/C-400, Ir/C-500, Ir/C-600, Ir/C-700 and
Accepted 15 July 2018
Ir/C-800) and bimetallic PteIr catalysts supported on active carbon (PteIr/C-400, PteIr/C-
Available online xxx
500, PteIr/C-600, PteIr/C-700 and PteIr/C-800 were prepared by the impregnationreduction-calcination method. Their catalytic activities were evaluated for HI decomposi-
Keywords:
tion in a fixed bed reactor at 400 and 500 C under atmospheric pressure. Their structures,
Thermochemical hydrogen
metal particles size and distribution, and specific surface area were characterized by X-ray
production
diffraction (XRD), Transmission electron microscopy (TEM) and Brunauer-Emmett-Teller
Iodineesulfur cycle
(BET) surface area, respectively. The results showed that the bimetallic PteIr catalyst had
Decomposition of hydrogen iodide
the excellent stability in terms of the anti-sintering structure and catalytic activity.
Supported PteIr catalysts
Therefore, the bimetallic PteIr catalysts are the good candidates to take the place of the
Calcination temperature
traditional monometallic Pt/C catalyst for catalyzing the HI decomposition.
© 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.
Introduction
The thermochemical water-splitting iodine-sulfur (IS) cycle
has been expected to be one of the most promising candidate
processes for large scale and cost effective hydrogen production. The IS cycle could be driven as the following three
reactions by using nuclear energy or solar radiation as the
heat source.
Bunsen reaction: SO2 þ I2 þ 2H2O ¼ 2HI þ H2SO4
HI decomposition: 2HI ¼ H2 þ I2
H2SO4 decomposition: H2SO4 ¼ SO2 þ 1/2O2 þ H2O
* Corresponding author.
E-mail addresses: 1509437063@qq.com (Y. Zhang), zhangping77@mail.tsinghua.edu.cn (P. Zhang), husz13@mails.tsinghua.edu.cn
(S. Hu), wanglaijun@mail.tsinghua.edu.cn (L. Wang), chenszh@mail.tsinghua.edu.cn (S. Chen), bjliu@cup.edu.cn (B. Liu).
https://doi.org/10.1016/j.ijhydene.2018.07.096
0360-3199/© 2018 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.
Please cite this article in press as: Zhang Y, et al., The stability of PteIr/C bimetallic catalysts in HI decomposition of the iodineesulfur
hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
2
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
Since the IS cycle was started by General Atomics (GA) in
1970s, several research groups have carried out the theoretical
and experimental studies about IS cycle [1,2]. Furthermore,
some integrated facilities of IS process have been built and
demonstrated for closed cycle operation by several institutes,
such as JAEA (Japan Atomic Energy Agency) [3,4], GA/SNL/CEA
(GA, Sandia National Laboratories, and Commissariat a
l'Energie Atomique) [5], KAERI (Korea Atomic Energy Research
Institute) [6], and INET (Institute of Nuclear and New Energy
Technology, Tsinghua University) [7].
As the key reaction of hydrogen evolution, the HI
decomposition has the very slow reaction rate and strongly
corrosive atmosphere in the IS cycle [1,2]. To realize the
workable decomposition of HI, high active and stable catalysts should be presented. Various types of carbon materials
have been examined for their performances to catalyze the
decomposition of HI [8e14]. Raw sources, preparation
methods, structures, and physicochemical properties of the
carbon materials have been revealed to influence differently
the performances of carbon catalysts. Various transition
metals such as Ni, Pd, Pt and Mo, supported on different
supports, including alumina, silica and carbon, have been
extensively studied for their catalytic activity to decompose
HI [8,15e21]. And supported Pt catalysts have been found to
show excellent catalytic performance for HI decomposition.
However, low durability and high cost for the Pt/C catalysts
are the major challenges hindering the large-scale implementation of HI decomposition. In order to increase the
catalyst stability and decrease the cost of Pt monometallic
catalysts, some bimetallic catalysts such as PdePt [22], NiePd
[23], PteIr [24], and NiePt [25] have been investigated for HI
decomposition. In our previous studies, we have confirmed
that the Pt based bimetallic catalysts show better activity and
stability than monometallic catalysts due to alloying of Pt
with other transition metals [22,24]. Recently, we have found
that PteIr bimetallic catalysts illustrated better performance
than both monometallic Pt and bimetallic catalysts (PtePd,
PdeIr) for HI decomposition [24,26]. However the antisintering properties for the PteIr/C catalysts calcinated at
different temperatures have not been studied for HI
decomposition.
In this study, a series of monometallic Pt/C, Ir/C and
bimetallic PteIr catalysts supported on active carbon were
prepared by the impregnation-reduction-calcination method.
Their catalytic activities were evaluated for HI decomposition
in a fixed bed reactor at 400 and 500 C under atmospheric
pressure. Their structures, metal particles size and distribution, and specific surface area were characterized by X-ray
diffraction (XRD), Transmission electron microscopy (TEM)
and Brunauer-Emmett-Teller (BET) surface area, respectively.
Experimental
Catalyst preparation
The commercial active carbon (AC) was purchased from
Xilong Chemical Company and was dried in air at 120 C for 4 h
before use. The samples containing 5 wt% of Pt, 5 wt% of Ir and
2.5 wt%e2.5 wt% of PteIr were prepared by incipient wetness
Table 1 e Specific surface area and porosity of catalysts at
different calcination temperature.
Sample
Fig. 1 e Effects of the calcination temperature on the
activity of Pt/C-Tcal, Ir/C-Tcal, and PteIr/C-Tcal for HI
decomposition at (a) 400 C, and (b) 500 C.
AC
2.5%Pte2.5%Ir/C-400
2.5%Pte2.5%Ir/C-500
2.5%Pte2.5%Ir/C-600
2.5%Pe2.5%Ir/C-700
2.5%Pte2.5%Ir/C-800
5%Ir/C-400
5%Ir/C-500
5%Ir/C-600
5%Ir/C-700
5%Ir/C-800
5%Pt/C-400
5%Pt/C-500
5%Pt/C-600
5%Pt/C-700
5%Pt/C-800
SBET
(m2/g)
Pore volume
(cm3/g)
Pore diameter
(nm)
1471.111
1160.182
1038.068
1025.549
842.660
830.289
1169.280
1101.152
893.651
830.515
793.549
1038.175
1040.736
982.269
818.777
809.370
0.312
0.207
0.106
0.134
0.154
0.149
0.178
0.161
0.126
0.119
0.105
0.156
0.120
0.208
0.154
0.177
19.144
17.077
17.187
17.198
19.203
17.058
16.950
17.061
17.155
17.051
17.123
17.235
17.046
17.059
17.142
17.145
Please cite this article in press as: Zhang Y, et al., The stability of PteIr/C bimetallic catalysts in HI decomposition of the iodineesulfur
hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
3
impregnation of AC with the H2PtCl6$6H2O, H2IrCl6$6H2O
(analytical reagent, Shanghai Guanghua Technology Co., Ltd.)
aqueous solution, respectively. After impregnation, the samples were dried at 120 C for 4 h, and then reduced by KBH4
aqueous solution at room temperature. The reduced samples
were filtrated and washed thoroughly with distilled water,
and finally dried in air at 120 C for 4 h. The obtained samples
were calcined at different temperatures (400e800 C) in a flow
of 30 ml/min with pure N2 for 2 h. Each resultant catalyst was
denoted as Pt/C-Tcal, Ir/C-Tcal, and PteIr/C-Tcal, where Tcal
referred to the calcination temperature.
decomposition was performed in a quartz tubular reactor
(outer diameter of 14 mm, inner diameter of 12 mm) under the
following conditions: catalyst mass of 100 mg, temperatures
at 400 and 500 C, atmospheric pressure, and hydriodic acid
flow rate of 1.0 mL/min, which was corresponded to the
weight hourly space velocity (WHSV) of about 1020 h. The
detailed activity evaluation of the catalysts was reported in a
previous publication [24]. After the reaction, the catalyst was
cooled to room temperature. TEM images were obtained to
characterize the morphology of the used catalysts.
Catalyst characterization
Results and discussion
Powder X-ray diffraction and Brunauer-Emmett-Teller surface
area measurements were performed in the same procedures
as described previously [19,24]. Transmission electron microscopy (TEM, Hitachi H-7650) images of the samples were also
obtained. For TEM sample preparation, the powder catalysts
were dispersed in alcohol through ultrasound for 10 min and
the aqueous suspension was dropped onto the holey carboncoated copper grids.
Activity comparisons of the bimetallic and monometallic
catalysts
Activity test
The catalytic activity test for hydriodic acid (7.4 mol/L,
analytical reagent, Rizhao Lideshi Chemical Co., Ltd.)
Fig. 1 shows the effects of calcination temperature on the
activities of the catalysts for HI decomposition at 400 C
(Fig. 1a) and 500 C (Fig. 1b). Generally, the activities of the Pt/
C catalysts are higher than those of the Ir/C catalysts, and the
bimetallic PteIr/C catalysts are highest under the same
experimental conditions. But the activity of Pt/C-800 became
lower than that of Ir/C-800, while the bimetallic PteIr/C-800
catalyst stayed the highest. So, it's clear that the addition of
appropriate amounts of Ir can considerably modify the catalytic activity of the Pt/C catalysts. Interestingly, in Fig. 1b,
Fig. 2 e XRD patterns of fresh monometallic and bimetallic catalysts calcinated at different temperature (a) Pt/C, (b) Ir/C and
(c) PteIr/C.
Please cite this article in press as: Zhang Y, et al., The stability of PteIr/C bimetallic catalysts in HI decomposition of the iodineesulfur
hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
4
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
the activities of the PteIr/C catalyst and the Ir/C catalyst
become similar, which indicates that the activity of the
catalyst for HI decomposition at high temperature (500 C)
relies mainly on Ir.
Surface areas and porosities of fresh catalysts
Table 1 shows the BET specific surface areas and porosities
of fresh catalysts at different calcination temperature. For
comparison, the BET specific surface areas and porosities of
AC were also obtained. It's clear that the surface areas and
pore volume of the catalysts decrease with the increase of
calcination temperature. That may be because of the
agglomeration of the metal nanoparticles under the calcination. It should be noted that the bimetallic catalysts have
similar specific surface areas with the monometallic Ir
catalyst, which are markedly higher than those of the
monometallic Pt catalyst under the same calcination
temperature.
XRD patterns of fresh and used catalysts
Fig. 2 shows the XRD patterns of monometallic and bimetallic
catalysts calcinated at different temperature (a) Pt/C, (b) Ir/C
and (c) PteIr/C. The peaks at around 2q ¼ 39.9 , 46.4 , 67.7 ,
81.5 are assigned to the metallic phase Pt. The other broad
peaks at around 2q ¼ 42 are associated with metal phase Ir,
which are observed for samples calcinated at 600 C. It is
noteworthy that the metallic Pt peak became more intense as
the calcination temperature increased, indicating increase in
the Pt particle size by sintering. The XRD patterns of the fresh
catalysts without calcination were typical of the amorphous
structure with complete absence of any sharp crystalline
peaks. When the calcination temperature was further
increased, crystallization began and several diffraction peaks
appeared. For Pt/C the diffraction peaks of the Pt (111), Pt (200),
Pt (220) and Pt (311) planes were quite clear at calcination
temperature of 600 C and all of them became more intense as
the calcination temperature increased. However, for PteIr/C
the diffraction peaks were still very weak below the calcination temperature of 700 C.
Fig. 3 displays the XRD patterns of the used monometallic
and bimetallic catalysts calcinated at different temperature (a)
used-Pt/C, (b) used-Ir/C and (c) used-PteIr/C. The typical Pt
diffraction peaks at approximately 39.9 (1 1 1), 46.4 (2 0 0),
67.7 (2 2 0), and 81.5 (3 1 1) are clear in the XRD patterns of the
used 5% Pt/C. The four diffraction peaks of the corresponding
crystalline planes can also be found in the XRD patterns of all
the PteIr bimetallic catalysts. Thus, the used PteIr/C bimetallic catalysts have the same FCC structure as the used Pt/C
monometallic catalysts. However, the diffraction peaks in the
used Pt catalysts are much sharper and stronger than those in
the used PteIr catalysts. The diffraction peaks in the used Ir
catalysts are very weak and board. As the calcination temperature increases, the diffraction peaks in the monometallic
and bimetallic catalysts become stronger and sharper. The
results show that the increase of calcination temperature
promotes the sintering of the metal nanoparticles, and the
addition of Ir improves the anti-sintering property and stability of the catalysts significantly.
TEM results of fresh and used catalysts
Fig. 3 e XRD patterns of used monometallic and bimetallic
catalysts calcinated at different temperature (a) Pt/C, (b) Ir/C
and (c) PteIr/C.
The TEM images (Fig. 4) of the monometallic and bimetallic
catalysts calcinated at 400 C and 700 C are taken for example
Please cite this article in press as: Zhang Y, et al., The stability of PteIr/C bimetallic catalysts in HI decomposition of the iodineesulfur
hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
to investigate the sintering of metallic particles, so do the used
catalysts (Fig. 5). Most of the particle diameters are in the
range of 1e5 nm. Obvious agglomeration of Pt nanoparticles
can be found in the TEM images of the used monometallic Pt
catalysts, which indicates that the stability of the supported
monometallic Pt catalysts is unsatisfactory for HI decomposition. This result is consistent with that of our previous study
[24,26]. The PteIr bimetallic particles are better dispersed on
the carbon support than the Pt monometallic particles.
Table 2 shows the average particle size (nm) based on the
TEM results of the fresh and used catalysts at different
calcination temperature. Compared with the fresh catalysts
calcinated at the same temperature, the used catalysts
5
generally have larger particle sizes, which may be because
of the agglomeration of the metal nanoparticles under the
harsh operating condition of HI decomposition. The sintering rates of monometallic Pt particles are significantly faster
than those of monometallic Ir and bimetallic PteIr particles,
which demonstrates that the monometallic Pt catalysts
have lower stability than the others. And with the increase
of calcination temperature, the average particle size of each
catalyst grows. These observations are well consistent with
the XRD results. Both TEM and XRD results reveal that the
addition of Ir increases the stability and dispersion of Pt
particles, which may play the important role for enhancing
the HI conversion.
Fig. 4 e The TEM images of the monometallic and bimetallic catalysts calcinated at 400 C and 700 C.
Please cite this article in press as: Zhang Y, et al., The stability of PteIr/C bimetallic catalysts in HI decomposition of the iodineesulfur
hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
6
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
Fig. 5 e The TEM images of the used monometallic and bimetallic catalysts (a) Pt/C-400, (b) Pt/C-700, (c) Ir/C-400, (d) Ir/C-700,
(e) PteIr/C-400, (f) PteIr/C-700.
Conclusions
Table 2 e Average particle size (nm) of catalysts at
different calcination temperature.
Sample
Temp.
400 C 500 C 600 C 700 C 800 C
fresh-5% Pt/C
fresh-5% Ir/C
fresh-2.5% Pt-2.5% Ir/C
used-5% Pt/C
used-5% Ir/C
used-2.5% Pt-2.5% Ir/C
3.06
2.19
1.74
14.33
2.86
3.63
3.87
2.59
2.20
15.19
2.95
4.11
4.20
2.58
2.43
16.53
3.42
3.59
4.51
2.91
3.29
16.74
3.48
3.66
4.86
3.53
3.75
21.76
3.69
4.25
The active carbon supported monometallic Pt, Ir and bimetallic PteIr catalysts under different calcination temperature
were prepared by impregnation-reduction-calcination
method. According to the comparative characterizations of
the fresh and used catalysts, the PteIr bimetallic catalysts
exhibit better stability than the monometallic Pt catalysts.
Bimetallic PteIr catalyst has small size and uniform distribution of supported metal nanoparticles, and is more antisintering than monometallic Pt catalyst. And the bimetallic
PteIr catalyst is more economical than the monometallic Pt
catalyst. As all above, the bimetallic PteIr catalysts are the
Please cite this article in press as: Zhang Y, et al., The stability of PteIr/C bimetallic catalysts in HI decomposition of the iodineesulfur
hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 8 ) 1 e7
good candidates to take the place of the traditional monometallic Pt/C catalyst for catalyzing the HI decomposition.
[13]
Acknowledgments
[14]
This work was supported by the National Natural Science
Foundation of China (Grant No. 21776155, 21576152, 21676153),
Chinese National S&T Major Projects (Grant Nos.
2017ZX06901-027 and 2018ZX06901-029), Program for Changjiang Scholars and Innovative Research Team in University
(IRT13026), and Beijing municipal S&T project (Grant No.
Z171100002017023).
[15]
[16]
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hydrogen production process, International Journal of Hydrogen Energy (2018), https://doi.org/10.1016/j.ijhydene.2018.07.096
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