development of pt-carbon catalysts using mcm-41 template for hi decomposition reaction in s–i...
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i n t e rn a t i o n a l j o u r n a l o f h y d r o g e n en e r g y 3 7 ( 2 0 1 2 ) 3 6 0 2e3 6 1 1
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Development of Pt-Carbon catalysts using MCM-41 templatefor HI decomposition reaction in SeI thermochemical cycle
Deepak Tyagi a, K. Scholz b, S. Varma a,*, K. Bhattacharya a, S. Mali c, P.S. Patil c,S.R. Bharadwaj a
aChemistry Division, Bhabha Atomic Research Centre, Mumbai 400085, IndiabDepartment of Chemistry, University of Otago, Dunedin, New ZealandcDepartment of Physics, Shivaji University, Kolhapur 416004, India
a r t i c l e i n f o
Article history:
Received 2 March 2011
Received in revised form
25 April 2011
Accepted 26 April 2011
Available online 1 June 2011
Keywords:
SeI cycle
HI decomposition reaction
Hard templating route
Pt-C catalysts
* Corresponding author. Tel.: þ91 22 2559228E-mail address: [email protected] (S. V
0360-3199/$ e see front matter Copyright ªdoi:10.1016/j.ijhydene.2011.04.206
a b s t r a c t
Different Pt-Carbon catalysts have been synthesized by hard templating route and have
been employed for production of hydrogen from liquid phase HI decomposition at 160 �C
temperature. The physical properties and catalytic activities of these catalysts are compared
with that of the platinum on activated carbon catalysts. These catalysts have been char-
acterised by X-Ray diffraction, Raman, SEM and BET surface area. Eluant analysis has been
carried out using ICP-OES for evaluation of the extent of noble metal leaching under the
catalytic activity test conditions. From the present study we have concluded that MCM-41
based Pt/carbon has higher catalytic activity and stability than other Pt/carbon catalysts.
Copyright ª 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights
reserved.
1. Introduction SulphureIodine cycle based on three step reactions where in
Hydrogen as a future energy carrier is a scenario of high
probability and necessity, considering the ill-effects and
depleting natural resources of fossil fuel based systems. For
this to be economically feasible, large scale production of
hydrogen has to be attained by environment friendly route.
Deployment of technologies based on nuclear or solar energy
for splitting of water to produce hydrogen provides a feasible
solution to this requirement. This way hydrogen can be
produced from water at temperatures much lower than the
direct water decomposition at 3000 �C.Various thermochemical cycles employing excess heat
from nuclear reactors are being evaluated for production of
hydrogen by splitting of water and these processes are at
different stages of development [1]. Among these, the
2; fax: þ91 22 25505151.arma).2011, Hydrogen Energy P
first step sulphur dioxide, iodine and water undergo Bunsen
reaction to produce sulphuric and hydriodic acids [2], is the
widely accepted one. Both the acids produced in first step get
separated based on the difference in their densities, in
presence of excess iodine in HI phase. Sulphuric acid is
decomposed at 800 �C to produce sulphur dioxide and oxygen
and hydriodic acid is decomposed at 400 �C to produce iodine
and hydrogen. Integration of all the three reactions into
a closed loop cycle results in an overall process leading to
splitting of water into hydrogen and oxygen. Decomposition
of hydriodic acid has a thermodynamic limitation due to
presence of a homogeneous azeotrope in the HIeH2O binary
system [3,4]. This makes the hydrogen production step highly
energy consuming one. Several alternatives have been
explored to improve efficiency of this process. The General
ublications, LLC. Published by Elsevier Ltd. All rights reserved.
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Atomic Co. group had proposed use of phosphoric acid for
concentration of the HI solution to obtain 99.7% HI vapour [5].
But, concentration of recycled phosphoric acid is again found
to consume large amount of heat and electricity. Various
other routes employing electro-electrodialysis concentration
method [6,7] and hydrogen permselective membrane reactor
[8] have also been reported by the JAERI group.
The alternate to such an approach exists in formof reactive
distillationwhich has an advantage of combining reaction and
separation in a single step leading to overall shift of equilib-
rium towards production of I2 and H2. This process was first
reported by Roth et al. [4] in 1989 and has been studied by
various research groups [9,10]. Hinshelwood et al. way back
in 1925 had demonstrated catalytic decomposition of HI gas
on platinum wire and reported the process to be kinetically
unimolecular [11]. Recently, there have been reports on
various platinum or nickel metal based catalysts for reactive
distillation of HI [12e14]. Various carbon based catalysts
systems have also been reported for this decomposition
reaction from 1980s onwards [15e17]. These studies have
highlighted the two major observations: (i) source of carbon
and its preparation method influence the surface
characteristics to a large extent and hence dictate its
catalytic activity and stability and (ii) presence of platinum
not only enhances the catalytic activity but also impedes
adsorption of iodine on the catalytic surface.
We in this paper report synthesis of different platinum
supported on carbon catalysts, where the porous carbon
supports are generated using hard template route. Platinum
incorporation has also been carried out either at carbonisation
stage or by impregnation after complete preparation of carbon
support. The prepared catalysts have been characterised
using XRD, SEM, Raman spectroscopy and N2 adsorption.
These catalysts have been evaluated for their stability under
the HI reflux conditions using ICP-MS. The conversion of HI to
hydrogen has also been assessed from this reflux.
2. Experimental
2.1. Catalyst preparation
Five platinum supported on carbon catalysts with 1 wt% noble
metal loading have been prepared for this study. Four of these
catalystswere based on porous carbon support synthesized by
hard template route.
2.1.1. Direct Pt-Carbon catalyst by hard template routeFor this purpose, 3 g of porous silica template like MCM-41
(prepared by the hydrothermal route, using CTAB as silica
directing agent, mentioned in detail on an earlier publication
[18]) or Fumed silica (Cab-o-sil� M-5) was mixed with 3 g
Sucrose, 6.3 ml chloroplatinic acid (1% solution) and 8.7 ml of
water, in a round bottom flask and stirred for 6 h and then
left standing overnight. The paste obtained was dried at
100 �C for 6 h and then carbonised at 160 �C for another 6 h.
The powder obtained was added to 2.4 g sucrose and 15 ml
water and whole process of stirring, drying and carbonisation
was repeated. The powder so obtained was heated at 800 �C(heating rate 2 �C/min) in nitrogen flow for 3 h, and reduced
in hydrogen flow at 300 �C for 3 h. Subsequently, the resulting
silica-platinum-carbon material was suspended in 25 ml of
40% hydrofluoric acid and stirred overnight at room
temperature. Finally, the product was then filtered,
thoroughly washed, and dried at 80 �C overnight. The sample
prepared by this route using MCM-41 and fumed silica as
template will be referred as Pt/MCM-C and Pt/FS-C in this
manuscript.
2.1.2. Indirect Pt-Carbon catalyst by hard template routeFor this purpose, 3 g of porous silica template (MCM-41 or
Fumed silica) was mixed with 3.75 g Sucrose, 0.42 g sulphuric
acid and 15ml of water, in a round bottomflask and stirred for
6 h and then left standing overnight. The paste obtained was
dried at 100 �C for 6 h and then carbonised at 160 �C for
another 6 h. The powder obtained was again mixed with 2.4 g
sucrose, 0.27 g sulphuric acid and 15 ml water and whole
process of stirring, drying and carbonisation was repeated.
The powder obtained was heated at 800 �C (heating rate 2 �C/min) in nitrogen flow for 3 h. Subsequently, the resulting
silica-carbon material was suspended in 25 ml of 40% hydro-
fluoric acid and stirred overnight at room temperature.
Finally, the pure porous carbon was then filtered, thoroughly
washed, and dried at 80 �C overnight and weighed. The yield
of porous carbon prepared fromMCM-41 (MCM-C) and Fumed
silica (FS-C) was found to be 2.15 g and 3.72 g, respectively. The
carbon support obtainedwasmixedwith appropriate quantity
of 1 wt% chloroplatinic acid solution (for final platinum
loading in catalyst to be of 1 wt %) and stirred for 6 h and left
standing overnight. The paste obtained was dried at 100 �C for
8 h. The platinum loaded carbon samples hence obtained
were reduced in hydrogen flow at 300 �C for 3 h. The sample
prepared by this route using MCM-41 and fumed silica as
template will be referred as MCM-C/Pt and FS-C/Pt in this
manuscript.
2.1.3. Impregnated Pt-Carbon catalystFor comparison purpose a catalyst was prepared by direct
impregnation of Pt on commercially available activated
carbon. For this purpose 10 g activated carbonwasmixedwith
2.1 ml chloroplatinic acid (1 wt%) solution, and stirred for 6 h
for impregnation step. The paste obtained after overnight
standing were dried at 100 �C for 8 h. These platinum loaded
samples were reduced in hydrogen flow at 300 �C for 3 h. The
sample prepared by this route using activated carbon as
support will be referred as AC-C/Pt in this manuscript.
2.2. Characterisation
The powder X-ray diffraction patterns were recorded on Phi-
lips analytical diffractometer (using Ni-filtered Cu Ka radia-
tion). The average crystallite size of noble metal particles was
determined according to the Scherer equation. The BET
surface areas of different samples were obtained from phys-
ical adsorption of N2 atw196 �C, on a Quantachrome Autosorb
- 1 instrument. The prepared samples were characterised by
spatially resolved Raman scattering spectrometer (Bruker
Model MultiRAM) using 1064 nm line of Nd:YAG laser, detec-
ted with a liquid-nitrogen cooled high resolution charge
coupled device (CCD) detector at 4 cm�1 resolution. The
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surface morphologies were studied using JEOL JSM-6360
scanning electron microscope.
Fig. 2 e XRDpatterns fordifferent freshsamples. (*Platinum).
2.3. Catalyst stability and activity test
Catalysts were evaluated for their catalytic activity for HI
decomposition reaction and stability employing a reactor
setup, as shown in Fig. 1. For a typical stability study, 250mg of
catalyst was added to 50 ml of 27% hydriodic acid solution in
250 ml round bottom flask. A water condenser (30 cm long)
was fixed at the top of the flask. The top of the condenser
was connected by tygon tube to two liquid traps containing
starch solution and 0.1 M silver nitrate solutions placed in
sequential order. The purpose of the traps was to ensure
that the gas bubbling out corresponds only to hydrogen and
not to Iodine and HI vapours. This also ensures that the gas
evolved as bubbles pertain only to hydrogen as other two
options are ruled out. The solution was heated at 160 �Ctemperature for 2 h duration. The selection of these
temperature conditions was based on the advantages of
liquid phase decomposition process over gas phase reactive
distillation as discussed by O’Keefe et al. [19]. The
equilibrium constant equation for decomposition of HI to H2
and I2 can be illustrated as given below:
Kp ¼P0:5I2P0:5H2
PHI(1)
It is evident from this equation that lowering of I2 partial
pressure is required for driving the reaction forward for
higher yield of H2 at a given partial pressure of HI. It has been
reported that a certain amount of iodine can remain adsor-
bed for decomposition reaction carried out at temperatures
in excess of 350 �C. This has been further supported by Kim
et al, that though iodine begins to desorb at 125 �C,
a constant amount of iodine gets adsorbed for temperatures
in excess of 325 �C [17]. In case of liquid phase decomposition
reaction, iodine formed at catalyst surface dissolves back
into as HI solution as polyiodide species. This dissolution
ensures an intimate contact between HI and catalyst
surface to maintain high reactivity levels even in presence
of I2. Upto 50% conversion is reported by O’Keefe et al. for
Fig. 1 e Reactor setup for catalytic activity and stability
studies.
48 h study at room temperature. Though the critical
temperature of pure hydrogen iodide is 150.8 �C, a solution
of iodine in HI will have a critical temperature somewhat
higher and that’s the reason for selection of 160 �C
temperature study for this study.
Two hour refluxing exhibits evolution of gas bubbles at
regular intervals. This gas evolved can be either hydrogen
produced or escaping hydroiodic acid or iodine. The gas
bubbling through trap does not lead to appearance of blue
colour or yellow precipitate in starch and silver nitrate
solutions, respectively. This confirms efficient refluxing of
produced iodine and unreacted HI within the reaction
vessel and hence the gas evolved is definitely hydrogen.
After cooling, the condenser washings were transferred to
the reaction bath and volume made up to 250 ml. Change in
Hþ and I� concentrations were analysed by acid-base and
iodometric titrations respectively, which help in indirect
assessment of the extent of HI decomposition. The solution
was filtered to separate the used catalyst and the eluant.
Table 1 e Surface area and pore volume of differentmaterials.
S. No. Catalyst Surface area(m2/g)
Pore volume(cc/g)
1. AC-C/Pt 325 0.18
2. Pt/MCM-C 725 0.46
3. Pt/FS-C 813 3.90
4. MCM-C/Pt 333 0.18
5. FS-C/Pt e e
6. MCM-41 1304 1.15
Fig. 3 e BET plots for calculation of surface area for different
samples.
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While, the spent catalysts were characterised by XRD,
Raman and SEM, the eluant was analysed using ICP-OES,
Model Activa, Horiba Jobin yvon, France, for the leached out
platinum. Hþ and I� concentrations were determined by
titrating them against 0.1 N NaOH and 0.1 NAgNO3 solu-
tions, respectively, using pH electrode and platinum elec-
trode on Titra Model auto titrator from Lab India. While
NaOH solution was standardised against solid KHP, AgNO3
solution was standardised against NaCl.
Fig. 4 e Pore size distribution for MCM-C/Pt and Pt/MCM-C
samples. (Inset: Adsorption Isotherm for Pt/MCM-C
sample).
3. Results and discussion
3.1. Characterisation
3.1.1. X-ray diffractionThe X-ray diffraction measurements were recorded in 10e80�
2q range. Fig. 2 shows XRD patterns recorded for different
samples. All the XRD patterns show a broad peak centring on
w23� value. This is matching with that for the amorphous
carbon materials. Pt/MCM-C and Pt/FS-C samples exhibit
distinct peak at 39.7� conforming to platinum metal (JCPDS
No. 04-0802). All other samples do not show any peak
corresponding to platinum. This implies that the during
direct Pt-Carbon catalyst synthesis by hard template route,
the platinum particles get sintered during high temperature
carbonisation step, whereas they remain uniformly
distributed in all other samples. The crystallite size as
calculated by Scherrer equation indicate for 33 and 42 nm
dimensions for platinum particles in Pt/MCM-C and Pt/FS-C
samples, respectively.
3.1.2. N2 adsorption measurementsNitrogen adsorption isotherms were recorded at �196 �Ctemperature. The sampleswere subjected to insitu evacuation
at 300 �C temperature for 12 h prior to recording of the
isotherm. The data obtained for different samples is compiled
in Table 1. All porous carbon based catalysts, prepared by hard
templating routes with direct or indirect noble metal
incorporation, were found to exhibit high surface area
ranging from 333 to 813 m2/g and their BET plots are as
shown in Fig. 3. The catalysts prepared by using MCM-41 as
the template showed a remarkable decrease in their surface
area and pore volume as compared to the parent MCM-41
itself. Their pore size distributions are as shown in Fig. 4
with the representative adsorption-desorption isotherm in
inset. Both the samples depict loss of order as most of the
pores exhibit size of less than 10 A dimension, but still
a peak can be observed at w40 A corresponding to presence
of mesopores. Among Pt/MCM-C and MCM-C/Pt catalysts,
the Pt/MCM-C catalyst exhibits more than double surface
area and pore volume. This indicates that either the noble
metal introduced before carbonisation has mostly become
a part of the carbon framework. Compared to this reduced
Fig. 5 e Raman spectra of (a) Pt/MCM-C, (b) Used Pt/MCM-C, (c) MCM-C/Pt, (d) Used MCM-C/Pt, (e) Pt/FS-C, (f) Used Pt/FS-C,
(g) FS-C/Pt and (h) Used FS-C/Pt samples.
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Table 2 e Raman data and calculated in-plane crystallitesize for different samples.
S. No. Catalyst Fresh sample Used sample
IG/ID ratio La (nm) IG/ID ratio La (nm)
1. Pt/MCM-C 0.89 274 0.85 262
2. Pt/FS-C 1.39 427 0.95 292
3. MCM-C/Pt 1.06 326 0.97 298
4. FS-C/Pt 1.15 354 1.05 323
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surface area and pore volume of MCM-C/Pt indicate for
platinum entering into the pores and hence blocking or
restricting them or is placed outside the pore structure as
separate low surface area phase. Sample prepared using
Fig. 6 e Scanning electron micrographs of (a) AC-C/Pt, (b) MCM-
samples.
fumed silica as template (Pt/FS-C) exhibits both high surface
area and also high pore volume.
3.1.3. Raman spectroscopyRaman spectroscopy is an effective method for the char-
acterisation of different carbon materials. Raman spectra of
the two crystalline forms of carbon i.e. diamond and
graphite are entirely different. Raman spectrum of FCC
lattice of diamond is simple, having first order band at
1332 cm�1 which is characteristic of CeC single bond (sp3
hybridisation). The Raman spectrum of graphite carbon
exhibits a single peak at w1580 cm�1 corresponding to the
E2g mode of vibration of sp2 hybridised carbon (G-band).
The porous carbon structures based on rolled in graphene
41, (c) Pt/MCM-C, (d) MCM-C/Pt, (e) Pt/FS-C and (f) FS-C/Pt
Table 3 e Catalytic activity and sample stability data forall samples.
S. No. Catalyst % Conversion(Hþ Titration)
% Conversion(I� Titration)
Pt ineluant(mg/l)
1. AC-C/Pt 13.1% 13.2% 39.7
2. Pt/MCM-C 17.0% e 39.8
3. Pt/FS-C 7.2% 5.7% 65.7
4. MCM-C/Pt 17.8% 17.5% 59.1
5. FS-C/Pt 6.5% e 80.7
6. Blank 2.8% 2.9% 11.4
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like units should also gives a peak at w1580 cm�1 due to
presence of sp2 carbon similar to that of graphite. Appear-
ance of another peak at w1300 cm�1 is inevitably observed
for such porous carbons and is assigned as D band, due to
defects in the carbon texture. This new band is an in-plane
mode which becomes active by small imperfections due to
the particle size effect and the loss of translational
symmetry in the disordered structure. The width and rela-
tive intensities of both G and D lines (IG/ID) vary with the
ordering of the structure and may be used to characterize
carbon materials (in general, a higher IG/ID ratio can be
correlated with a lower degree of disorder) [20].
As shown in Fig. 5, all the porous carbon catalysts (Pt/MCM-
C,MCM-C/Pt. Pt/FS-C and FS-C/Pt) prepared byhard templating
Fig. 7 e XRDpatterns for differentusedsamples. (* Platinum).
route exhibit well defined G-band along with a very broad
D-band. The presence of narrow peak around 1580 cm�1,
signifies presence of sp2-bonded carbon atoms in a two
dimensional hexagonal lattice, similar to graphitic carbon
species. Broad D-band is the result of defects within the
carbon textures and suggests for existence of disordered
graphitized domains. IG/ID ratios for all four catalysts, as given
in Table 2, are observed to be close to 1 and found to be in
good agreement with similar mesoporous carbon materials
as reported in literature [21,22]. IG/ID ratios obtained here are
almost double of the values reported for mesoporous carbons
with semi graphitized walls synthesized by Wu et al. [23]
using methane as carbon precursor at 1000 �C. Also, the in-
plane crystallite size (La) is calculated from IG/ID ratio using
eq. (2), as reported by Pimenta et al. [20] and the calculated
values are given in Table 2. The La values obtained are found
to be in 250e450 nm range. Though there is no direct
evidence of incorporation of Pt into the carbon chain from tell
tale shift in G-band value, the crystallite size of Pt (30e40 nm
obtained from XRD) may be the contributing factor for such
high La values.
LaðnmÞ ¼ �2:4 x 10�10
�l4laser
�IGID
�(2)
These data indicate for long range ordering of the graphi-
tized carbon with co-existence of defects. The long range
ordering and defects both can be attributed to presence of
noble metal incorporated on the carbon support.
3.1.4. Scanning electron microscopyScanning electron microscopy was employed to compare
morphology of the catalyst particles. Fig. 6a for AC-C/Pt
catalyst shows smooth surface with few large pore openings
and particles. This observation goes well with the low
surface area as obtained from N2 adsorption studies.
Compared to this, Pt/MCM-C (Fig. 6c) and MCM-C/Pt (Fig. 6d)
catalysts show rough surface with lot of trough and crest
like features but very few pore openings or particles.
Morphology of both these catalysts is very much different
from that for the MCM-41 that was used as template. The
carbon samples prepared using fumed silica as template,
Pt/FS-C (Fig. 6e) and FS-C/Pt (Fig. 6f) presents rough surface
morphology with some lose particles. There are no visible
macro pore openings for Pt/FS-C catalyst.
3.2. Catalyst stability and activity
3.2.1. Catalyst stabilityThe analysis of the eluant obtained after 2 h refluxing was
carried out using ICP-OES technique for leaching of noble
metal from the platinum carbon catalysts prepared in this
study. The data obtained is presented in Table 3. It is obvious
that platinum leaching is very much limited. Even for FS-C/Pt
catalyst, with highest platinum content in the eluant, the
amount of noble metal detected is merely 0.008% of the
initial loading. In general all the five catalysts have good
retention of the noble metal within the carbon matrix and
Pt/MCM-C and AC-C/Pt catalysts are found to be most stable.
XRD pattern recorded for the samples after the stability
studiesareshown inFig.7.TheXRDpattern for remainsimilar to
Fig. 8 e Scanningelectronmicrographsof (a)UsedAC-C/Pt, (b)MCM-41, (c)UsedPt/MCM-C, (d)UsedMCM-C/Pt, (e)UsedPt/FS-C
and (f) Used FS-C/Pt samples.
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original samples with broad peak at w23� 2theta value
corresponding to the amorphous carbon. Though XRD pattern
for used MCM-C/Pt and AC-C/Pt catalysts remain exactly same
as for the original samples, some variations are observed in the
peak corresponding to platinum at w39.6� value for remaining
samples. This suggests for some redistribution of the platinum
metal during the catalytic activity measurements. Sharp
prominent peaks corresponding to crystalline platinum
particle for Pt/MCM-C and Pt/FS-C catalysts are drastically
reduced and indicate for disintegration of larger particles into
smaller entities and their redistribution over the carbon
support. Pt/MCM-C has also shown minimum leaching of
noble metal (Table 3). FS-C/Pt catalyst shows a different kind
of behaviour with appearance of a sharp peak at 39.6�,indicating for the growth of noble metal particle in this
particular catalyst.
Raman spectra for the used samples as shown in Fig. 5 (b, d,
f and h) do not show much variation as compared to original
samples. The presences of graphene like basic units are
retained after HI decomposition. In general IG/ID ratio show
only marginal decrease for all the samples. Only Pt/FS-C
catalyst with high degree of ordering (IG/ID ¼ 1.39) for
original sample has a dramatic decrease in IG/ID ratio (0.95),
suggesting for increase in disorder for the carbon framework
structure. Still the ratios remain around 1 for all samples for
retention of graphene like carbon framework.
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Surface morphology of the used samples was analysed
using scanning electronmicroscopy and is shown in Fig. 8. The
activated carbon based samples (Fig. 8a) and the samples
prepared using fumed silica as template (Fig. 8e and f) are
found to retain morphological features similar to the ones
observed for fresh catalysts. The catalysts prepared using
MCM-41 as template, Pt/MCM-C (Fig. 8c) and MCM-C/Pt
(Fig. 8d), show slight change in surface morphology with over
all smoothening of the features. The surface morphology of
both these catalysts starts to show some resemblance to that
of MCM-41 template (Fig. 8b). In all no drastic changes are
observed in the catalyst surface morphology.
3.2.2. Catalyst activityThe catalytic activity of all the catalysts used in this study for
HI decomposition using the setup as given on Fig. 1, is as given
in Table 3. Percent conversions as calculated usingHþ titration
and I� titration are found to be in good agreement. The
procedure adopted and setup used has been designed taking
into consideration the volatility of hydriodic acid and iodine
under the experimental conditions and the total refluxing of
both these species has been ensured. The blank solution
without catalysts yields HI conversion of w2.8% after 2 h of
refluxing. Compared to this, Pt/FS-C and FS-C/Pt catalysts
yielded a conversion in 6e7 percent range. Catalyst prepared
by direct impregnation of activated carbon provides even
better catalytic with 13% hydriodic acid decomposition. The
platinum/carbon catalysts based on MCM-41 hard template
(Pt/MCM-C and MCM-C/Pt) exhibit best catalytic activity with
HI conversion over 17%.
Despite of the fact that Pt/FS-C catalyst has surface area and
platinum particle size similar to Pt/MCM-C catalyst and lot
higher pore volume its catalytic activity is still very low. The
activated carbon catalyst with low surface area but with mac-
roporousmorphologyexhibit reasonably good catalytic activity.
Among, Pt/MCM-C andMCM-C/Pt catalysts the activity remains
similar despite of vast difference in their surface area, pore
volume and platinum particle size. Only similarity between
these two catalysts is their surface morphology and meso-
porous nature of the pores. This indicates for the vital impact of
surface morphology and pore dimensions on the catalytic
activity for HI decomposition reaction. This is expected due to
large size of iodinemoiety,which has to be removed for smooth
functioning of the catalyst.
Overall the work reported in this paper, suggests that the
high surface area carbon support prepared using MCM-41 as
template acts as a good stable support for platinum. The
stability and catalytic activity of these catalysts is indepen-
dent of the stage at which platinum is incorporated and both
forms of catalysts are promising candidates for future work.
4. Conclusions
High surface area carbon supports were prepared using
MCM-41 and fumed silica based hard templates and were
found to be stable under liquid phase HI decomposition
conditions. The efficiencies of these materials for HI
decomposition reaction were found to be dependent on the
structural nature of the porous carbon and their surface
morphologies. Both the catalysts prepared using MCM-41 as
template with platinum incorporation before and after car-
bonisation stage are found to be effective catalysts for HI
decomposition reaction and are found to be stable under the
reported reaction conditions.
Acknowledgment
Dr. Kerstin Scholz is grateful to the Deutsche For-
schungsgemeinschaft (DFG no. BO 3238/1-1) for funding her
research at Bhabha Atomic Research Centre, Mumbai.
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