Enhancement of Carbon Oxides Hydrogenation on Iron-Based Nanoparticles by In-Situ Water Removal

Article abstract of DOI:10.1002/cctc.201800821

The carbidization of Fe(0) nanoparticles (NPs) under syngas (CO/H₂) produces crystalline Fe_2.2C iron carbide NPs (ICNPs) displaying excellent hyperthermia properties, however, this transformation is significantly delayed by the concomitant water formation. Consequently, very long carbidization times (～140 h) are needed to obtain ICNPs with high specific absorption rate. In this paper, we show that the rate of the carbidization process can be greatly enhanced by the in-situ removal of water using activated molecular sieves. As a result, ICNPs displaying very high heating power were obtained after only 40 h. Using this strategy, CO was successfully replaced by CO₂ as a carbon source in the carbidization process, resulting in the efficient conversion of Fe(0) NPs to ICNPs at relatively low temperature (230 °C). Without water removal, carbidization did not occur under these conditions, and the Fe(0) NPs were clearly oxidized. In addition, this approach was successfully applied to displace the equilibrium of CO₂ hydrogenation and accelerate the rate of the magnetically induced hydrogenation of CO₂ on ICNPs. Interestingly, the in-situ water removal had also a strong influence on the product distribution and especially the chain growth process, leading to a higher selectivity towards the formation of C₃H₈ (～11 %).

Full text of DOI:10.1002/cctc.201800821

Accepted Article
Title: Enhancement of carbon oxides hydrogenation on iron-based
nanoparticles by in-situ water removal
Authors: Alexis Bordet, Juan M. Asensio, Katerina Soulantica, and
Bruno Chaudret
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To be cited as: ChemCatChem 10.1002/cctc.201800821
Link to VoR: http://dx.doi.org/10.1002/cctc.201800821
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10.1002/cctc.201800821
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Enhancement of carbon oxides hydrogenation on iron-based
nanoparticles by in-situ water removal
Alexis Bordet,[a]† Juan Manuel Asensio,[a] Katerina Soulantica,[a] Bruno Chaudret*[a]
hyperthermia properties, such as ferrites,[1a] Fe(0)[4] or iron
Abstract: The carbidization of Fe(0) nanoparticles (NPs) under
carbides[3h,5] is necessary.
syngas (CO/H2) produces crystalline Fe2.2C iron carbide NPs
A synthesis of 15 nm iron carbide NPs (ICNPs) displaying
excellent specific absorption rates, and their use for the
(ICNPs) displaying excellent hyperthermia properties, however,
this transformation is significantly delayed by the concomitant
magnetically induced hydrogenation of carbon dioxide has
been recently reported.[3h] Inspired from the Fischer-Tropsch
water formation. Consequently, very long carbidization times
(~140 h) are needed to obtain ICNPs with high specific
absorption rate. In this paper, we show that the rate of the
carbidization process can be greatly enhanced by the in-situ
removal of water using activated molecular sieves. As a result,
ICNPs displaying very high heating power were obtained after
only 40 h. Using this strategy, CO was successfully replaced by
CO2 as a carbon source in the carbidization process, resulting in
the efficient conversion of Fe(0) NPs to ICNPs at relatively low
temperature (230°C). Without water removal, carbidization did not
occur under these conditions, and the Fe(0) NPs were clearly
oxidized. In addition, this approach was successfully applied to
displace the equilibrium of CO2 hydrogenation and accelerate the
rate of the magnetically induced hydrogenation of CO2 on ICNPs.
Interestingly, the in-situ water removal had also a strong influence
on the product distribution and especially the chain growth
process, leading to a higher selectivity towards the formation of
C3H8 (~11%).
synthesis, the carbidization process is based on the reaction
between preformed Fe(0) NPs and a mixture of CO and H2 at
150°C.[3h,6] These NPs contain more than 80% of the carbon-
rich Fe2.2C crystallographic phase, which was demonstrated
to be the key to their enhanced heating power. Nevertheless,
this process generates water as
a byproduct, which
significantly slows down the hydrogenation of CO to C + H2O.
Consequently, very long carbidization times (140 h) are
needed to produce ICNPs displaying high SAR. Water
formation during carbon oxide hydrogenation is a well-known
issue in the Fischer-Tropsch synthesis, where it deactivates
the catalysts through oxidation. Considering iron catalyzed
Fischer-Tropsch synthesis, the presence of water also favors
the conversion of CO to CO2 through the water gas shift,[7]
and thus the production of H2 which may be responsible for
local reversibility of the carbide formation.[6] To solve these
problems, some processes now integrate complex hydrophilic
membranes to separate water from reactants and products.[8]
In this study, the water resulting from the carbidization
reaction was trapped i) to prevent the water gas shift reaction
and ii) to shift the equilibrium toward the formation of C + H2O
and thus speed up the conversion of 9.0 and 12.5 nm Fe(0)
NPs into Fe2.2C. We demonstrate that the in-situ water
removal using simple molecular sieves dramatically
accelerates the carbidization process while preventing the
oxidation of the NPs. As a result, high quality ICNPs
displaying high SAR could be obtained by carbidization of
Fe(0) NPs in only 40 h, which is three times faster than
without water removal. In addition, water removal by the
same approach resulted in a significant improvement in the
catalytic performance of ICNPs in the magnetically induced
hydrogenation of CO2 to hydrocarbons.
The synthesis of magnetic nanoparticles (NPs) able to
efficiently convert electromagnetic energy into heat through
magnetic hyperthermia is of special interest in the fields of
biomedicine and catalysis. NPs displaying high specific
absorption rates (SARs) indeed represent powerful
multifunctional tools which can be used in a wide range of
applications, such as medical magnetic hyperthermia,[1] drug
delivery,[1c,2] and magnetically induced catalysis.[3] While the
field of biomedicine still concentrates most of the applications
involving magnetic heating NPs[1b] – with iron oxides as
candidates of choice –, magnetic induction appears to be of
growing interest in the field of catalysis.[3] Considering
heterogeneously catalyzed reactions such as the Fischer-
Tropsch synthesis or the Sabatier reaction, which are
performed at relatively high temperatures (> 200°C for the
Fischer-Tropsch synthesis, > 250°C for the Sabatier reaction)
heating NPs should possess the appropriate magnetic
properties to reach these temperatures. Iron oxides being
inappropriate, designing NPs displaying more efficient
Monodisperse 9.0 and 12.5 nm Fe(0) NPs were synthesized
following a previously reported procedure[9] involving the
decomposition of an organometallic precursor under H2 in the
presence of a system of two ligands (Figure SI1). These
preformed NPs can then be carbidized by reaction with
H2/CO to yield Fe2.2
water.[3h,5] However, a long reaction time, typically 7-8 days at
150°C under syngas, is required for the formation of Fe2.2
C iron carbide nanoparticles and
C
ICNPs displaying high heating capacities. To reduce the
elaboration time, our strategy is to favor the formation of the
Fe2.2C iron carbide phase by continuously removing the water
produced during the reaction. Following the Le Chatelier
principle, a decrease in water partial pressure in the reactor
should indeed drive the reaction toward the formation of
water, and thus toward the incorporation of carbon atoms in
the Fe(0) NPs. To trap the water produced during the
carbidization process, molecular sieves previously activated
under vacuum at 350°C were used. In order to (i) avoid NPs
from entering in the molecular sieves and (ii) keep the
molecular sieves in a moderate temperature so that water is
not desorbed back to the solution, the sieves were placed in a
[a]
Dr A. Bordet, Dr. J. M. Asensio, Dr K. Soulantica, Dr B. Chaudret
LPCNO, Université de Toulouse, CNRS, INSA, UPS, 135 avenue de
Rangueil,
31077
Toulouse,
France
*E-mail: bruno.chaudret@insa-toulouse.fr
†
Present address: Max-Planck Institute for Chemical Energy
Conversion, Stiftstraße 34-36, 45470 Mülheim an der Ruhr
Supporting information for this article is given via a link at the end of
the document.
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10.1002/cctc.201800821
ChemCatChem
COMMUNICATION
glass cartridge in the interior of the Fischer-Porter head
(Figure SI2). This set-up avoids any contact of the
nanoparticle solution with the molecular sieves, which remain
close to room temperature. During the reaction, the effect of
the presence of molecular sieves is clearly visible. While in
the absence of molecular sieves, condensation and reflux of
water on the Fischer-Porter bottle walls is obvious, this
phenomenon is not visible in the presence of molecular
sieves. The effect of water removal on the carbidization rate
of Fe(0) NPs was investigated using XRD and VSM analysis.
The conversion of the bcc Fe(0) phase into the pseudo-
hexagonal Fe2.2C phase can be easily monitored by XRD. In
addition, the carbidization extent can be correlated to the
coercive field of the resulting NPs. Figure 1 displays XRD
diffractograms, TEM images and magnetic measurements of
NPs obtained after 40 h carbidization without and with
molecular
sieve.
Figure 1. XRD, TEM and VSM analysis of NPs obtained after 40 h carbidization (a,b,c) without molecular sieves, (d,e,f) with molecular sieves.
After 40 h under classical conditions, the diffractogram in
Figure 1b shows that the NPs contain a mixture of Fe(0) and
Fe2.2C. In sharp contrast, NPs reacted for 40 h in the
presence of molecular sieves appear to be fully converted to
the Fe2.2C phase, without any traces of the initial bcc Fe(0)
structure being visible (Figure 1e). The magnetic
measurements also show major differences, with a much
higher coercive field for the NPs carbidized in the presence of
molecular sieves (100 mT against 44 mT, Figures 1c and 1f
respectively). These results demonstrate that the presence of
molecular sieves speed up the transformation of Fe(0) into
iron carbide.
under classical conditions since the diffusion of carbon is of
course easier in smaller NPs (Figure 2b).
Magnetic hyperthermia measurements were undertaken in
order to determine if this method could also decrease
significantly the time needed to obtain ICNPs displaying high
specific absorption rate. The SARs of ICNPs were determined
by calorimetry using a coil with an adjustable magnetic field
amplitude μ0Hrms in the range 0 – 47.4 mT, working at a fixed
frequency f = 100 kHz (Figure 2). Additional details are
available in the supporting information (Section hyperthermia
measurements and Figure SI3).
While under classical conditions, a 40 h carbidization time of
12.5 nm NPs (Figure 2a) yields NPs possessing very poor
heating power, the same reaction time in the presence of
molecular sieves gave ICNPs with very high SARs. In
addition, it appears that ICNPs produced through this
approach display SARs very similar to the ones observed for
ICNPs obtained after 140 h of carbidization in the absence of
molecular sieves. Removing water during the carbidization of
Fe(0) NPs thus allowed us to divide by three the reaction time
needed to obtain high SARs. The SAR measured at 47 mT
reaches ~ 3000 W.g- 1 at 100 kHz, which is similar to that
obtained after 140 h, the highest value by far ever reported
for iron based NPs.[3h] Interestingly, the same phenomenon
could be observed starting from 9.0 nm Fe(0) NPs. In this
case also, the addition of molecular sieves allowed obtaining
ICNPs displaying very high SAR in only 24 h, against 120 h
Figure 2. Heating properties of ICNPs obtained from a) 12.5 nm Fe(0)
NPs, b) 9.0 nm Fe(0) NPs. SAR measurement at 100 kHz.
Carbon monoxide being a highly toxic gas, it was of great
interest to look for a safer carbon source in the carbidization
process. We thus investigated the possibility to perform the
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carbidization of Fe(0) NPs with a mixture of carbon dioxide
and dihydrogen. The objective is to achieve the in-situ
reduction of CO2 to CO through the iron-catalyzed reverse
water gas shift reaction. The CO produced can then react
with H2 at the surface of the NPs to form the carbide phase.
The first attempt to carbidize 9.0 nm Fe(0) NPs using CO2
and H2 was performed under the same conditions as with CO
and H2. As expected, a temperature of 150°C is insufficient to
activate the CO2 molecule.[6] Consequently, the temperature
was increased to 230°C, and the carbidization of 9.0 nm
Fe(0) NPs was performed in the solid state during 24 h, in the
absence and in the presence of molecular sieves. At the end
of the reaction, the resulting NPs were characterized by TEM
and XRD (Figure 3).
induced iron carbide catalyzed hydrogenation of carbon
dioxide to hydrocarbons. We recently showed that ICNPs are
moderately active for this reaction.[3h] Therefore, our objective
was to shift the equilibrium of the Sabatier reaction toward the
formation of hydrocarbons by the in-situ removal of the water
produced.
The effect of molecular sieves on the catalytic hydrogenation
of carbon dioxide was investigated in a batch reactor
(Fischer- Porter bottle, see Figure SI2). H2 and CO2 (3 bars,
ratio H2/CO2 = 4/1) were reacted for different periods of time
on magnetically activated ICNPs (35 mT, 300 kHz), in the
presence or not of molecular sieves. At the end of the
reactions, the CO2 conversion and product distribution were
determined by gas chromatography (see Figure SI4 for an
example). Representative mass spectra are also given in
Figure SI5.
The time profiles and results associated to these reactions
are presented in Table 1.
For both series of experiments, the formation of carbon
monoxide (CO), methane (CH4), C2 products (ethene C2H4
and ethane C2H6) and propane (C3H8) is evidenced, meaning
that ICNPs are able to reach, through magnetic induction, the
temperature required to activate the Sabatier reaction.
The results show that the hydrogenation of CO2 is
significantly faster in the presence of molecular sieves (43%
vs 32% after 30 min, 79% vs 69% after 7 h).
Furthermore, significant differences are observed for the
formation of CO, CH4, C2 and C3H8 in both series.
The first observation deals with the evolution of the product
selectivities as a function of reaction time. For the series of
experiments performed in the presence of molecular sieves,
the selectivities towards the formation of CO, CH4, and C2 are
constant for the reaction times considered (respectively ~
15%; ~ 60% and ~ 20%). This suggests a good stability
(magnetic and catalytic properties) of the catalyst.
In sharp contrast, without molecular sieves the selectivity
towards the formation of CO, CH4, C2 and C3H8 is clearly
dependent on the reaction time. Thus, from 15 min to 7 h, the
selectivity decreases from 35% to 20% for CO, 34% to 22%
for C2 and increases from 31% to 52% for CH4 and from 0%
to 4% for C3H8. These changes of selectivity tend to indicate
Figure 3. Characterization of NPs after 24 h reaction under CO2/H2 (1/2, 3
bars) at 230°C. (a) TEM, (b) XRD of NPs obtained after reaction in the
absence of molecular sieves; (c) TEM, (d) XRD of NPs obtained after
reaction in the presence of molecular sieves.
For the reaction without molecular sieves, the TEM
micrograph shows a slight coalescence of the NPs, while the
XRD diffractogram evidence major modifications of the NPs
structure. The carbidization is however poorly efficient, the
main visible peaks still corresponding to the bcc Fe(0) phase.
Moreover, the NPs were clearly oxidized during the process,
producing crystalline Fe3O4. We assume that the temperature
is sufficient to activate the CO2 molecule toward CO and H2O
(reverse WGSR), but the carbidization process is very slow
and the NPs get oxidized by the water released. These
results show that despite the high temperature, carbon could
not be easily incorporated in Fe(0) NPs starting from a
mixture of CO2 and H2.
a
poor catalyst stability or/and a modification of the
equilibrium due to the increasing concentration of water in the
reactor. The decrease in CO selectivity supports the latter
explanation, since the Water Gas Shift Reaction (reversible
formation of CO2 and H2 from CO and H2O) is expected to be
faster in the presence of water.
Then, a direct comparison of the values evidences a lower
selectivity towards the formation of CO (5 to 15% lower) when
molecular sieves are used, showing
a more efficient
conversion of CO to hydrocarbons when water is removed.
Interestingly, the selectivity towards the formation of C3H8 is
higher (~ 11% vs ~ 4%) in the presence of molecular sieves
after 7 hours of reaction, indicating that the chain growth
process may be favored under these conditions even at low
conversions, i.e. far from the thermodynamic equilibrium.
After 7 h of reaction, the molecular sieves were regenerated
under vacuum at 250°C and the desorption products
analyzed by mass spectrometry. The results evidence the
presence of small quantities of water, H2 and CO2, but no CO
or hydrocarbons (Figure SI6). This fact suggests that water is
the only reaction product resulting from CO2 hydrogenation
that is trapped by the molecular sieves, and thus the
difference of reactivity in the two series of experiments can be
attributed to the difference in water content in the reactors.
For the reaction performed in the presence of molecular
sieves, TEM analysis evidences a slight coalescence of the
NPs, while XRD results show that the NPs are mainly
composed of Fe2.2C. The in-situ removal of water thus
enables the hydrogenation of CO2 over Fe(0) NPs under mild
conditions (230°C), that is, at a temperature lower than what
is usually required on iron catalysts (> 250°C). This approach
also prevents the oxidation of the NPs, which is crucial in
order to obtain suitable magnetic properties. Further
optimization of the carbidization reaction with CO2/H2 is
nevertheless required to avoid NPs agglomeration. That is
why ICNPs prepared by carbidization under CO/H2 were used
in the following catalytic study.
The possibility to enhance the CO2 activation on iron-based
nanoparticles using molecular sieves led us to investigate the
catalytic version of this reaction, namely the magnetically
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Without molecular sieves
Product distribution (Selectivity) %
With molecular sieves
Product distribution (Selectivity) %
CO2 Conv.
CO
CH4
C2*
C3H8
CO2 Conv.
CO
CH4
C2*
C3H8
Time (h)
0.25
0.5
1
26
32
41
58
67
69
9 (35)
11 (34)
12 (24)
12 (23)
13 (22)
13 (21)
8 (31)
11 (35)
18 (45)
30 (53)
35 (52)
36 (54)
9 (34)
10 (31)
10 (24)
12 (21)
14 (22)
15 (22)
0 (-)
0 (-)
1 (2)
2 (4)
3 (5)
3 (4)
33
43
53
71
77
79
6 (18)
7 (16)
19 (58)
25 (58)
31 (58)
40 (56)
43 (56)
44 (56)
7 (21)
9 (21)
1 (3)
2 (5)
8 (15)
10 (20)
14 (20)
15 (19)
15 (19)
4 (7)
3
10 (14)
11 (14)
11 (14)
7 (10)
8 (11)
9 (11)
5
7
Table 1. Catalytic results forthe magnetically induced CO2 hydrogenation on ICNPs without and with molecular sieves (AC magnetic field parameters: 300 kHz, 35
mT). The CO2 conversion and product distribution were determined by gas chromatography. *C2 products (C2H6 + C2H4)
To conclude, here we show that carbon oxides hydrogenation
over iron-based NPs can be greatly improved through the in-
situ removal of the water produced during the reaction. In the
presence of molecular sieves, the carbidization rate of
preformed Fe(0) NPs with CO/H2 was significantly improved,
resulting in ICNPs displaying very high SARs after only 40 h
reaction, against 140 h under classical conditions. More
importantly, the carbidization process could even be initiated
at 230°C using CO2 as a carbon source, while using such a
low temperature is not efficient without molecular sieves and
results in the oxidation of the NPs. Water elimination during
the reaction thus allows the replacement of CO by CO2 as
carbon source in the carbidization reaction, which is a crucial
step in the development of a green and safe process.
Interestingly, in-situ water removal does not only provide an
acceleration of the carbidization process, but also ensures the
good quality of the NPs by preventing their oxidation.
Keywords: CO2 Hydrogenation
Nanoparticles • Magnetic Hyperthermia • Water Removal
•
Iron Carbide
•
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COMMUNICATION
Alexis Bordet, Juan Manuel Asensio,
Katerina Soulantica, Bruno Chaudret*
Page No. – Page No.
Enhancement of carbon oxides
hydrogenation
nanoparticles
removal
on
iron-based
in-situ water
by
The synthesis of Fe2.2C iron carbide NPs was improved by removing the water
produced during the reaction. This strategy dramatically reduces the time needed to
produce NPs with exceptional hyperthermia properties and prevent their oxidation.
Iron carbide NPs were used for the magnetically induced hydrogenation of CO2,
during which the removal of water lead to an enhancement of the CO2
hydrogenation and to an increase in the yield of C3H8.
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