Effect of preparation method on physicochemical properties of a novel Co–Fe nano catalyst

Article abstract of DOI:10.1007/s13738-021-02176-1

The main approach of this study was to investigate the effect of the type of synthesis method on the improvement of catalyst performance in Fischer–Tropsch reaction. For this purpose, a series of the novel catalysts were synthesized using iron and cobalt nitrate salts, tetraethoxysilane and novolac phenolic resin by different method. These catalysts were abbreviated as M1–Co–Fe–novolac/SiO₂, M2–Co–Fe–novolac/SiO₂, and M3–Co–Fe–novolac/SiO₂ and characterized using different techniques. The results of the Brunauer–Emmett–Teller and Fourier transform infrared techniques showed that M2–Co–Fe–novolac/SiO₂ catalyst has a higher surface area than the other two ones. This catalyst was analyzed by using X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray, and temperature-programed reduction (TPR) techniques. The XRD results confirmed the appearance of suitable active phases, such as metal phase, carbide, and low oxidation state of metals. Based on TPR results, the lower reduction temperature, compared with similar samples, confirmed the high activity of the M2–Co–Fe–novolac/SiO₂ catalyst. Catalytic activity and selectivity for Fischer–Tropsch reaction were investigated in the standard conditions by using catalytic tests. The high conversion percentage of CO indicated high activity of the catalyst. On the other hand, the olefin to paraffin ratio (O/P), which was a criterion for catalytic efficiency in industrial, was also acceptable.

Full text of DOI:10.1007/s13738-021-02176-1

Journal of the Iranian Chemical Society
https://doi.org/10.1007/s13738-021-02176-1
ORIGINAL PAPER
Efect of preparation method on physicochemical properties of a novel
Co–Fe nano catalyst
Mahsa Ehsani Nia1 · Behnam Sedighi1 · Mohammad Joshaghani1
Received: 25 August 2020 / Accepted: 2 January 2021
© Iranian Chemical Society 2021
Abstract
The main approach of this study was to investigate the efect of the type of synthesis method on the improvement of catalyst
performance in Fischer–Tropsch reaction. For this purpose, a series of the novel catalysts were synthesized using iron and
cobalt nitrate salts, tetraethoxysilane and novolac phenolic resin by diferent method. These catalysts were abbreviated as M1–
Co–Fe–novolac/SiO2, M2–Co–Fe–novolac/SiO2, and M3–Co–Fe–novolac/SiO2 and characterized using diferent techniques.
The results of the Brunauer–Emmett–Teller and Fourier transform infrared techniques showed that M2–Co–Fe–novolac/
SiO2 catalyst has a higher surface area than the other two ones. This catalyst was analyzed by using X-ray difraction (XRD),
scanning electron microscopy, energy-dispersive X-ray, and temperature-programed reduction (TPR) techniques. The XRD
results confrmed the appearance of suitable active phases, such as metal phase, carbide, and low oxidation state of metals.
Based on TPR results, the lower reduction temperature, compared with similar samples, confrmed the high activity of the
M2–Co–Fe–novolac/SiO2 catalyst. Catalytic activity and selectivity for Fischer–Tropsch reaction were investigated in the
standard conditions by using catalytic tests. The high conversion percentage of CO indicated high activity of the catalyst.
On the other hand, the olefn to parafn ratio (O/P), which was a criterion for catalytic efciency in industrial, was also
acceptable.
Keywords Fischer–Tropsch synthesis · Nano catalyst · Cobalt/iron catalyst · Novolac phenolic resin
Introduction
and Co have been able to gain the necessary economic and
operational acceptance that each of them has its own unique
and valuable features. For example, iron has a special place
because it is cheaper than cobalt, and cobalt is considered
because of its stability and high activity [10]. For this rea-
son, iron and cobalt are used either as individual single-core
[11–13] or dual-core systems [14–17].
It is essential to have a clean process that can provide a reli-
able alternative to global hydrocarbons fuels with the least
environmental tensions [1]. Fischer–Tropsch (FT) synthesis
as a capable process can provide a wide range of hydro-
carbons including a variety of linear and branched alpha
and alcohol compounds [2, 3]. On the other hand, the gaso-
line and diesel fuel produced by this process do not need to
increase the octane number again, and it is free of any sulfur
and nitrogen contamination [4, 5]. As a result, the synthe-
sis of FT was considered by many researchers as a suitable
source for a wide range of organic compounds [5, 6].
The active phase is usually selected in such a way as to
provide maximum selectivity for the desired products and
to minimize the production of undesirable products in the
process [6]. For this reason, one of the advantages of using
bimetallic catalysts is to increase catalytic activity and selec-
tivity of valuable products [18].
Transition metals such as Co, Fe, and Ru were usually
used as catalyst in the Fischer–Tropsch reaction [7–9].
Among all metals that used in industrial catalysts, only Fe
Since the conversion reactions occur on the catalyst
surface, the high surface area is very important. If the
catalysts are prepared by simple impregnation, the reduc-
tion of specifc surface is inevitable [19]. To overcome this
problem, the use of organic polymers has become wide-
spread. These polymeric compounds provide a more suit-
able substrate for active phase distribution [16]. For exam-
ple, Liang et al. reported that the presence of resorcinol
* Behnam Sedighi
bseddighi@razi.ac.ir; manheb61@yahoo.com
1
Department of Inorganic Chemistry, Faculty of Chemistry,
Razi University, P.O. Box +98-67149, Kermanshah, Iran
Vol.:(0123456789)
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Journal of the Iranian Chemical Society
formaldehyde resin gel during the synthesis of the Co/
SiO2 catalyst is an efective factor in increasing the efec-
tive surface area of the catalyst [20]. It is also reported
that among diferent polymers, phenolic resol resins have
been used in Co–Fe catalysts and increased the activity
and selectivity of Fischer–Tropsch reactions [18]. The pol-
ymer resin is decomposed and removed during calcination,
and eventually, a porous catalyst with the high surface area
is created [16].
Experimental
Catalyst preparation
The Co–Fe–novolac/SiO2 catalysts were prepared by three dif-
ferent methods as described below.
Method 1: In the frst step two separate solutions A and B
were prepared as follow:
Solution A: To a solution of Fe(NO3)3·9H2O (4.1 g,
0.01 mol) and Co(NO3)2·6H2O (8.8 g, 0.03 mol) in 40 mL of
ethanol was added tetraethoxysilane (TEOS) (4.2 g, 0.02 mol),
and the solution was heated to 70 °C.
The physical properties, chemical composition, and
structure of the catalyst have essential role in the Fis-
cher–Tropsch synthesis [21, 22]. For example, active
phases of Co with an average pore diameter of 3.5–10 nm
have led to an increase in methane production and a
decrease in a tendency toward liquid products [21–27].
Since these properties depend on preparation method,
we synthesized a novel Co–Fe–novolac/SiO2 nanocata-
lyst using diferent methods and investigated the efect of
preparation method on the catalytic activity and selectiv-
ity of FT reactions. In other studies, Li et al. [10] also
investigated the efect of the chemical composition of
the catalyst on its performance in Fischer–Tropsch reac-
tions. By using iron-nickel bimetallic catalysts, they were
Solution B: Solution B was prepared by dissolving novolac
phenolic resin (5.0 g) in 40 mL of ethanol. Then, oxalic acid
(8.8 g, 0.097 mol) was added to this solution [26].
In the second step, solution B was added dropwise to the
solution A and the mixture was aged for 3 h. A creamy white
solid was precipitated which was washed twice with absolute
alcohol, fltered and dried in the oven at 120 °C for 20 h and
calcined at 650 °C in air for 6 h. The obtained catalyst was
labeled as M1–Co–Fe–novolac/SiO2.
Method 2: Fe(NO3)3·9H2O (4.1 g, 0.01 mol) and
Co(NO3)2·6H2O (8.8 g, 0.03 mol) were dissolved in 40 mL
of ethanol. Then, ammonia solution (10%) was added to form
the hydroxide deposit. Aging for 3 h followed by washing the
precipitate twice with absolute alcohol, fltering and drying
in the oven at 120 °C for 20 h resulted in a white creamy
solid. In another beaker, the novolac phenolic resin solution
was prepared by dissolving 5.0 g of resin in 40 mL of eth-
anol [29]. TEOS (5.2 g, 0.025 mol) and oxalic acid (8.9 g,
0.098 mol) were added to this solution and stirred until the gel
was formed. The solid involve metal oxide powder was added
to the gel with stirring, and the resulting mixture was heated
at 70 °C. Aging for 3 h followed by washing the precipitate
twice with absolute alcohol, fltering and drying in the oven at
120 °C for 20 h led to catalyst precursor which was calcined
at 650 °C in air for 6 h. The obtained catalyst was labeled as
M2–Co–Fe–novolac/SiO2.
+
able to efectively increase C5 production while reduc-
ing methane production. According to their results, the
use of bimetallic catalysts increases the conversion rate
of CO by improving the metal distribution at the catalyst
base, and investigated of the Mossbauer spectrum of the
catalyst, shows the production of a mixture of iron oxide
and carbide on the surface of the catalyst during the reac-
tion. Increasing nickel to iron-containing catalysts, while
reducing carbide production, increases metal oxide pro-
duction at the catalyst surface which continuation of this
process causes a sharp shift in the product distribution
from heavy hydrocarbons to lighter compounds and even-
tually methane. Also Shimura et al., by studying diferent
phase species of cobalt alumina catalyst, showed that the
porosity and phase structure of the catalyst greatly efect
on its activity [1].
Method 3: Fe(NO3)3·9H2O (2.05 g, 0.005 mol) and
Co(NO3)2·6H2O (4.4 g, 0.015 mol) were dissolved in 20 mL
of ethanol. TEOS (2.1 g, 0.01 mol) was added and the solu-
tion was heated to 70 °C. Then, the novolac phenolic resin
solution (novolac (2.5 g), oxalic acid (8.9 g, 0.098 mol), and
ethanol (40 mL)) were added dropwise, and the mixture was
aged for 3 h [28]. The mixture was placed in an autoclave with
a temperature of 160 °C. The resulting catalyst was calcined
at 650 °C in air for 6 h. The obtained catalyst was labeled as
M3–Co–Fe–novolac/SiO2.
The surface area, chemical composition, and structure of
the catalyst are dependent on the preparation method. How-
ever, the efect of the synthetic method on the efciency of
the FT catalysts has not been sufciently investigated.
Therefore, in the present work, we synthesized a novel
Co–Fe–novolac/SiO2 nanocatalyst using some differ-
ent methods and investigated the efect of the preparation
method on the catalytic activity and selectivity of FT reac-
tions. The physicochemical properties of the catalysts were
characterized by Fourier transform infrared (FT-IR), X-ray
difraction (XRD), Brunauer, Emmet and Teller (BET),
temperature-programed reduction (TPR), scanning electron
microscopy (SEM), and energy-dispersive X-ray (EDX)
methods.
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Journal of the Iranian Chemical Society
Catalyst characterization
Results and discussion
An ALPHA Bruker FT-IR spectrophotometer
(400–4000 cm−1) was used for FT-IR spectra. The XRD data
were obtained using Equinox 3000 inel, X-ray difractometer
(40 kV, 30 mA) using a Cu Kα radiation source (λ=1.542°A)
and a nickel flter. A NOVA 2200 Quantachrome instrument
was used for recording N2 adsorption–desorption isotherm at
liquid nitrogen temperature (−196 °C) and determination of
specifc surface area, total pore volume and the mean pore
diameter. All samples were degassed in advance at 110 °C in
an N2 fow for 3 h to remove the moisture and other adsorbates.
A micromeritic TPD-TPR 290 system was used to recorder
the TPR profle of catalysts using a mixture gas of (5/95: H2/
Ar; v/v) with 50 ml/min fow rate and heating to 820 °C at a
heating rate of 4 °C min. The SEM images of catalysts and
precursors were prepared using AIS2300C microscope con-
taining an IXRF model 550i accessory for energy-dispersive
X-ray (EDX) analysis.
Catalyst characterization
The changes of the samples during calcination were inves-
tigated by FT-IR spectroscopy (Fig. 1). For all synthesized
precursors, a broad band was observed above 3000 cm−1 and
was assigned to the water of crystallization of nitrate salts.
Catalyst performance
Catalytic performance was performed in a stainless steel-fxed
bed reactor loaded with 1.0 g of the catalyst. Gases fow was
controlled by a mass fow controller (MFC) and the reaction
pressure was measure by back pressure regulator (BPR). Ini-
tially, the catalyst was reduced using a H2 gas fow (30 ml/min)
at 450 °C under 1 bar pressure for 16 h. Then the tempera-
ture, pressure, mole ratio of H2/CO and GHSV were adjusted
according to the standard conditions [18]. The gasifed prod-
ucts were analyzed on-line by Varian gas chromatograph (star
3600CX) containing a thermal conductivity detector (TCD)
and a chromosorb column. The liquifed products were ana-
lyzed of-line by Varian CP 3800 containing a fame ionization
detector (FID) and a petrol TM DH100 fused silica capillary
column. The CO conversion and selectivity toward each prod-
uct were computed after reaching the steady state using the
normalization equation:
mol COin − mol COout
CO conversion (%) =
× 100
mol COin
niMi
Si(%) =
× 100
mol COin − mol COout
where ni is the number of carbon atoms, and Mi is the mole
of the product.
Fig. 1 FT-IR spectra of Co–Fe–novolac/SiO2 catalysts a precursor
and b before the test
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Journal of the Iranian Chemical Society
There was also a sharp band above 1641 cm−1 which was
assigned to vibrations of the aromatic functional of novo-
lac [18, 30]. These bands were almost disappeared in the
FT-IR spectra of the samples, which confrm the approxi-
mate decomposition of novolac during the calcination at
650 °C. This result confrms the data obtained from BET
method. Two vibration bands were observed in 570 cm−1
and 670 cm−1 for the calcined catalysts, which is due to
vibrations of Co–O bonds in Co3O4 [31].
Co3O4 (cubic, JCPDS No. 00-042-1467), Fe2O3 (rhombo-
hedral, JCPDS No. 00-089-0599) CoFe2O4 (cubic, JCPDS
No. 00-022-1086). Besides, the metal silicates including
Co2SiO4 (orthorhombic, JCPDS No. 00-070-2115) and
Fe2SiO4 (orthorhombic, JCPDS No. 00-076-0512) were
formed. However, the phases after the test were mainly
found in carbide, metallic, and low oxidation states forms
of cobalt and iron, including Fe, Co3C, Fe3O4, CoO, and
Fe2SiO4 [32].
Table 1 shows the textural parameters of the catalysts.
For all three catalysts, the surface area was much greater
after the calcination. This is mainly due to decomposition
and release of novolac during the calcination, which has
made this catalyst more porous with more surface area
[18], Liang et al. reported similar behavior in the Co-res-
orcinol/SiO2 catalyst [20]. The highest surface area belongs
to M2–Co–Fe–novolac/SiO2 which was prepared via the
method 2. Thus, M2–Co–Fe–novolac/SiO2 catalyst was
selected for more investigation.
The EDX technique was used to determine the purity
of the catalyst at the precursor level and before the test
for M2–Co–Fe–novolac/SiO2, which showed their purity
(Fig. 3). The signals below 2v are the result of the remain-
ing novolac [30]. This confrms the results of FT-IR, which
represented the approximate decomposition of novolac, as
well as confrms the X-ray difraction pattern, which indi-
cates the presence of carbide phases after catalyst testing.
SEM analysis of M2–Co–Fe–novolac/SiO2 samples is
shown in Fig. 4. The precursor shows an irregular dense
mass with diferent sizes which indicates that it has not yet
fully completed the preparation conditions. While the cata-
lyst after calcination and before the test shows the progres-
sive growing the crystals on the surface. The catalyst after
the test shows an irregular porous surface as more porous
as the precursor. This may be due to the release of reactive
substances or products of the FT synthesis to active phases
or phase changes during the FT reaction [20].
The XRD pattern of M2–Co–Fe–novolac/SiO2 before the
test shows slightly amorphous silicate phases (wide peak
2θ = 15–30°) (Fig. 2). The pattern before the test shows
high oxidation states iron and cobalt oxides including
Table 1 Textural properties of the precursor and Co–Fe–novolac/
SiO2 Catalyst before the test for three methods
Sample
Specifc surface Pore
Pore
To determine the surface reactivity of the
M2–Co–Fe–novolac/SiO2 catalyst, the TPR technique was
used (Fig. 5). Reduction peak temperature indicated the ease
of reduction and degree of interaction between diferent spe-
cies present in the catalyst sample [33]. Three-peaks in the
catalyst spectrum were observed. The frst peak at 250 °C
is probably due to the reduction of Fe2O3 to Fe3O4 and/or
Co3O4 to CoO [34]. The second peak at 400 °C can be due
to the reduction of Fe3O4 to FeO and/or CoO to Co. The last
area (m2/g)
volume
diameter
(Å)
(cm3/g)
Method 1
Method 2
Method 3
Precursor
Before test
Precursor
Before test
Precursor
Before test
151.384
318.446
164.831
343.823
144.816
296.738
0.16
0.41
0.38
0.41
0.52
0.82
12.9
12.9
12.9
12.9
12.9
12.9
Fig. 2 XRD patterns of precur-
sor and M2–Co–Fe–novolac/
SiO2 catalyst (before and
after the test). Black flled
circle Co3O4 (Cubic); black
circle Fe2O3 (rhombohedral);
black flled triangle CoFe2O4
(cubic); black triangle Co2SiO4
(orthorhombic); black flled
star Fe2SiO4 (orthorhombic);
black flled four pointed star
Fe3C (orthorhombic); Co3C
(orthorhombic); black square
Fe3O4 (cubic); black flled
oval CoO (cubic); black flled
diamond Fe (Cubic)
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Journal of the Iranian Chemical Society
Fig. 3 The EDX spectrum of the M2–Co–Fe–novolac/SiO2 catalyst in
a precursor, b catalyst before the test
peak at 520 °C can be due to reduction of FeO to Fe [35].
Compared to similar Co–Fe catalysts, the M2–Co–Fe–novo-
lac/SiO2 reduction temperature is lower, which is in agree-
ment with its high catalytic activity [18, 30]. Lower reduc-
tion temperatures increase the number of active phases such
as carbide and metal phases, which are responsible for con-
verting CO. The fnal two-peak area is greater than the frst
peak, indicating a complete reduction of the initial oxide
state that in line with the XRD results, a similar situation has
been reported in other examples of Co–Fe catalysts [18, 20].
According to the results of FT-IR, XRD, and TPR, during
the reduction before testing, the phases of iron oxide and
cobalt (Fe2O3, Co3O4) decreased to lower oxidation state
(Fe3O4, CoO).
Fig. 4 SEM images of M2–Co–Fe–novolac/SiO2 catalyst in a precur-
sor, b catalyst before the test and c catalyst after the test
Four important factors namely the total pressure (7, 4, and
10 bar), feed mole ratio (2, 2.5 H2/CO), GHSV (3, 6 mol/
min), and temperature (350 °C, 375 °C) were selected [18,
30]. On the other hand, the conversion of CO was chosen
as a response for catalyst activity, while products selectivity
was chosen as a measure of catalyst selectivity. The results
are summarized in (Table 2).
Catalyst testing
A catalyst activity test was performed to determine the activ-
ity and selectivity of the M2–Co–Fe–novolac/SiO2 catalyst.
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Journal of the Iranian Chemical Society
Fig. 5 TPR profle of the M2–
Co–Fe–novolac/SiO2 catalyst
before the test
Table 2 Catalytic performance of the M2–Co–Fe–novolac/SiO2 catalyst under diferent operational conditions during FT reaction
Std H2/CO T (°C) P (bar) GHSVa CO Con. CO2 (%) CH4 (%) C2–4(P) (%) C2–4(O) (%) O/P ratio C5+ (%) ROH (%)
(min−1
)
1
2
3
2
2.5
2.5
350
375
375
7
4
10
3
6
6
83.74
77.32
68.93
5.1
5.2
6.0
6.7
7.7
8.3
12.7
12.6
10.9
27.2
29.1
24.9
2.13
2.31
2.29
44.1
40.3
43.6
4.2
5.0
6.3
aGHSV Gas hourly space velocity
As can be seen, with increasing the GHSV, the CO con-
version was decreased, probably because of the less contact
time of the feed with the active catalytic phases [36, 37].
Also, with increasing the pressure, the CO conversion was
decreased, which is probably related to decreasing in the
bulk difusivity. As the temperature rises, the conversion
of CO was decreased, probably because of the infuence of
heavy products such as waxes onto pores and creation of
coke on the catalyst level [18]. Finally, it was observed that
by increasing the H2/CO molar ratio, the conversion of CO
was decreased, which is most likely related to greater efect
of the water–gas shift reaction [30].
Table 3 Comparison of O/P molar ratios for M2–Co–Fe–novolac/
SiO2, Co–Fe–resol/SiO2 catalysts and Fe–Mn-resol/SiO2
Entry
Catalyst
O/P ratio
References
1
2
3
O/P for Co–Fe–novolac/SiO2
O/P for Co–Fe–resol/SiO2
O/P for Fe–Mn–resol/SiO2
2.13
1.59
2.58
This work
[18]
[30]
FTS synthesis yields a wide series of olefn and parafn
products, the former is more valuable and uses in many of
industries. The potential application of the catalyst in indus-
try was determined by the aid of O/P ratio. The higher ratio
represents better industrial application [38, 39]. The O/P
ratio was increased with increasing the GHSV. The O/P ratio
depended on the catalyst type, under similar reaction con-
ditions, the O/P ratio of M2–Co–Fe–novolac/SiO2 catalyst
was lower than of Fe–Mn–novolac/SiO2 catalyst [30], but
compared to the same sample [18], the M2–Co–Fe–novolac/
SiO2 catalyst has an acceptable O/P ratio, which confrms
the efciency of this catalyst in the industry (Table 3).
decomposition of the novolac resin during calcination and
its removal resulted in an increase in the surface area and
pore volume. Based on the results of the BET and FT-IR
characterization tests, the M2–Co–Fe–novolac/SiO2 as the
optimal catalyst had a higher efective surface area than
two other ones.
Also, based on the results of XRD, TPR, SEM, and
EDX, the catalyst had suitable active phases such as metal-
lic phases, carbides, and low oxidation of metals. The
lower reduction temperature of the M2–Co–Fe–novolac/
SiO2 catalyst, compared to similar samples, confrmed the
greater activity of this catalyst.
Also, the catalytic test indicated the effective
CO conversion and an acceptable O/P ratio for the
M2–Co–Fe–novolac/SiO2 sample which confrmed the
efciency of the catalyst for industrial purposes.
Conclusions
The Co–Fe–novolac/SiO2 catalysts were prepared by
three diferent methods. In order to raise the efective sur-
face area of the catalyst, the novolac resin was used. The
Acknowledgements The authors would like to acknowledge Razi Uni-
versity for the fnancial support provided for this work.
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