Selective Catalytic Reduction of NO by NH3 over MoO3 Promoted Fe2O3 Catalyst

Article abstract of DOI:10.1134/S002315841805018X

A series of MoO₃ doped Fe₂O₃ catalysts prepared by the co-precipitation method were investigated in the selective catalytic reduction of NO by NH₃ (NH₃-SCR). The catalysts displayed excellent catalytic activity from 225 to 400°C and high tolerance to SO₂/H₂O poisoning at 300°C. To characterize the catalysts the N₂-BET, XRD, Raman, NO-TPD, NH₃-TPD and in situ DRIFTS were carried out. It was found that the main reason explaining a high NH₃-SCR performance might be the synergistic effect between Fe and Mo species in the catalyst that could enhance the dispersion of Fe₂O₃ and increase NH₃ adsorption on the catalyst surface.

Full text of DOI:10.1134/S002315841805018X

ISSN 0023-1584, Kinetics and Catalysis, 2018, Vol. 59, No. 5, pp. 628–634. © Pleiades Publishing, Ltd., 2018.
Selective Catalytic Reduction of NO by NH3 over MoO3
Promoted Fe2O3 Catalyst1
J. Wanga, Zh. Xua, W. Zhaoa, and X. Lia, *
aState Key Laboratory Breeding Base of Coal Science and Technology Co-founded by Shanxi Province
and the Ministry of Science and Technology, Taiyuan University of Technology, Shanxi, Taiyuan 030024 P.R. China
*e-mail: lixiaoliang@tyut.edu.cn
Received November 4, 2017
Abstract—A series of MoO3 doped Fe2O3 catalysts prepared by the co-precipitation method were investigated
in the selective catalytic reduction of NO by NH3 (NH3-SCR). The catalysts displayed excellent catalytic activity
from 225 to 400oC and high tolerance to SO2/H2O poisoning at 300oC. To characterize the catalysts the N2-BET,
XRD, Raman, NO-TPD, NH3-TPD and in situ DRIFTS were carried out. It was found that the main reason
explaining a high NH3-SCR performance might be the synergistic effect between Fe and Mo species in the catalyst
that could enhance the dispersion of Fe2O3 and increase NH3 adsorption on the catalyst surface.
Keywords: NO, NH3-SCR, MoO3 modified catalysts, synergistic effect
DOI: 10.1134/S002315841805018X
INTRODUCTION
mance under the conditions used in the catalytic test-
ing. Therefore, it could be a good choice to introduce
the suitable additive into the pure Fe2O3 to enhance its
NH3-SCR performance.
Nitrogen oxides NOx, produced by the combustion
of fossil fuel, could cause many environmental issues,
such as acid rain, ozone depletion and photochemical
smog [1, 2]. The selective catalytic reduction of NO by
NH3 (NH3-SCR) is the state-of-art technology for the
NOx abatement. For the coal fired power plants, the
V2O5–WO3 (MoO3)/TiO2 has been put into real appli-
cation for many years due to its high De–NOx effi-
ciency and excellent tolerance to SO2 poisoning.
However, a narrow reaction temperature window of
300–400°C and the biological toxicity of vanadium spe-
cies to the environment and human beings are some
drawbacks of these catalysts [3, 4]. The development of
the environmentally benign NH3-SCR catalyst that can
maintain promising catalytic performance has received
increased attention in recent years.
The investigation of iron based oxide catalysts
remains an active area of research because these mate-
rials exhibit a high level of the NH3-SCR activity,
high resistance to the SO2 poisoning, environmentally
friendly and relatively high redox properties. However,
the NO conversion over pure Fe2O3 is far from satis-
factory at low temperatures since iron oxide shows a
relatively low surface area and acidity. To improve its
NH3-SCR performance, iron oxides have been doped
with different promoters such as Fe–Ti [5], Fe–V [6],
Fe–W [7, 8], Fe–Mn [9, 10], Fe–V–Ti [11] and Fe–
Ce [12], all of which showed high NH3-SCR perfor-
Alternatively, MoO3 has been used as a promoter to
improve the NH3-SCR activity. MoO3 modified
CeAlOx showed high denitration efficiency and the
redox ability with the total acidity of the catalyst
enhanced by the introduction of Mo [13]. It was found
that by adding MoO3 into CeO2/TiO2 it is possible not
only to increase the population of Brønsted acid sites
but also reduce the thermal stability of the inactive
nitrate species on the catalyst surface [14]. Meanwhile,
Ding et al. reported that the introducing Mo to Ce–Zr
mixed oxide catalyst could inhibit the growth of the
CeO2 particle size, improve the redox ability and
increase the amount of surface Lewis acidity [15].
Based on the idea that iron based mixed oxide are
highly active in the NH3-SCR and MoO3 exerts a pos-
itive promoting effect of in the denitration reaction the
MoO3 we have initiated the synthesis of modified
Fe2O3 catalysts by co-precipitation method in order to
compare the catalytic performance of these materials.
EXPERIMENTAL
Catalyst Preparation
MoO3 modified Fe2O3 catalysts were synthesized
by the co-precipitation method using Fe(NO3)3
·
9H2O and (NH4)6Mo7O24 · 5H2O as precursors and
25 wt % NH3 · H2O as precipitator. The aqueous solu-
1
The article is published in the original.
628

SELECTIVE CATALYTIC REDUCTION OF NO BY NH3 OVER MoO3
629
tions of (NH4)6Mo7O24 · 5H2O with equal weight measured with an online chemiluminescent NO/NOx
H2C2O4 · 2H2O were added to deionized water. After analyzer (KM9106, Kane Inc., UK) and the N2O con-
the (NH4)6 Mo7O24 · 5H2O was dissolved completely, centration was analyzed by a gas chromatograph
(FULI 9790, Zhejiang Wenling Inc., China) with a
porapak Q column. NO conversion and N2O selectiv-
ity were calculated by using:
the Fe(NO3)3 · 9H2O was added into the aqueous solu-
tion with required molar ratio (Fe/Mo = 1 : 1, 2 : 1,
4 : 1 and 8 : 1). Excessive 25 wt % NH3 · H2O solution
was dropped into the mixed solution under vigorous
agitation until pH 10. The precipitated solids were col-
lected by filtration and washed with distilled water,
followed by drying at 105°C for 12 h and subsequently
calcination at 500°C for 5 h in the static air atmo-
sphere. Finally, the catalyst pellets were crushed and
sieved and an aliquot of the 40–60 mesh fraction was
used in further experiments. For comparison purpose,
pure Fe2O3 and MoO3 were also prepared using the
same synthetic method.
[NOx] − [NOx]
in
NO conversion =
out ×100%,
[NOx]
in
2[N2O]out
N2O selectivity =
×100%,
[NOx]in − [NOx]out
NO = NO + NO .
[
]
[
]
[
]
x
2
RESULTS AND DISCUSSION
Activity Test
Characterization of Catalysts
The NO conversion and N2O selectivity in the
selective catalytic reduction of NO by NH3 as a func-
tion of temperature over Fe2O3, MoO3 and MoO3
modified Fe2O3 catalysts are shown in Fig. 1. It can be
readily seen that pure MoO3 exhibited negligible SCR
activity and N2O selectivity over the whole tempera-
ture range. Pure Fe2O3 also showed poor NH3-SCR
catalytic performance with the maximum NO conver-
sion at 250°C not exceeding 32.6%. However, the
NH3-SCR activity could be improved markedly upon
adding MoO3 to Fe2O3. At the Fe/Mo molar ratio =
1 : 1, more than 40% of NO was converted and N2O
selectivity below 5% was achieved in the temperature
range from 250 to 450°C. When the Fe/Mo molar
ratio reached a value of 2 : 1, the SCR activity and N2O
selectivity was further improved over the whole tem-
perature range used in the test. When the Fe/Mo
molar ratio was increased to 4 : 1, the highest activity
was attained in the tested temperature range, with the
NO conversion >90% and N2O selectivity <5%. How-
ever, further increasing the Fe/Mo molar ratio
decreased the NO conversion at both low and high
temperatures. Therefore, the activity was probably
associated with the Fe/Mo molar ratio and the opti-
mal ratio was 4 : 1.
The specific surface area, pore volume and the
average pore size of the samples were obtained by N2
adsorption/desorption at 77 K using a Micromeritics
Tristar-3000 system (Micromeritics, US). The crystal-
linity of the catalysts were measured by means of pow-
der XRD patterns obtained on a Rigaku D/max 2500
X-ray diffractometer (Rigaku, Japan) with CuKα radi-
ation. Visible Raman spectra were registered at room
temperature on a Spex 1877 D triplemate spectro-
graph (HORIBA Jobin Yvon, France) with spectral
resolution of 2 cm–1. NO-TPD and NH3-TPD profiles
were measured by the Autosorb-iQ-C chemisorption
analyzer (Quantachrome Instruments, US). Prior to
NO-TPD the sample was first pretreated in a flow of
He at 400°C for 1 h and then cooled to 100°C. After-
wards, the sample was exposed to a flow of 500 ppm
NO for 1 h, followed by He purge for 1 h. Finally, NO-
TPD was run by heating the samples in He from 100 to
600°C at 10°C/min. In the case of NH3-TPD, the
samples were pretreated at 400°C under He for 1h,
then cooled to 50°C and saturated with 10% NH3/He
for 1 h, followed by purging with He for 30 min. Finally,
the samples were heated from 50 to 600°C at a rate of
10°C/min. The in situ DRIFTS experiments were per-
formed on a Fourier transform infrared (FT-IR) spec-
trometer (Nicolet Nexus 670, (Nicolet, US) equipped
with an in situ diffuse reflection chamber and high sen-
sitivity mercury-cadmium-telluride (MCT) detector.
For the purposes of evaluating the anti-poisoning
tolerance to SO2 and H2O, the Fe4MoOx catalyst was
selected to investigate the impact of 100 ppm SO2
and/or 5 vol % H2O on its catalytic performance at
300oC with the corresponding results collected in
Fig. 2. It could be seen that the Fe4MoOx catalyst
maintained nearly 100% NO conversion during the
tested period in the present of 5 vol % of H2O. When
100 ppm of SO2 was injected into the reaction gases,
the NO conversion decreased and gradually became
stable. The NO conversion was recovered after remov-
Activity Test
A fixed bed reactor was used to evaluate the NH3-
SCR activity. The flue composition was as follows:
500 ppm NO, 500 ppm NH3, 5% O2, 5 vol % H2O
(when used), 100 ppm SO2 (when used), N2 flow into
balance and a total flow rate of 500 mL/min. To main-
tain the GHSV at 50000 h–1 a fixed volume of the cat- ing SO2. As the 100 ppm of SO2 and 5 vol % H2O were
alyst (0.6 mL) was used. The concentrations of NO
and NO2 in the inlet and outlet gas were quantitatively
introduced into the reaction gases synchronously, the
NO conversion decreased much more markedly,
KINETICS AND CATALYSIS Vol. 59 No. 5 2018

630
WANG et al.
(a)
(a)
NO conversion, %
NO conversion, %
100
100
90
80
70
60
50
40
30
20
10
0
90
Add
Removal
Removal
Removal
80
(b)
(c)
100
90
Add
80
100
90
100 150 200 250 300 350 400 450
Add
T, °C
80
2
4
6
8
10 12 14 16 18 20
Time, h
(b)
N2O selectivity, %
50
45
40
35
30
25
20
15
10
5
Fig. 2. NH -SCR activity over Fe MoO catalyst in the
3
4
x
presence of H O/SO : (a) 5% H O, m; (b) 100 ppm SO , j;
2
2
2
2
(c) 5% H O + 100 ppm SO ,.. At 300°C under GHSV
2
2
–1
of 50000 h
.
increasing Fe/Mo molar ratio remaining however
much larger than those found for pure Fe2O3 and
MoO3. This trend was also consistent with the varia-
tions in the NO conversion over the temperature range
of 250–450°C. However, reductions in the average
pore diameter associated with the addition of MoO3
into the Fe2O3 catalyst cannot be correlated with the
amount of the dopant. It could be therefore implied
that the catalyst structural parameters are hardly the
key factors determining the NH3-SCR activity. Com-
bining the NH3-SCR performance and BET analysis
results, it also could be suggested that incorporation of
Mo into Fe oxide results in the formation of MoO3
promoted Fe2O3 catalysts with properties different
from a mechanical mixture of two oxides.
0
100 150 200 250 300 350 400 450
T, °C
Fig. 1. NH -SCR activity (a) and N O selectivity (b) as
function of temperature over Fe O , MoO and MoO
modified Fe O catalysts (j Fe : Mo = 1 : 1, d Fe : Mo =
2 : 1, m Fe : Mo = 4 : 1, . Fe : Mo = 8 : 1, b Fe O ,
3
2
2
3
3
3
2
3
2
3
–1
c MoO ) under GHSV of 50000 h
.
3
which could be attributed to the presence of
NH4HSO4 deposited on the catalyst surface [15].
However, the NO conversion exceeded values of 89%
during the tested period. All these results suggest that
the catalyst showed an adequate tolerance to SO2/H2O
poisoning.
XRD and Raman Analysis
The presence of crystal phase of Fe2O3 in the MoO3
modified Fe2O3 catalyst is confirmed by X-ray diffrac-
tion study (Fig. 3a). XRD patterns of all samples show
characteristic broad peaks at 24.3°, 33.4°, 35.8°, 41.1°,
49.6°, 54.2°, 57.8°, 62.7°, 64.2°, 72.3° and 75.6° (2θ)
corresponding to the typical Hematite-Fe2O3
(PDF33-0664). At the same time, no characteristic
diffraction peaks of MoO3 were observed. A weak
crystallization or a good dispersion on the MoO3
modified Fe2O3 surface may be a reason. Table 1
shows the crystallite sizes of Hematite-Fe2O3 in the
BET Result
The BET physical property parameters of the
Fe2O3, MoO3 and Mo modified Fe2O3 catalysts are
summarized in Table. It could be found that the BET
surface area and pore volume of the Fe–Mo mixed
oxide increased at first and then decreased with tested catalysts calculated by using the Scherrer equa-
KINETICS AND CATALYSIS
Vol. 59
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SELECTIVE CATALYTIC REDUCTION OF NO BY NH3 OVER MoO3
Table 1. The BET physical parameters of the MoO3 modified Fe2O3 catalysts
631
Crystallite size
*
BET surface area,
BJH pore volume,
Average pore size,
Sample
m2/g
cm3/g
nm
of
, nm
Fe2O3
Fe2O3
42.4
64.9
73.2
82.7
76.2
1.6
0.23
0.36
0.45
0.58
0.49
0.02
17.1
10.3
13.2
14.4
21.6
45.8
22.7
19.6
17.5
14.1
15.1
–
FeMoOx
Fe2MoOx
Fe4MoOx
Fe8MoOx
MoO3
*Fe O crystallite size calculated by Scherrer equation from XRD results.
2
3
tion. The data indicate variations in the crystallite 245°C for Fe2O3 can be ascribed to the decomposition
dimensions of the catalyst samples prepared with dif-
ferent Fe/Mo molar ratio. The lower Hematite-Fe2O3
crystallite sizes were registered for the Fe2O3 catalysts
containing increased amounts MoO3. It can be thus
inferred that the incorporation of molybdenum oxide
decreases the crystallite size of Fe2O3 thus enhancing
the dispersion of Fe2O3 on the catalyst surface.
of bridging nitrate. Desorption peaks at 307°C for
Fe4MoOx and 347°C for Fe2O3 are assigned to the
decomposition of monodentate nitrate [17]. It appears
that only sites associated with iron atoms are available
for adsorption of NO over these three catalysts and the
addition of MoO3 on the Fe4MoOx could inhibit the
formation of nitrate species to a certain degree. The
inhibition may be related to a reduced thermal stability
of the inactive nitrate specie on the catalyst surface
[14]. Although adsorption power of the Fe4MoOx
towards NO is weaker than that of the pure Fe2O3,
doping with Mo markedly improved the NH3-SCR
activity. The above results imply that some synergetic
effect between Mo and Fe species might exist in the
catalyst and make a material contribution to the
improvement of the NH3-SCR performance.
For the purposes of further understanding of the
structural characteristics, Raman spectroscopy was
also employed with the corresponding results col-
lected in Fig. 3b. As can be seen, the spectrum of
MoO3 showed nine Raman bands at 116, 129, 158,
284, 337, 378, 665, 819 and 995 cm–1 [16, 17]. In the
spectrum of Fe2O3 four bands at 215, 281, 391 and
587 cm–1 could be observed assignable to hematite
with small differences in peak positions ( 5 cm–1)
[18]. The band at 215 cm–1 is due to the Raman active
A1g mode of hematite and three peaks at 281, 391 and
The amount of acid sites on the catalyst surface
plays a crucial role in the NH3-SCR performance.
The acid content on the catalysts surface is character-
ized by using NH3-TPD with the corresponding pro-
files shown in Fig. 4b. It can be seen that the desorp-
tion curve for the Fe2O3 catalyst has two main peaks at
107 and 368°C. The peak at 107°C can be assigned to
the weakly adsorbed NH3, the peak at 368°C can be
attributed to the strongly adsorbed NH3 and the total
587 cm–1 are ascribed to Eg modes of hematite [19].
No MoO3 species were detected in the Fe–Mo based
catalysts. In addition, the band intensities due to
Fe2O3 on Fe–Mo mixed oxides decreased, indicating
that doping with Mo inhibited the crystallization of
Fe2O3 phase. Given that crystalline MoO3 could be
otherwise easily detected on the catalyst surface by
using Raman spectrum, the absence of the signals cor-
responding to MoO3 crystalline phase on the MoO3
modified Fe2O3 catalysts suggests a high degree of dis-
persion of MoO3 species on the catalyst surface. The
corresponding analytical data are in good agreement
with the XRD results.
acidity of the Fe2O3 catalyst was ~9.37 μmol g–1m–2.
Notably, the intensity of the Fe4MoOx desorption
peak was enhanced significantly by doping with Mo.
The peak due to the strongly adsorbed NH3 at 368°C
was shifted at 409°C and the total acidity was
increased to about 13.84 μmol g–1m–2. An explanation
can be offered that ammonia was coordinatively
bound to Mo surface cation species or protonated as
NO-TPD and NH3-TPD Analysis
The NO adsorption on the Fe2O3, MoO3 and
Fe4MoOx catalysts was characterized by using NO-
TPD with the corresponding results presented in
Fig. 4a. Fe2O3 and Fe4MoOx had two desorption lyst surface [21]. It seems that the increase in the sur-
peaks, whereas for MoO3 no peak was observed in the face acidity is a key factor contributing to the improve-
spectra. Desorption peaks at 210°C for Fe4MoOx and ment of the NH3-SCR activity.
NH4+
by interacting with Mo–OH groups on the cata-
KINETICS AND CATALYSIS Vol. 59 No. 5 2018

632
WANG et al.
(a)
(a)
Intensity
Intensity
245
Hematite-Fe2O3
5
4
3
2
1
347
Fe2O3
307
Fe4MoOx
MoO3
100
200
300
400
500
600
20
30
40
50
60
70
80
2θ, deg
Temperature, °C
(b)
Intensity
(b)
Intensity
409
103
819
995
Fe4MoOx
Fe2O3
129
116
284
158
665
337
378
MoO3
6
5
107
215
281
368
391
587
4
3
2
447
MoO3
1
50 100 150 200 250 300 350 400 450 500 550 600
Temperature, °C
200
400
600
800
1000
Raman shift, cm–1
Fig. 4. NO-TPD (a) and NH -TPD (b) profiles of Fe O ,
3
2 3
MoO , and Fe MoO .
3
4
x
Fig. 3. (a) XRD profiles of the catalysts: (1) Fe O ,
2
3
(2) FeMoO , (3) Fe MoO , (4) Fe MoO , (5) Fe MoO .
x
2
x
4
x
8
x
can be assigned to ionic
+ species on Brønsted acid
NH4
(b) Raman spectra of the catalysts: (1) Fe O ,
2
3
sites [6]. The bands at 3160, 3255 and 3347 cm–1 due
to N–H stretching vibration modes and three negative
bands at 3579, 3648 and 3724 cm–1 caused by the sur-
face O–H stretching were also observed [23–27].
(2) FeMoO , (3) Fe MoO , (4) Fe MoO , (5) Fe MoO ,
x
2
x
4
x
8
x
(6) MoO , (λ = 514.5 nm).
3
ex
In situ DRIFTS Results Analysis
After introducing NH3 to the Fe4MoOx sample, the
band attributable to ionic
+
species disappeared.
NH4
The in situ DRIFTS analysis was performed to
study NH3 adsorption and NO + O2 adsorption on the
However, the affinity of Lewis acid sites to NH3 mol-
ecules strengthened evidently. In the N–H stretching
region, three new bands were found at 3162, 3265 and
3349 cm–1. In addition, another three negative bands
appeared at 3632, 3655 and 3720 cm–1, which could be
assigned to absorption of hydroxyl groups. The NH3
adsorption results were consistent with the NH3-TPD
testing data. After introducing NO + O2 into the
DRIFT cell, some bands appeared at 1203, 1215, 1350,
MoO3, Fe2O3 and Fe4MoOx catalysts at 200oC.
According to the in situ DRIFTS information shown
in Fig. 5, no bands could be observed after adsorption
of NH3 or NO + O2 on the surface of MoO3. When the
sample of Fe2O3 was exposed to NH3, several bands
appeared at 1205, 1429, 1602, 3160, 3255, 3347, 3579,
3648 and 3724 cm–1. The band at 1205/1602 cm–1
could be attributed to NH3 coordinatively bound to
Lewis acid sites [21, 22], while the band at 1420 cm–1 1548, 1566, 1595 and 1597 cm–1. The bands at 1203
KINETICS AND CATALYSIS
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SELECTIVE CATALYTIC REDUCTION OF NO BY NH3 OVER MoO3
633
(a)
Intensity
MoO3
1205
3265
3349
3162
1602
3655
3720
3632
Fe4MoOx
1205
3255
3347
3160
1602
1429
3724
3648
3579
Fe2O3
1200
4000
3500
1800
1600
1400
Wavenumber, cm–1
(b)
Intensity
MoO3
1566
1597
1203
1350
Fe4MoOx
1548
1595
1215
1350
Fe2O3
1800 1700 1600 1500 1400 1300 1200 1000
Wavenumber, cm–1
Fig. 5. In situ DRIFTS of NH adsorption (a), NO + O adsorption (b) on the Fe O , MoO , and Fe MoO catalyst at 200°C.
3
2
2
3
3
4
x
NO2−
and 1350 cm–1 were assigned to chelated
and
Fe2O3 catalysts can be postulated, which could
strengthen the adsorption power of the catalyst surface
chelating nitrites, respectively [28, 29]. The bands at
1215, 1595 and 1597 cm–1 are due to bridging nitrate to NH3 and in this way enhance the de-NOx activity.
species [30, 31], the bands attributable to monoden-
In conclusion, MoO3 modified Fe2O3 catalysts
prepared by conventional co-precipitation method
exhibited excellent NH3-SCR activity over a relatively
wide temperature range from 225 to 400°C and strong
resistance to SO2 and H2O poisoning. The existence of
the synergistic effect between Fe and Mo species in the
tate nitrate were also found at 1548 and 1566 cm–1 [22,
32]. The intensity of the bands on the Fe4MoOx cata-
lyst was slightly compared to those of Fe2O3 in agree-
ment with the NO-TPD results. From the above anal-
ysis, the development of a certain synergistic effect
between Fe and Mo species in the MoO3 modified
KINETICS AND CATALYSIS Vol. 59 No. 5 2018

634
WANG et al.
17. Seguin, L., Figlarz, M., Cavagnat, R., and Lassègues, J.C.,
MoO3 modified Fe2O3 catalyst was crucial for achiev-
ing an improved NH3-SCR performance.
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18. Wan, Y., Shi, X., Xia, H., and Xie, J., Mater. Res. Bull.,
2013, vol. 48, p. 4791.
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KINETICS AND CATALYSIS
Vol. 59
No. 5
2018