Simultaneous Desulfurization and Hydrogenation of Model Diesel Fuel over Ni/ZnO–PdPt/USY Hybrid Catalyst

Article abstract of DOI:10.1134/S0036024418110213

Abstract: The clean production requires deep desulfurization to meet stringent environmental specification and aromatics hydrogenation to improve the quality of transport fuels. To achieve this objective, hybrid catalyst was prepared by mixing of PdPt/USY with Ni/ZnO powders. It was found that the hybrid showed higher activity and stability to hydrodesulfurization (HDS) of dibenzothiophene (DBT) and hydrogenation of tetralin than Ni/ZnO or PtPd/USY counterparts. PdPt/USY containing catalysts exhibited high trans/cis ration of decalin, this can be attributed to the isomerization on the acid sites of USY and the reduced interaction between olefinic intermediates with PdPt bimetals. The hybrid catalyst also had high hydrogenation ability and stability to bulky aromatics of pyrene with the existence of DBT. The XRD, XPS, and BET characterizations revealed that PdPt/USY is responsible for DBT HDS, HYD and isomerization whereas Ni/ZnO play supporting role as sulfur adsorbent in hybrid catalyst. Hydrogen spillover between Ni/ZnO and PdPt/USY components facilitates the aromatic hydrogenation and DBT HDS. This study proposed that the PdPt/USY–Ni/ZnO hybrid catalyst may be an alternative in the hydrotreatment of diesel fuel.

Full text of DOI:10.1134/S0036024418110213

ISSN 0036-0244, Russian Journal of Physical Chemistry A, 2018, Vol. 92, No. 11, pp. 2148–2153. © Pleiades Publishing, Ltd., 2018.
CHEMICAL KINETICS
AND CATALYSIS
Simultaneous Desulfurization and Hydrogenation of Model Diesel
Fuel over Ni/ZnO–PdPt/USY Hybrid Catalyst1
Lichun Huanga,b,*, Mingxian Duc, Weixing Wangc, Mingxing Tangc, and Hui Gec,**
a Ordos Dalu Institute of Coal Chemical Industry, Ordos, Inner Mongolia, 010320 China
b Synfuels China Inner Mongolia Co., Ltd, Ordos, Inner Mongolia, 010320 China
c State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences,
Taiyuan, Shanxi, 030001 China
* e-mail: huanglichunno1@163.com
** e-mail: gehui@sxicc.ac.cn
Received August 24, 2017
Abstract—The clean production requires deep desulfurization to meet stringent environmental specification
and aromatics hydrogenation to improve the quality of transport fuels. To achieve this objective, hybrid cat-
alyst was prepared by mixing of PdPt/USY with Ni/ZnO powders. It was found that the hybrid showed higher
activity and stability to hydrodesulfurization (HDS) of dibenzothiophene (DBT) and hydrogenation of
tetralin than Ni/ZnO or PtPd/USY counterparts. PdPt/USY containing catalysts exhibited high trans/cis
ration of decalin, this can be attributed to the isomerization on the acid sites of USY and the reduced inter-
action between olefinic intermediates with PdPt bimetals. The hybrid catalyst also had high hydrogenation
ability and stability to bulky aromatics of pyrene with the existence of DBT. The XRD, XPS, and BET char-
acterizations revealed that PdPt/USY is responsible for DBT HDS, HYD and isomerization whereas
Ni/ZnO play supporting role as sulfur adsorbent in hybrid catalyst. Hydrogen spillover between Ni/ZnO and
PdPt/USY components facilitates the aromatic hydrogenation and DBT HDS. This study proposed that the
PdPt/USY–Ni/ZnO hybrid catalyst may be an alternative in the hydrotreatment of diesel fuel.
Keywords: hydrogenation, desulfurization, sulfur tolerance, PdPt catalyst, Ni/ZnO catalyst
DOI: 10.1134/S0036024418110213
INTRODUCTION
ability to aromatics which can improve the fuel quality
in some extent [15, 16].
Traditional CoMo or NiMo catalysts have long
been applied in the hydrotreating process to achieve
hydrodesulfurization and hydrogenation of refining
oil streams. However, more stringent regulations
reducing the content of sulfur and aromatics in fuels
have brought increasing attention to the novel process
technologies [1]. Recently, Ni/ZnO has been found to
be a promising absorbent for the reactive adsorption
desulfurization (RADS) of transport fuels [2, 3].
Owing to no H2S gas release, its inhibition effect can
be avoided [4, 5]. Thus, the sulfur content in the gaso-
line or diesel can be decreased to very low level [6–9].
In the RADS process, Ni-rich particles are considered
to be the active sites for desulfurization of sulfur con-
taining compounds, the ZnO adsorbent component
accepts the sulfur from the sulfided Ni species and
regenerates the Ni active sites [10, 11]. This Ni/ZnO
system has been extensively used in the RADS of gas-
oline, kerosene and diesel etc. [12–14]. Furthermore,
the Ni/ZnO adsorbent showed some hydrogenation
The noble metal catalyst features the saturation of
aromatics under relative low temperature [17]. Many
reports [18–21] have demonstrated the superior
hydrogenation ability of bimetallic PdPt catalysts with
some sulfur tolerance, particularly when prepared on
acidic zeolites. Many factors, such as the preparation
details, size of PdPt particles and sulfidation of noble
metals, influences the sulfur tolerance and hydroge-
nation ability of PdPt catalyst [22–24]. And the nar-
row pore size of zeolites confines the deep hydrogena-
tion of bulky aromatics [25].
In this study, we combined the merits of the
Ni/ZnO adsorbent and PdPt catalyst to achieve the
simultaneous desulfurization and hydrogenation of
model diesel fuels. Firstly, a series of Ni/ZnO catalysts
calcined and reduced at different temperatures were
tested for RADS of dibenzothiophene (DBT) and the
hydrogenation of tetralin. And the Ni/ZnO with the
best performance was mixed with PdPt/USY to pre-
pare hybrid catalyst for improving the hydrogenation
and desulfurization of model diesel fuel. XRD, XPS,
1
The article is published in the original.
2148

SIMULTANEOUS DESULFURIZATION AND HYDROGENATION
Catalyst Characterization
2149
and BET characterization were conducted to illustrate
the synergy of Ni/ZnO adsorbent with PdPt/USY cata-
lyst.
Powder X-ray diffraction (XRD) patterns were col-
lected on a RIGAKU D/max-rB diffractometer, using
CuKα radiation. The X-ray photoelectron spectros-
copy (XPS) was conducted with a Kratos Axis Ultra
DLD spectrometer employing a monochromated
AlKα X-ray source. Binding energy (Eb) value was cal-
ibrated with the signal of contamination carbon at
EXPERIMENTAL
Catalyst Preparation
The Ni/ZnO sample was prepared by co-precipita- 284.5 eV. XPSPEAK41 software was employed for data
processing. The Shirley-type background was sub-
tracted and the experimental curve was fitted to a mix-
ture of Gaussian (80%) and Lorentzian (20%) pro-
files. The BET surface area and pore parameters of
catalysts were determined by nitrogen adsorption at
77.4 K with ASAP 2020 instrument (Micromeritics,
USA). The samples were degassed at 200°C and 5 Pa
for 4–5 h prior to the measurement.
tion from Ni(NO3)2 · 6H2O and Zn(NO3)2 · 6H2O
solution with Na2CO3 (1 M) solution under vigorous
stirring at 80°C. The precipitate was filtrated and
washed six times with distilled water in order to
remove the residual sodium, and then washed another
time with ethanol. After that, the precipitate was dried
at 120°C overnight and then calcined in air for 4 h at
260, 300, 350, and 400°C, respectively. The catalysts
were denoted as Ni/ZnO-x, where the x represents the
calcined temperature. The Ni content in Ni/ZnO sam-
ple is 7.0 wt %, which is verified by inductively coupled
plasma atomic emission spectrometry (ICP-AES).
RESULTS AND DISCUSSION
Figure 1 shows the conversion of tetralin, ratio of
trans-decalin/cis-decalin and conversion of DBT over
various catalysts. Among Ni/ZnO series, Ni/ZnO-300
showed the highest activity for tetralin hydrogenation
(Fig. 1a). However, Ni/ZnO-300 and Ni/ZnO-350
deactivated totally at about 56 h although they exhib-
ited higher catalytic activities than PdPt/USY at initial
stage. Ni/ZnO-400 and Ni/ZnO-260 deactivated even
more quickly, losing activity at 24 and 36 h, respec-
tively. The quick deactivation can be ascribed to the
high affinity of Ni metal to sulfur [26]. The PdPt sup-
ported on USY presented high conversion of tetralin
and catalytic stability, in agreement with the reports in
the literature [26–28]. And the PdPt/USY–Ni/ZnO
hybrid catalyst had the highest tetralin conversion and
stability among all samples.
The PdPt catalyst was obtained through the wet co-
impregnation with aqueous solution of H2PtCl6
·
6H2O and PdCl2 of USY zeolite. The impregnation
lasted for 20 h; after that, the sample was dried at
110°C for 12 h and calcined at 450°C for 4 h, which was
called PdPt/USY. The PdPt bimetallic content is
1.2 wt % and the Pd/Pt mole ratio is 4. The hybrid cat-
alyst was obtained by mechanical mixing the same
weights of PdPt/USY and Ni/ZnO-300 powders and
tableting, designated as PdPt/USY-Ni/ZnO.
Catalytic Activity Measurements
The catalytic test was performed in a micro fixed-
bed flow reactor with an inner diameter of 6.0 mm.
About 0.2 g 40–60 mesh catalyst was mixed with 0.3 g
quartz and then was loaded in each run. Before the
test, the catalyst was reduced at a hydrogen flow of
65 mL min–1 and 4.0 MPa for 4 h. For Ni/ZnO series,
the reduction temperature was the same as the calci-
nation temperature. The PdPt/USY and PdPt/USY–
Ni/ZnO catalysts were reduced at 300°C. After reduc-
tion, the reactor was cooled down to the 260°C. Then
the feedstock was pumped into the reactor. The feed-
stock consists of tetralin (30.0 wt %), n-nonane
(69.8 wt %) and dibenzothiophene (DBT) (S =
300 ppm). Typical reaction conditions were 4.0 MPa,
260°C, WHSV of 11.7 h–1 and H2/oil mole ratio of
1000. The liquid products were collected and analyzed
with an FID gas chromatograph (Shimadzu GC-2010)
equipped with an Rtx-1 column (0.25 mm × 60 m). For
investigating the hydrogenation for bulky aromatics,
pyrene (2.0 wt %) solved in n-nonane with addition of
DBT (S = 300 ppm) was used as feedstock.
Hydrogenation of tetralin can produce trans- or
cis-decalin. The trans/cis ratio of decalin over
PdPt/USY catalyst decreased from 7.0 to 1.1 when the
conversion of tetralin decreased from 99 to 55%
(Fig. 1b). Schmitz et al. [29] suggested that the
reduced interaction between olefinic intermediates
and PdPt bimetals favors trans-decalin, i.e., higher
trans-decalin/cis-decalin selectivity. They found in
naphthalene hydrogenation that selectivity for trans-
decalin increased with the number of weak acid sites of
HY. As for Ni/ZnO series, however, the trans/cis
selectivity of decalin is never over 1.6 no matter how
high the conversion of tetralin is. Apart from the defi-
ciency of acid sites, a different path of hydrogenation
may be present. It is found that the evolutions of
tetralin conversion and trans-decalin/cis-decalin
selectivity of PdPt/USY–Ni/ZnO hybrid are more
like those of PdPt/USY catalyst than those of
Ni/ZnO-300. The high trans/cis ration of decalin over
PdPt/USY containing catalysts can be attributed to
the isomerization on the acid sites of USY, as well as
RUSSIAN JOURNAL OF PHYSICAL CHEMISTRY A Vol. 92 No. 11 2018

2150
LICHUN HUANG et al.
(a)
80
100
90
80
40
PdPt/USY
PdPt-Ni/ZnO
0
8
4
0
20
40
60
80
100
(b)
Time on stream, h
PdPt/USY
PdPt−Ni/ZnO
Ni/ZnO-260
Ni/ZnO-300
Ni/ZnO-350
Ni/ZnO-400
Fig. 2. Conversion of pyrene over PdPt/USY and PdPt–
Ni/ZnO catalysts. 4.0 MPa, 260°C, WHSV = 11.7 h
oil/H = 1000.
–1
,
2
of PdPt bimetals is decreased by the RADS on
Ni/ZnO absorbent, thus the hybrid catalyst presented
high activity and stability for hydrogenation and HDS.
0
(c)
100
The small pore size of USY zeolite support inhibits
the large molecules access to the noble active metals.
To investigate the steric hindrance effect of polycyclic
aromatics, the hydrogenation of pyrene was con-
ducted with DBT (300 ppm S) in the model fuel. The
results are presented in Fig. 2. PdPt/USY–Ni/ZnO
showed higher conversion of pyrene and catalytic sta-
bility than its counterpart PdPt/USY. Due to the cir-
cular 12-membered ring windows of 0.74 nm in USY
zeolite inhibiting the diffusion of bulky aromatics in
inner pores, thus the hydrogenation of pyrene
occurred only on the extra surface of zeolite. On the
contrary, Ni/ZnO-300 component had large pore (see
below); pyrene could diffuse in the inner pore and
might also be hydrogenated on the Ni metal.
80
60
10
30
50
Time on stream, h
70
90
Fig. 1. Conversion of tetralin (a), the ratio of trans- and
cis-decalin (b) and conversion of DBT (c) over catalysts;
4.0 MPa, 260°C, WHSV = 11.7 h , oil/H = 1000.
–1
2
Figure 3 shows XRD patterns of the spent catalysts.
With Ni/ZnO series, only ZnS and ZnO phases are
observed, suggesting that sulfur had been transferred
from nickel sulfide to zinc oxide. The size of ZnS crys-
tallites in the direction normal to the (110) planes at
47.8° increased from 10.2 to 11.8 nm when the calcina-
tion temperature increased from 260 up to 400°C, as
calculated by the Scherrer equation [29]. The absence
of peaks of metallic nickel, nickel sulfide or nickel
oxide proposes a well dispersion of Ni species. With
PdPt/USY catalyst, the characteristic patterns of Y
zeolite support are observed. However, phases involv-
ing in Pd or Pt species are not detectable, indicating
that noble metals were sufficiently dispersed on the
surface of USY. The PdPt/USY–Ni/ZnO hybrid
shows the features of both PdPt/USY and Ni/ZnO but
with less strength.
the reduced interaction between olefinic intermedi-
ates with PdPt bimetals [30, 31].
As shown in Fig. 1c, all sample showed high desul-
furization activity of DBT at initial stage. However,
the stability presented apparent differences. During
reaction period, PdPt/USY–Ni/ZnO hybrid and
PdPt/USY catalyst keeps better stabilities. The stabil-
ity is in the sequence of PdPt/USY–Ni/ZnO >
PdPt/USY > Ni/ZnO-300 > Ni/ZnO-260 > Ni/ZnO-
350 ≈ Ni/ZnO-400. It notes that the PdPt/USY–
Ni/ZnO hybrid catalyst showed no deactivation in
90 h reaction time.
It is observed that the change trends of PdPt/USY
and hybrid PdPt/USY–Ni/ZnO are similar in all the
reactions. Meanwhile the performance of hybrid is
better than that of PdPt/USY. The hybrid shows 10–
20% higher tetralin conversion. It has higher trans/cis
selectivity, especially in initial stage. For DBT HDS,
the hybrid is more stable. We deduce that the hydroge-
nation of tetralin and RADS of DBT occurs on the
Figure 4 shows XPS spectra of (a) Ni 2p3/2, (b)
Zn 2p3/2 and (c) S 2p regions of the spent Ni/ZnO cat-
alysts. The Ni 2p spectra were fitted using doublets for
the 2p3/2 and 2p1/2 separated by a spin–orbit splitting of
about 17.8 eV. The Ni 2p doublet with Ni 2p3/2 at
PdPt/USY and Ni/ZnO respectively. The S poisoning 852.5 0.1 eV is a characteristic pattern of metallic Ni
RUSSIAN JOURNAL OF PHYSICAL CHEMISTRY A
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SIMULTANEOUS DESULFURIZATION AND HYDROGENATION
2151
Ni 2p
∇
∇
(a)
∇
∇
∇
∇
PdPt/USY
Ni/ZnO-260
PdPt−Ni/ZnO-350
*
Ni/ZnO-400
Ni/ZnO-300
*
*
o
Ni/ZnO-350
*
o
o
o
o
*
NI/ZnO-350
Ni/ZnO-400
Ni/ZnO-300
Ni/ZnO-260
20
40
60
80
2θ, deg
885 880 875 870 865 860 855 850
E, eV
Fig. 3. XRD patterns of spent catalysts. (*) ZnS; (o) ZnO;
( ) Y zeolite.
ꢀ
(b)
Zn 2p2/3
Ni/ZnO-260
or NiS (Fig. 4a) [32]. The doublet with Ni 2p3/2 at
855.8 0.2 eV is the feature of NiO, which can be
attributed to incomplete reduction of Ni oxide or part
oxidation of Ni metal by exposing sample to air [32].
The appearance of strong satellites at higher binding
energy indicates the presence of electronic relation.
The spectra of Zn 2p3/2 were deconvoluted into two
peaks at 1021.3 0.1 and 1022.2 0.3 eV, representing
ZnS and ZnO, respectively (Fig. 4b) [33]. The main
difference in the Ni/ZnO-260 and Ni/ZnO-300 cases
as compared to the Ni/ZnO-350 and Ni/ZnO-400
cases is a significant increase in the concentration of
ZnS species. This proposes that the ZnS was enriched
on the surface at low temperature. At high tempera-
ture, the H2S was prone to penetrate into bulky phase.
Curve fitting spectra of S 2p (Fig. 4c) shows two dou-
blets with S 2p3/2 located at 161.1 0.2 and 161.7
0.2 eV, respectively. It is suggested that Ni metal and
ZnO were sulfided simultaneously. However, it is
impossible to clearly differentiate NiS from ZnS due to
the overlap of their binding energies [34].
Ni/ZnO-300
Ni/ZnO-350
Ni/ZnO-400
1026
1024
1022
1020
1018
E, eV
(c)
S 2p
Ni/ZnO-260
Ni/ZnO-300
Ni/ZnO-350
Table 1 lists the BET surface area, pore volume and
average pore diameter of USY support, PdPt/USY,
and Ni/ZnO calcined at various temperatures. The
surface area and pore volume decreases from 679 to
551 m2 g–1 and from 0.36 to 0.30 cm3 g–1, respectively
after the USY zeolite impregnated with Pd and Pt
bimetals. For Ni/ZnO series, upon increasing the cal-
cination temperature from 260 to 450°C, the surface
area and pore volume increase firstly and then
decrease gradually with the maximum at 300°C. And
the pore size changed in opposite direction. This pro-
poses that the pore structures can be well formed at
about 300°C. When increasing calcination tempera-
ture over 350°C, collapse of pores and sinter of crystal-
Ni/ZnO-400
164
165
163
162
161
160
E, eV
Fig. 4. (a) Ni 2p, (b) Zn 2p , and (c) S 2p XPS spectra of
spent Ni/ZnO catalysts calcined and reduced at various
temperatures.
3/2
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LICHUN HUANG et al.
Table 1. BET analysis of catalysts and support
ACKNOWLEDGMENTS
SBET, m2 g–1 Vtotal, cm3 g–1
The authors are grateful for the National Natural
Science Foundation of China (21473231 and
21603256).
Daverage, nm
Catalyst
USY
PtPd/USY
Ni/ZnO-260
Ni/ZnO-300
Ni/ZnO-350
Ni/ZnO-400
679
551
86
0.36
0.30
0.29
0.46
0.46
0.41
2.1
2.1
13.5
10.8
17.9
24.0
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