One-pot synthesized hierarchical zeolite supported metal nanoparticles for highly efficient biomass conversion

Article abstract of DOI:10.1039/c5cc06212h

Hierarchically porous zeolite supported metal nanoparticles are successfully prepared through a base-assisted chemoselective interaction between the silicon species on the zeolite crystal surface and metal salts, in which in situ construction of mesopores and high dispersion of metal species are realized simultaneously.

Full text of DOI:10.1039/c5cc06212h

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DOI: 10.1039/C5CC06212H
Graphic Abstract
(I)
Ni precursor + Base
Hydrothermal Process
ZSM-5
Ni3Si2O5(OH)4
SiO2
Ni NPs
One-pot synthesis of hierarchical zeolite supported metal nanoparticle catalysts
are realized through a base-assisted chemoselective interaction.

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DOI: 10.1039/C5CC06212H
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One-Pot Synthesized Hierarchical Zeolites Supported Metal
Nanoparticles for Highly Efficient Biomass Conversion†
Received 00th January 20xx,
Accepted 00th January 20xx
Darui Wang, Bing Ma, Bo Wang, Chen Zhao* and Peng Wu*
DOI: 10.1039/x0xx00000x
www.rsc.org/
Hierarchically porous zeolites supported metal nanoparticles are and nickel nitrate by using ethylene glycol as either a solvent
successfully prepared through a base-assisted chemoselective or a ligand for nickel.14 Unfortunately, the nickel particle size
interaction between the silicon species on zeolite crystal surface becomes larger than 10 nm when its loading is over 10 wt%.15
and metal salts, in which in-situ construction of mesopores and The deposition-precipitation (DP) method developed by Geus
high dispersion of metal species are realized simultaneously.
et al.16 is promising to achieve a high metal dispersion at
relatively high loadings. In order to improve the catalytic
properties and to shorten the preparation time, the amount of
metal compound added in initial solution often greatly exceeds
that of actually loaded on supports.6,17-19 Therefore, it is highly
expected to develop eco-efficient approaches for achieving
highly dispersed and stable metal NPs at high loadings.
Hierarchical materials are known to serve as good supports
for dispersing and stabilizing metal NPs or other coordinate
compounds. Recently, great efforts have been devoted to the
design and controlled fabrication of hierarchical materials with
novel structures.20-25 For instance, Jin et al. once prepared
copper-silicate hollow fibers with a ultra small nanotube-
assembled and double-walled structure.26 The as-prepared
hollow fibers possess mesopores centered at 3.4 nm and a
high surface area, and they exhibit an excellent performance
as an ideal support for noble metal catalysts. Recently, we
have prepared core-shell structured ZSM-5@mesosilica and
further incorporated Pt NPs into the mesosilica shell, resulting
in an effective catalyst towards n-hexadecane hydrocracking.27
Generally, the preparing procedures for hierarchical materials
are inevitably complicated, and additional steps are required
to confine the metal NPs in mesopores.
Synthetic zeolites with well-defined crystalline structures,
unique microporosity and high surface areas have attracted
technological and scientific research attentions in the
adsorption, separation and catalysis fields.1 Supporting metal
nanoparticles (NPs) on zeolites, preferably with stable
characters and uniform nanosize, leads to useful catalysts for
F-T synthesis,2 CO oxidation,3 hydroisomerization4 and
hydrodeoxygenation etc.5-7 It is well acceptable that the
physiochemical properties and catalytic activity of NPs are
superior to those of bulk metals. However, smaller NPs tend to
aggregate because of a large surface area-to-volume ratio,
which greatly limits their actual applications.8-10 The
preparation method is thus an important factor dominating
the catalytic properties and performances of metal NPs
catalysts.
Wetness impregnation (IM) is
a simple preparation
technique widely used in the industrial process. However,
metal-based catalysts prepared by conventional IM procedure
encounters the drawbacks of large and non-uniform metal
particles as the metal-support interaction is relatively weak for
silica-based zeolite supports,11 leading to low metal dispersion
and unsatisfied catalytic activity.6,12 On the other hand, the
ion-exchange process can obtain small metal particles with a
higher dispersion, but the metal loading amount is limited by
the exchange capacity of zeolites.13 Metal-based catalyst has
also been prepared by sol-gel method. For example, Ueno and
co-workers prepared Ni/SiO2 from tetraethoxysilane (TEOS)
Herein, we communicate a facile route for synthesizing
hierarchical ZSM-5 supported Ni NPs starting from
conventional crystals. The construction of flower-like
hierarchical ZSM-5 structure and incorporation of highly
dispersed and stable Ni active sites are accomplished in one
pot. The obtained Ni/ZSM-5 catalysts are highly efficient to the
hydrodeoxygenation of bioacids to liquid fules.
As illustrated in Scheme 1, in the first step, the flower-like
nickel silicate precursors were chemically formed and coated
on the polycrystalline particles of zeolite via base-assisted
chemoselective interaction with corresponding metal source.
Shanghai Key Laboratory of Green Chemistry and Chemical Process, School of
Chemistry and Molecular Engineering, East China Normal University , North
Zhongshan Rd. 3663, Shanghai 200062, China
E-mail: pwu@chem.ecnu.edu.cn, czhao@chem.ecnu.edu.cn;
Fax: (+)86-21-62232292
†Electronic Supplementary Information (ESI) available: Details of experimental
procedures and material characterization. See DOI: 10.1039/x0xx00000x
This journal is © The Royal Society of Chemistry 20xx
J. Name., 2013, 00, 1-3 | 1
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nickel silicate (Ni3Si2O5(OH)4, JCPDS No. 49-1859).29 Fig. 1c
View Article Online
displays the XRD pattern of Ni/ZSM-5DaOfIt:e10r.1r0e3d9/uCc5tCioCn0.62T1h2He
weak peaks centered at 44.5o and 51.8o, corresponding to the
[111] and [200] planes of cubic Ni (JCPDS No. 04-0850),30 were
observed with the disappearance of nickel silicate phase. The
results indicated that the Ni species in layered nickel silicate
were converted into metal Ni particles by H2 reduction at high
temperature. FT-IR spectroscopy was utilized to detect the
(I)
Ni precursor + Base
Hydrothermal Process
formed functional groups.
A new band emerged for
NiSiO2/ZSM-5 at around 670 cm-1 (Fig. S3, ESI†), which is
ascribed to the Si-O-Ni stretching vibrations.31 This further
verified the formation of nickel silicate precursors after
hydrothermal reaction. This band disappeared for Ni/ZSM-5
after H2 reduction, reasonably because that the Si-O-Ni
ZSM-5
Ni3Si2O5(OH)4
SiO2
Ni NPs
Scheme 1 Schematic illustration of the preparation procedures for Ni nanoparticles linkages were broken instead of forming Ni NPs.
supported on hierarchical ZSM-5 zeolite crystals.
The morphology, structure, and composition of the samples
obtained at different stages were investigated by various
This process involved the selective and partial dissolving of characterization techniques. The SEM image shows that the
silica species off the ZSM-5 crystals to form silicate anions and pristine ZSM-5 was of the polycrystalline particles with a
then in situ interaction with the nickel cations in solution to relatively smooth surface and a regular size of 1 - 2 μm (Fig.
form the layered nickel silicate, giving rise to a composite 2a). After hydrothermal treatment with Ni source, the as-
material NiSiO2/ZSM-5. The hydrothermal reaction between fabricated NiSiO2/ZSM-5 precursors retained almost the
SiO2 and Ni2+ took place as follows: 2SiO2 + 3Ni2+ + 5H2O = original crystal shape and size (Fig. 2b). Careful observation by
Ni3Si2O5(OH)4 + 6H+.28 Secondly, the nickel silicate precursors
underwent decomposition and reduction in a hydrogen
atmosphere. The remaining SiO2 matrixes still maintaining
flower-like structure, whereas highly dispersed Ni NPs were
immobilized therein, obtaining Ni/ZSM-5 catalyst. This novel
host-guest method is featured by the simultaneous
construction of hierarchical zeolite structure and confined
metal NPs.
a
b
500 nm
500 nm
2.5 μm
2.5 μm
Well-structured NiSiO2/ZSM-5 materials were prepared
readily by hydrothermal reaction under optimal temperature
and time of 120 oC and 3 h (Fig. S1 and S2, ESI†). The
supporting of highly dispersed Ni NPs on hierarchical ZSM-5 by
this novel method has been traced with the XRD patterns and
FT-IR spectra. The XRD pattern of the pristine ZSM-5 was
characteristic of a typical MFI structure (Fig. 1a). After the
hydrothermal treatment in nickel acetate-containing solution,
the resultant NiSiO2/ZSM-5 showed additional XRD diffractions
around 34.1o, 36.7o and 60.5o in high angle region (Fig. 1b),
which are indexed as the [200], [202] and [060] planes of
0.452 nm
(110)
c
d
Ni3Si2O5(OH)4
5 nm
ZSM-5
20 nm
200 nm
e
f
Ni (111)
0.204 nm
1 nm
Ni3Si2O5(OH)4
NiNPs
Ni NPs
ZSM-5
X 6
c
200 nm
10 nm
X 6
X 6
g
b
a
JCPDS No.49-1859
10
20
30
40
50
60
70
80
2Theta (deg.)
Fig. 2 SEM images of pristine ZSM-5 (a) and NiSiO2/ZSM-5 (b); TEM images of
Fig. 1 XRD patterns of the pristine ZSM-5 (a), NiSiO2/SM-5 (b), Ni/ZSM-5 (c) and
NiSiO2/ZSM-5 (c, d) and Ni/ZSM-5 (e, f); and elemental mapping of NiSiO2/ZSM-5
(g).
nickel silicate.
2 | J. Name., 2012, 00, 1-3
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the high-magnification SEM image indicated that the surface of inset, ESI†). This synthetic method has an obvious advantage
View Article Online
these precursors was no longer smooth but composed of that the monodispersed Ni NPs do not cDluOmI:p10t.o10g3e9t/hCe5Cr Ca0t6u2l1t2rHa
numerous nanosheets (Fig. 2b, inset). The TEM image (Fig. 2c) high loadings.
clearly displays that the precursors possessed a typical
The N2 adsorption/desorption isotherms and pore size
core/shell like structure, with flexible nanosheets uniformly distribution are shown in Fig. S11 (ESI†). After introducing Ni
coating on the ZSM-5 crystals. A representative high-resolution NPs, Ni/ZSM-5 showed the isotherms combining type I and
TEM image indentified clearly that the composite materials type IV characters, indicating the presence of both micropores
contained the flower-like nanosheets and the crystalline ZSM-5 and mesopores. The pore size distribution showed that
crystal, confirming the presence of a core/shell structure (Fig. Ni/ZSM-5 possessed the mesopores with 5 - 30 nm diameters.
2d). The inset in Fig. 2d and Fig. S4 (ESI†) show the enlarged The mesopores are mainly ascribed to the disordered
image of nanosheets, indicating they possessed a layered assembly of the flexible SiO2 matrixes. The mesopore surface
structure. The distance of the adjacent lattice fringes was areas increased from 25 m2 g-1 to 126 m2 g-1 and mesopore
determined to be about 0.452 nm and 0.153 nm, volumes increased from 0.08 cm3 g-1 to 0.29 cm3 g-1 when 30.6
corresponding well to the d110 and d060 spacing of wt% Ni was incorporated into ZSM-5 (Table S1, ESI†). These
Ni3Si2O5(OH)4 (JCPDS No. 49-1859), respectively. Elemental novel materials, with confined space and enhanced mass
mapping by energy-dispersive X-ray spectroscopy (EDX) transfer rate, would have potential applications as bifunctional
verified that the elements Si, Al, O, Ni were homogeneously catalysts.
distributed throughout the whole single particle (Fig. 2g). This
The acidity of pristine ZSM-5 and Ni/ZSM-5 was investigated
implies that a high dispersion of Ni NPs would be achieved by pyridine-IR (Fig. S12, ESI†). Compared with ZSM-5, Ni/ZSM-5
after thermal reduction. In addition, a similar hydrothermal possessed slightly lower concentration of Brønsted acid sites
treatment without using Ni source was also done, Fig. S5 (ESI†) and higher concentration of Lewis acid sites. Those ionic Ni
shows that the treated ZSM-5 have the same morphological species, partially unreduced as evidenced by H2-TPR
features and textural properties as the pristine ZSM-5, which investigation (Fig. S13, ESI†), are speculated to be the potential
means the microporous characteristics of the core.
Lewis acid sites.33 The state of Al was also investigated by 27Al
The TEM images (Fig. 2e) and SEM images (Fig. S6, ESI†) MAS NMR (Fig. S14, ESI†), the microenvironment of Al became
indicated that the reduced samples of Ni/ZSM-5 also showed a more asymmetric in coordination states after incorporating
good core/shell structure, as the remaining silica parts still nickel content.
existed as shell matrixes after decomposition of nickel silicate
The Ni/ZSM-5 catalyst was evaluated in the conversion of
precursors. The spherical Ni NPs were dispersed uniformly on biomass to fuel using hydrodeoxygenation of stearic acid with
the SiO2 matrixes, just like “diamond on the beach” (Fig. S7, H2 at 260 oC and 4 MPa. Fig. 3a presents the conversion of the
ESI†). In the HRTEM image (Fig. 2f), the spherical Ni NPs of stearic acid over Ni/ZSM-5 with different Ni loadings. The
about 5 nm can be easily observed. The distance of the conversion of stearic acid increased from 39.2% to 86.1% at 60
adjacent lattice fringes in NPs was determined to be about min, as the Ni loading was increased from 7.6 wt% to 30.6 wt%.
0.204 nm, corresponding well to the d111 spacing of cubic Ni Accordingly, the reaction rate increased from 34 to 44, 69 and
(JCPDS No. 04-0850).32
76 mmol g-1 h-1 (Table S3, ESI†). A kinetic curve revealed that
To demonstrate the synthetic controllability, the products the reaction took place proportionally to the time, giving the
were synthesized with different nickel contents, corresponding n-C18 alkanes as major products (Fig. S15, ESI†).
to theoretical loading amounts of 7.5, 10.0, 20.0 and 30.0 wt%.
90
80
70
60
50
40
30
20
10
0
90
80
70
60
50
40
30
20
10
0
(b)
(a)
ICP analyses indicated the Ni contents actually loaded on
zeolite were 7.6, 10.3, 20.4 and 30.6 wt%, respectively. Thus,
this method gave a utilization efficiency of nickel source close
to 100 % and easily controlled the Ni loading amounts in a
relatively wide range.
Fig. S8 (ESI†) shows the SEM images of NiSiO2/ZSM-5 with
different nickel contents. At lower Ni loadings of 7.6 wt% and
10.3 wt%, although small amounts of flower-like nanosheets
were assembled on the ZSM-5 crystals, the rough surfaces
were already observed clearly. Certainly, larger amount
nanosheets were formed when the nickel contents reached
20.4 wt% and 30.6 wt%. Fig. S9 (ESI†) gives the corresponding
SEM images of Ni/ZSM-5. The amounts of remaining SiO2
matrixes increased with an increasing nickel content, as more
nickel silicate precursors were decomposed and reduced. The
HRTEM images verified that ultrafine Ni NPs were well
dispersed among the SiO2 matrixes independent of high nickel
C17
iso-C18
n-C18
C18-OH
C17
iso-C18
n-C18
C18-OH
Conv.
Conv.
5
10
15
20
25
30
5
10
15
20
25
30
Content of nickel (wt%)
Content of nickel (wt%)
78.1%
(c)
80
60
40
20
0
80
60
40
20
0
(d)
74.6%
72.3%
68.2%
22.1%
1
19.0%
2
16.8%
3
13.7%
4
1
2
3
4
Number of cycles
Number of cycles
Fig. 3 Yield and conversion for stearic acid hydrodeoxygenation over Ni/ZSM-5 (a)
and IM-Ni/ZSM-5 (b) with different Ni contents; stability tests for the Ni/ZSM-5 (c)
and IM-Ni/ZSM-5 (d) catalysts, Ni contents are about 20.4 wt% and 20.2 wt%,
loadings (Fig. S10, ESI†). The particle size was still centered at respectively. Reaction conditions: 5.0 g stearic acid, 0.2 g catalyst, 80 mL dodecane,
260 oC, 4 MPa H2, 60 min, stirring at 600 rpm.
about 6.0 nm even at a high loading of 30.6 wt% (Fig. S10d,
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J. Lu, C. Aydin, N. D. Browning and B. C. Gates, Angew. Chem.
IM-Ni/ZSM-5 with different Ni contents was synthesized by
wetness impregnation for comparison. It is obvious that the
catalytic activity of IM-Ni/ZSM-5 was much lower than that of
Ni/ZSM-5 when compared at the same Ni loadings (Fig. 3b).
The textural properties and the size of Ni NPs were considered
to contribute the high catalytic activity. Compared with
Ni/ZSM-5, IM-Ni/ZSM-5 showed no increase in mesopore
surface area or mesopore volume (Fig. S16 and Table S2, ESI†)
and possessed larger Ni NPs with an average diameter of 30
nm (Fig. S17, ESI†). The CO chemisorption measurement
evidenced that Ni/ZSM-5 contained more highly dispersed Ni
NPs than IM-Ni/ZSM-5 (Table S3, ESI†).
In a following step, the stabilities of Ni/ZSM-5 and IM-
Ni/ZSM-5 were checked by recycling the catalyst. No notable
changes in activity were observed over four cycles for Ni/ZSM-
5 (Fig. 3c), the stearic acid conversion dropped slightly from
78.1% to 68.2%. However, IM-Ni/ZSM-5 lost about 40% of its
initial activity after four reaction runs (Fig. 3d). The activity loss
was presumed mainly due to the aggregation of Ni NPs during
the successive reaction. For the reused Ni/ZSM-5 catalyst, the
morphology maintained well, and the average diameters of Ni
particles were still much smaller than that of the reused IM-
Ni/ZSM-5 (Fig. S18, ESI†). To undertake a deeper investigation
into this issue, the stability was further checked by treating the
catalysts at 800 oC for 24 h in a flow of H2. Ni/ZSM-5
demonstrated a much higher stability against sintering with
slight increase of Ni particles size (Fig. S19a, ESI†).
Importantly, the synthetic strategy described above is quite
general. We have successfully prepared other bifunctional
catalysts by simply varying types of zeolites or metal salts in
the hydrothermal reaction, such as Ni/MOR, Ni/Beta, Ni/HY,
Ni/MCM-22, Cu/ZSM-5 and Co/ZSM-5 (Fig. S20-22, ESI†).
In summary, we have developed a facile route for preparing
well-dispersed metal NPs supported on hierarchical zeolites, in
which mesopores and metal active sites can be incorporated in
one pot. The as prepared Ni/ZSM-5 catalysts exhibit excellent
catalytic activity and stability in the hydrodeoxygenation of
bioacid. The mesoporous SiO2 matrixes effectively prevent the
Ni NPs from sintering. In particular, the synthetic strategy
provides an useful idea for controllable supporting of other
metal NPs on different zeolites, and gives rise to promising
bifunctional catalysts for industrial processes, such as F-T
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Int. Ed., 2012, 51, 5842.
DOI: 10.1039/C5CC06212H
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