Advanced Powder Technology 29 (2018) 1112–1118

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Advanced Powder Technology

journal homepage: www.elsevier.com/locate/apt

Original Research Paper

Preparation of high silica microporous zeolite SSZ-13 using solid waste

silica fume as silica source
Yuanhui Wang a, Jieyu Chen a,b,⇑, Xinrong Lei a,b,⇑, Yuujie Ren a, Ji Wu a
a
Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430074, PR China
b
Engineering Research Center of Nano-Geo Materials of Ministry of Education, China University of Geosciences, Wuhan 430074, PR China

a r t i c l e i n f o a b s t r a c t

Article history: Silica fume (SF) is a kind of solid waste that produced in the process of industrial silicon smelting. The
Received 6 April 2017 disposal of SF for environmental problem is of great urgency. Here, a facile and novel one-step approach
Received in revised form 14 December 2017 of high silica microporous materials SSZ-13 (SF-SSZ-13) were hydrothermally synthesized using silica
Accepted 1 February 2018
fume (SF) as silica source. This method requires significantly shorter reaction times (48 h) compared to
Available online 13 February 2018
conventional SSZ-13. The as-synthesized SF-SSZ-13 exhibited high purity structure, popcorn-like mor-
phology, and a large BET surface area of 545.74 m2 g 1. Additionally, on the basis of controlled growth
Keywords:
under different hydrothermal times, the formation mechanism of the SF-SSZ-13 outlined for further
Solid waste
Silica fume
extension to other materials. The results on time- and energy-efficient of SF-based preparation of SSZ-
Silica microporous materials 13 pave the way for the reducing the cost of production of raw materials and decreasing environment
SSZ-13 load of solid waste, and also extend the application of silica fume.
Ó 2018 Published by Elsevier B.V. on behalf of The Society of Powder Technology Japan. All rights
reserved.

1. Introduction practical applications of mesoporous silica materials are severely

hampered [11,12]. Therefore, microporous zeolite can fill the gap
Industrial solid waste seriously threatened social and environ- for wide application.
mental stability due to its large quantity of emission, low availabil- SSZ-13, a typical member of the chabazite (CHA) family of
ity and serious pollution. The recycling of solid waste has become a microporous aluminosilicate zeolite, is known to possess a three-
challenge in recent years. Silica fume (SF) is a kind of primary dimensional pore system with large ellipsoidal cages (6.7 10 Å)
industrial solid waste from smoke emission of metallic silicon or that are accessible via 8-membered ring windows (3.8 3.8 Å)
ferrosilicon manufacturing processes, and it exists as non- [13]. Numerous studies had been devoted for the special pore size
crystalline solid powder [1]. SF typically exhibits a light weight, (0.38 nm), showing various applications in CO2/N2 adsorption [14–
spherical morphology, large specific surface area (15–30 m2/g), 16] and superior catalytic performance (such as DeNOx [17–19]
fine grained (particle size < 1um), and high activity [2,3]. Because and propylene production from ethylene, methanol-to-olefin
of these characteristics, SF had excellent pozzolanic properties as [20–22]). The discovery of high-silica chabazite SSZ-13 has
the most extensive additional material that was mainly applied attracted great interest because they exhibit specific thermal and
in concrete and refractory materials [4–6]. According to statistics, acid stabilities, and hence, novel application of this material has
a silicon furnace produced 200–400 kg of silica fume from per been widely investigated [17,23]. Generally, SSZ-13 zeolite can
ton of silicon metal, where equals of 8–15% of the quartz feed be synthesized using a variety of silica precursors, such as sodium
[7]. Such a huge amount of SF results in the waste of resource silicate, silica sol, and tetraethyl orthosilicate [24,25]. However,
and environmental pollution, SF could not be used efficiently and these silica precursors suffer from the cost for chemical regent con-
effectively in virtue of constrains of its applications [8]. More sumption, as well as a mass of hazard waste for chemical regent
recently, potential for using SF as silica source to produce meso- removal. Other silica source like solid waste (coal fly ash, silica
porous silicate materials has become a reality [9,10]. Due to the fume) has shown prospects as favorable substitutes for silica
poor hydrothermal stability of mesoporous silicate materials, the source. Among the several of solid waste, silica fume (SF) consider
as a strong candidates for the synthesis of microporous zeolite
⇑ Corresponding authors at: 388 Lumo Road, 430074 Wuhan, PR China. SSZ-13 owing to the high activity and rich content of SiO2
E-mail addresses: [email protected] (J. Chen), [email protected] (X. Lei). (>95%wt). The use of the microporous materials from solid waste

https://doi.org/10.1016/j.apt.2018.02.001
0921-8831/Ó 2018 Published by Elsevier B.V. on behalf of The Society of Powder Technology Japan. All rights reserved.
Y. Wang et al. / Advanced Powder Technology 29 (2018) 1112–1118 1113

has also adopted as an attractive method due to the economic and deionized water for several times until PH of the filtrate was near
environmental advantages. neutral. The solid filter residue obtained was dried at 105 °C for
In the present work, we reported the preparation and character- 2 h, and then calcined at 550 °C for 5 h to eliminate the organic tem-
ization of SSZ-13 synthesized by using SF as silica source. Various plate. The final product was yield, which was designed as SF-SSZ-13.
techniques (XRD, SEM, FT-IR, Laser-particle-size) were used to
characterize the structure and morphology, and the physicochem-
2.3. Characterization
ical performances were analyzed by chemical composition (XRF),
particle size distribution (PSD) and N2 adsorption-desorption
The chemical composition was detected by X-ray fluorescence
(BET). In addition, the mechanism of zeolite crystallization was
(XRF, AXIOSmAX, PANalytical Netherlands). The crystal structure
considered.
was analyzed by using X-ray diffraction (XRD, D8-FOCUS,
BrokerAXS Germany), whose diffractometer using CuKa radiation
2. Experimental and methods in the 2h range of 5–40°. XRD Rietveld profile refinements of the
structural models and textural analysis were performed with the
2.1. Materials use of Fullprof software. The background profile was edited manu-
ally by choosing 40 points over the pattern and further using a
SF was obtained from blast furnace fly ash of metal silicon smelt- cubicspline interpolation. The peak profiles were modeled using
ing enterprise, and it was used as silica source of zeolite. Sodium a Pseudo-Voigt function, while accounting for asymmetry below
hydroxide (NaOH), aluminum sulfate (Al2(SO4)318H2O), N, N, N- 10° 2h. Only symmetry constraints were used while modeling the
trimethyl-1-adamantanammonium (TMAdOH, 25 wt%) were sup- position of atoms in the unit cell. All trigonal positions were mod-
plied by Sinopharm Chemical Reagent Co., Ltd. All chemicals were eled as Si atoms. The thermal parameters (Biso) for all oxygen
analytically pure and used as received without further purification, atoms were grouped during the refinement. The morphology of
and deionized water was used in the whole experiment. as-synthesized samples were characterized by using a field emis-
sion scanning electron microscope (FE-SEM, SU8010, Hitachi
Japan) with an acceleration voltage of 10 kv. The framework for-
2.2. Preparation of SSZ-13 from SF
mation of samples was obtained by Fourier transformation infrared
spectroscopy (FT-IR). FT-IR spectra of the samples were obtained
In the traditional SSZ-13 zeolite synthesis, silica sol was added to
by means of a FT-IR spectrometer (Nicolent iS50, Thermo Scientific
an aqueous solution containing NaOH, Al2(SO4)318H2O as an alu-
American) using KBr pellet technique, whose spectrum was col-
minum source was added to the mixture. Then the mixture was
lected in the range 450–4000 cm 1. The particle size distribution
hydrothermally synthesized at 155 °C for 5 days by using N,N,N-
(PSD) of samples was determined by laser diffraction apparatus
trimethyl adamant ammonium hydroxide (TMAdaOH) as an
(BT-9300HT, DPSA) after the sample dispersed in deionized water
organic-structure-directing agen (OSDA), according to the previous
was ultrasonic treatment. Nitrogen gas adsorption-desorption
report.
experiments were performed at 77 K using an automatic surface
Differently in this study, we use SF as the silica source within
area and porosimetry system (ASAP2020, Micromeritics, America)
shorter time to obtain SSZ-13. The detailed hydrothermal process
and the specific surface area was calculated by the Brunauer-
was shown in Fig. 1. Firstly, Al2(SO4)318H2O and SF were dissolved
Emmet-Teller method (BET).
in deionized water, and the mixture was vigorously stirred for 30
min. Then NaOH was added, followed by the addition of TMAdOH,
where molar ratio of solution was set as SiO2:Al2O3:Na2O:TMA- 3. Results and discussion
dOH:H2O = 80:1:34:7.2:1800. After the mixture was vigorously stir-
ring at room temperature for 2 h, the gel was then transferred into 3.1. The structure and morphology
Teflon-lined stainless-steel autoclave and heated at 155 °C for
48 h. After the above hydrothermal reaction was completed, the 3.1.1. XRD analysis
reaction was cooled to room temperature, and the solid phase was The XRD patterns of the SF and as-synthesized product were
separated from the solution, washed and filtrated thoroughly in shown in Fig. 2. As observed, SF (Fig. 2a) typically exhibited one

Fig. 1. The preparation of SSZ-13 zeolite.

1114 Y. Wang et al. / Advanced Powder Technology 29 (2018) 1112–1118

3.1.3. FTIR study

The FTIR spectra of SF and as-synthesized SSZ-13 were showed
in Fig. 4. The spectra were recorded from 400 cm 1 to4000cm 1. A
broad band in the spectra around 3400 cm 1 were appeared in the
sample of SF and SSZ-13 simultaneously, which was attributed to
the stretching vibration of Si–OH groups and O–H bending vibra-
tion water molecules. The bonds centered at 1628 cm 1 and
1635 cm 1 were due to the stretching vibration of –OH groups in
H2O molecules [29]. In the SF sample (Fig. 4a), the strongest bonds
at around 1118 cm 1, 806 cm 1 and 479 cm 1, represented con-
densed silica. The bands at 1118 cm 1 and 806 cm 1 were attribu-
ted to asymmetric and symmetric stretching vibrations of Si–O–Si
respectively, while the peak at 479 cm 1 was owing to the bending
vibration of O–Si–O [30].
After SF was transformed into the zeolite SSZ-13, some changes
were observed in Fig. 4b. The spectra of SSZ-13 showed a shift to
lower wavenumber (3446.68 cm 1 and 1635.13 cm 1) comparing
with SF for the band at 3435.35 cm 1 and 1628.73 cm 1, which
Fig. 2. XRD patterns of SF, SF-SSZ-13 and standard SSZ-13. were attributed to stretching and bending vibrations of N–H in
the ammonium ions from TMAdaOH [31–33]. The band at
1083 cm 1 showed asymmetric stretching vibration of O–Si–O or
O–Al–O, typically lower frequencies were exhibited that polycon-
Table 1 densation with alternating Si–O and Al–O bonds at lower degree
Lattice parameters of S-SSZ-13 and SF-SSZ-13. [30]. The Al–O symmetric stretching vibration in the SSZ-13 was
corresponded to the band at range of 800 cm 1–700 cm 1. Two
Samples a b c a b c
bands at around 540 cm 1 and 640 cm 1 was responsible for the
S-SSZ-13 13.675 13.675 14.767 90° 90° 120°
formation of double six-membered ring of CHA framework and
SF-SSZ-13 13.5836 13.5836 14.7898 90° 90° 120°
the stretching and bending T–O (T–Si or Al) vibrations of silicon-
oxygen or aluminum-oxide tetrahedrons respectively [34,35].
Accordingly, FT-IR analysis assured the typical vibration frequen-
cies of SSZ-13 and indicated the formation of SSZ-13 from SF.
hump centered at 2h between 35° and 36° (2h), indicating the
amorphous structure of SF. In the case of SF-SSZ-13 (Fig. 2b), it
3.2. Physicochemical properties
showed the characteristic of CHA topology without impure phase,
and the diffraction peaks also matched well with the standard
3.2.1. XRF analysis
diffraction of zeolite SSZ-13 from (1 0 0), (1 0 1), ( 1 1 1),
Table 2 showed the chemical composition of SF and SF-SSZ-13.
(1 1 1), (1 0 2), (0 2 2), (1 3 1) and (3 1 0) crystal planes
SF was mainly composed of SiO2, whose content reached 95 wt%.
(Fig. 2c) [13]. The relative crystallinity of SF-SSZ-13 calculated from
After SF transformed into SF-SSZ-13 zeolite, the loss on ignition
the XRD pattern was 80% (The relative crystallinity is defined as
(LOI) and sodium of the sample were increased, which indicated
the ratio of the sum of intensities of the 9 reflections of the
that sodium and –OH existed in the zeolite structure [36]. How-
sample over the sum of the intensities of the same 9 reflections
ever, the Si/Al ratio of the synthesized SF-SSZ-13 was smaller than
of the standard sample) [26]. Moreover, lattice parameters
initial gel. The lower Si/Al ratio was probably due to the higher
of the hydrothermal product were refined by Rietveld method
alkalinity of the hydrothermal reaction [23]. From the XRF result,
using XRD data. Table 1 showed the unit cell parameters of
the synthesized SF-SSZ-13 had higher Si/Al ratio, it seems that
standard SSZ-13 (S-SSZ-13) and refined sample SF-SSZ-13. As
the diffusion pathway through SF is shorter than for the conven-
observed, the unit cell parameters of SF-SSZ-13 had a slight change
tional high-silica SSZ-13 samples. It should be noted that the
compared to S-SSZ-13, which may explained that the chemical
hydrolyzation of SF can be validated absolutely.
composition of SF. The crystal with unit cell c-parameter increased,
while a and b-parameter decreased, which may interpreted as
3.2.2. The particle size distribution
silica source resulted in the change of SSZ-13 unit cell. Base on
The particle size distribution was obtained by DPSA analysis
the above XRD results, it evidenced that SF had been transformed
and the statistics of distribution was calculated from the results
into well crystallized SSZ-13 zeolite after the hydrothermal
using the derived diameters, an internationally agreed method of
process.
defining the mean and other moments of particle size [37], which
were shown in Fig. 5. The major population of SF had a particle size
3.1.2. SEM analysis in the range of 0.2–130 mm (Fig. 5a), revealing that the obtained
The SEM images of SF and as-synthesized product (SF-SSZ-13) product were homogeneous in size. While SF-SSZ-13 displayed
were displayed in Fig. 3.1 SF exhibited smooth spherical particles two peaks at range of 3.42–4.23 mm and 17–40 mm (Fig. 5b). Note
with diameter about 50–500 nm (Fig. 3a). After the hydrothermal that the particle sizes of SF-SSZ-13 from the DPSA were the size
reaction, the as-synthesized SF-SSZ-13 zeolite (Fig. 3b) displayed and distribution of bulk particles which might be composed of sev-
overall popcorn-like morphology, each popcorn particle was eral small particles aggregated together, and this was similar with
appeared as an assembly of agglomerated small cubic-like crystal, the results from the SEM which displayed images of cluster parti-
and the typical trigonal prism shape shown insert Fig. 3b (red circle), cles [38]. The standard volume percentiles (10%, 50%, 90%) and
which is consistent with earlier reports [27,28]. average particle size of SF and SF-SSZ-13 were displayed in Table 3.
SF-SSZ-13 had lower particle size compared with the SF, which
1
For interpretation of color in Fig. 3, the reader is referred to the web version of attributed to the dissolution and polymerization of SF. The large
this article. SSZ-13 particles, in agreement with previous reference, which
Y. Wang et al. / Advanced Powder Technology 29 (2018) 1112–1118 1115

Fig. 3. SEM images of (A) SF, (B) as-synthesized SF-SSZ-13.

indicated a high degree of silica concentration decrease to the

formation of terraces with sharp edges as well as an increase in
particle size and crystal domain size [39].

3.2.3. Adsorption property

Due to the small pore size of zeolite SSZ-13 (0.38 nm), the
adsorption of large size molecule was limited. N2 (0.304 nm) could
utilized as an alternative to evaluate the absorptivity of the synthe-
sized microporous zeolite SF-SSZ-13. Fig. 6 exhibited N2 sorption/
desorption isotherms of SF and as-synthesized SF-SSZ-13. SF exhib-
ited a characteristic type III (defined by IUPAC) isotherm that not
suitable for porous materials (Fig. 6a) [40]. Fig. 6b showed the zeo-
lites display a nitrogen sorption isotherm of Type I with a H4 hys-
teresis. The H4 hysteresis and Type I sorption isotherm are typical
for microporous zeolitic materials [16]. In general, the trend of the
adsorption isotherms of nitrogen clearly depends on the strength
of the electric field in the zeolites [41]. As shown in Fig. 6b, the iso-
therm of SF-SSZ-13 exhibited a clear, steep increase in N2 adsorp-
tion volume at the region of P/P0 < 0.15, corresponding to quick
Fig. 4. FTIR spectra of SF and as-synthesized SSZ-13 (a) SF (b) SF-SSZ-13.
adsorption of N2 on the external surface and a concave to nearly

Table 2
Chemical composition of SF and SSZ-13 by XRF analysis (wt.%).

Sample SiO2 Al2O3 Na2O Fe2O3 TiO2 CaO MnO K2O P2O5 LOIa
SF 95.465 0.528 0.208 0.107 0.005 0.999 0.014 0.688 0.091 1.52
SF-SSAZ-13 75.172 6.246 5.606 0.363 0.022 3.132 0.034 0.313 0.008 8.01
a
LOI: Loss on ignition at 1000 °C.

Fig. 5. Particle size distribution of samples (a) SF; (b) as-synthesized SF-SSZ-13.
1116 Y. Wang et al. / Advanced Powder Technology 29 (2018) 1112–1118

Table 3
Percentile of SF and SF-SSZ-13 particle size distribution analyzed by DPSA.

Samples D10 (mm) D50 (mm) D90 (mm) Average particle size (mm)
SF 3.598 31.90 61.03 32.40
SF-SSZ-13 2.168 9.364 38.30 15.55

Fig. 6. N2 adsorption/desorption isotherm curves of (a) SF and (b) SF-SSZ-13.

Fig. 7. SEM images of the SF-SSZ-13 obtained after different hydrothermal time.

constant volume due to monolayer adsorption, this sharp increase flat indicating that adsorption saturation occurred. Moreover,
also suggested the presence of microporous in the SF-SSZ-13. SF-SSZ-13 had a large BET surface area of 545.74 m2/g, a BJH
Increasing with the relative pressure P/P0, the slopes were nearly average pore size diameter of 1.69 nm and total pore volume of
Y. Wang et al. / Advanced Powder Technology 29 (2018) 1112–1118 1117

Fig. 8. SF-SSZ-13 zeolite formation and crystal growth mechanism.

Table 4 4. Conclusions
Particle size and surface area of SF-SSZ-13 obtained after different hydrothermal time.
In summary, this work provided an inexpensive and shorter
Samples Particle size (mm) BET Surface area (m2 g 1
)
time for the preparation of high silica microporous material
SF-SSZ-13@12h 24.57 295.61
SSZ-13 using SF as the silica source. The obtained product showed
SF-SSZ-13@24h 19.12 413.27
SF-SSZ-13@48h 15.55 545.74 the nearly similar structure and morphology compared to previous
SF-SSZ-13@72h 14.55 485.36 study, and exhibited high surface area (545.74 m2 g 1). A plausible
growth mechanism to achieve this microporous material SSZ-13 is
also presented. These results will pave a generalized approach to
effectively synthesize other silica or silicon aluminum materials.
0.23 cm3/g. Application of the BET equation to the physisorption of Hence, such a simple solid waste (SF) can open up a new avenue
the SF-SSZ-13 proved that an excellent N2 adsorption capacity was as alternative and cheap source of silica for the production of a
exhibited due to the fact that the higher surface area. Therefore, high-value zeolite product, and highlighted the economic benefits
there was a potential for small pore adsorption application. of reusing the SF.

3.3. Formation mechanism

Acknowledgments

On the basis of the above analysis, a possible process for the

The Project was Supported by the Fundamental Research Funds
formation of microporous zeolite SSZ-13 using SF as silicate
for the Central Universities, China University of Geosciences
source was proposed based on the SEM images in Fig. 7 of these
(Wuhan) (CUG160231), and Open project for Engineering Research
samples under the different hydrothermal times. The deduced
Center of Nano-Geo Materials of Ministry of Education, China
schematic diagram of the SF-SSZ-13 growth mechanism can be
University of Geosciences (Wuhan) (NGM2018KF018).
seen in Fig. 8. Zeolites grew by layer-by-layer adsorption of
growth units, which then migrated to their optimum position
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