Journal of Cleaner Production 32 (2012) 204e209

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Journal of Cleaner Production

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Simultaneous preparation of silica and activated carbon from rice husk ash
Yan Liu, Yupeng Guo, Wei Gao, Zhuo Wang, Yuejia Ma, Zichen Wang*
College of Chemistry, Jilin University, Changchun, 130012, China

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

Article history: Silica and activated carbon were simultaneously produced from rice husk ash with K2CO3. The surface
Received 23 September 2011 area and average pore size of the activated carbon were 1713 m2/g and 4 nm. The maximum adsorption
Received in revised form capacity of activated carbon was 210 mg/g for methylene blue and the capacitance value reached 190 F/g.
14 March 2012
The yield of silica reached 96.84% and the particle size was 40e50 nm. Potassium carbonate could be
Accepted 17 March 2012
recycled. The entire synthetic procedure was simple, environmental-friendly and economical-effectively.
Available online 4 April 2012
Ó 2012 Elsevier Ltd. All rights reserved.
Keywords:
Rice husk ash
Silica
Activated carbon
Environmental-friendly

1. Introduction (Tongpoothorn et al., 2011). Therefore, with many earlier studies,

activated carbon has been prepared from biomass (Yang et al., 2010;
In recent years, renewable energies prepared from biomass have Bagheri and Abedi, 2009; Sumathi et al., 2009; Arami-Niya et al.,
received considerable attention because of the high price of fossil 2010; Kalderis et al., 2008; Sathishkumar et al., 2012). But only a few
fuels and their environmental pollution problems (Lay et al., 2012). research of activated carbon prepared from rice husk ash were
Over the last two decades, a special attention has been paid to the reported (An et al., 2011; Liu et al., 2011). On the other hand, rice
conversion of biomass into biofuels (Zheng et al., 2008; Wang et al., husk ash not only consists of carbon, but also an important kind of
2009; Ikura et al., 2003; Silalertruksa et al., 2011; Börjesson and environmental-friendly silicon source. Silica, which is a basic raw
Tufvesson, 2011). During the converting progress, large amount of material in electronics, ceramic, and polymer material industries,
solid residue (biomass ash) is generated. However, rarely also can be prepared from rice husk ash (An et al., 2010a, b). In
researches are concerning about its utilization. If the biomass ash is earlier researches, activated carbon and silica were prepared sepa-
not utilized properly, it will become tremendous waste, causing rately, and the activator recycling has not been mentioned. While in
energy loss and environmental pollution. present studies, rice husk ash utilizations are focused on harmful
Rice husk is a kind of agricultural by-product. It is reported that substances adsorption (Manique et al., 2012; Chen et al., 2012),
the annual outputs of rice husk worldwide and in China are about catalysis preparation (Ali et al., 2011; Rafiee et al., 2011) and additive
800,000 and 400,000 t, respectively (Li and Wang, 2008; Zhang area (Ramasamy, 2012). The carbon source and silicon source could
et al., 2010), and the rice husk was utilized as fuel to prepare bio- not be sufficiently utilized, and the procedure was complex. In
oil (Zheng, 2007). The plentiful solid residue produced after the particular, the activator was not recycled. Therefore, it is very
above process is called rice husk ash. The main components of rice important to find a simple method to fully utilize rice husk ash to
husk ash are carbon (45%) and silica (52%). prepared functional material SiO2 and activated carbon.
Activated carbon is a well-known material used in both gas and In our work, the aim is to prepared silica and activated carbon
liquid phases, including medicinal use, capacitors, pollutant and from rice husk ash simultaneously, and to recycle the activator.
odor removal, gas separation, and catalysis (Nabais et al., 2008; Green and sustainable chemistry is now regarded as a major
Lillo-Ródenas et al., 2006). Agricultural wastes are the ones, which scientific discipline and the studies in this area have led to the
are considered as feed stocks for activated carbon preparation development of cleaner and relatively less toxic chemical processes
with many new technologies each year (Solhy et al., 2010). Based on
those methods, a green producing process was built, where
* Corresponding author. Tel./fax: þ86 43185155358. wastewater and the carbon dioxide have been collected and reu-
E-mail address: [email protected] (Z. Wang). tilized at the same time.

0959-6526/$ e see front matter Ó 2012 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jclepro.2012.03.021
 Y. Liu et al. / Journal of Cleaner Production 32 (2012) 204e209 205

2. Materials and methods conditions of activation and dissolution were important factors to
determine the properties of the resulting products. These factors
2.1. Materials and treatment were extensively examined in the present study. The pore struc-
tures of activated carbon and the character of silica were discussed.
All chemicals and solvents used in this study were analytical In order to depict the degree of activation reaction, the yield of silica
grade and used without further purification. Anhydrous potassium was defined as the percent of Ms/Mr, in which Ms was the mass of
carbonate (K2CO3) and hydrochloric acid (HCl) were purchased silica product and Mr was the mass of the silica in rice husk ash.
from the Beijing Reagent Factory of China. Distilled water was These results were discussed separately as follows.
applied for all synthesis and treatment processes. The rice husk ash
was obtained from pyrolytic rice husk. 3.1. Choice of activation agent

2.2. Preparation of activated carbon The preparation of activated carbons generally involves two
steps: pyrolysis and physical and/or chemical activation (Shi et al.,
Ten grams of rice husk ash after acid pre-treatment was uniform 2010). Chemical activation can be accomplished in a single step by
mixed with K2CO3 powder in a porcelain reactor at a certain carrying out thermal decomposition of raw material with chemical
impregnation ratio. Then the reactor was put into a tube furnace, reagents. The most widely used chemicals include ZnCl2, H3PO4,
which was heated to a designed temperature under nitrogen flow H2SO4, KOH and K2CO3 (Uçar et al., 2009; Girgis et al., 2009; Gerçel
for a certain period of time. In this procedure, the energy can be et al., 2007; Basta et al., 2009; Denga et al., 2010).
provided by bio-oil. The combustion heat of oil which comes from According to our investigation, ZnCl2 and H3PO4 are usually used
pyrolysis rice husk is 25.72 MJ/kg. The system was cooled to 100  C for activating biomass which is rich in cellulose, hemicellulose and
within, and then transferred to a covered 500 mL three-necked lignin such as wood and nut shell (Puziy et al., 2002; Hussein et al.,
flask. A certain amount of water was added to the covered three- 1996). KOH, K2CO3 and Na2CO3 are usually used for activating
necked flask. The suspension was kept boiling for 30 min under residue which is rich in ash. But compared with KOH, the carbonate
reflux condenser and vigorous stirring conditions. Finally, the has lower cost, and the green recycling route is achieved easily.
dispersions were filtered. The activated carbon was washed thor- However, Na2CO3 has poor activation effect (Guo et al., 2000). In
oughly with distilled water and dried for 12 h at 120  C, and the summary, K2CO3 is the optimum activated agent.
filtrate was transferred into a carbonating reactor to prepare silica.
A series of impregnation ratios were used. The impregnation
3.2. Effects of activated conditions on the yields of silica and pore
ratio is given by
volume of activated carbon
Impregnation ratio ¼ ðWeight of rice husk ashÞ=
3.2.1. Activated temperature
 ðWeight of K2 CO3 powderÞ Fig. 1 shows the influence of activated temperature on the pore
volume of the prepared activated carbons and the yield of silica. The
pore volume of the prepared activated carbon increased with
activated temperature between 850 and 1000  C, and obtained the
2.3. Preparation of silica
maximum value of 1.3 mL/g. When the activated temperature
increased from 1000  C to 1050  C, the pore volume was decreased.
The carbonating reactor with obtained filtrate was kept at
This progressive activated temperature increased the C-K2CO3
appointed temperature of 70e95  C, and carbon dioxide was
reaction rate, resulting in increasing carbon “burn-off”. Contem-
introduced into the reactor through a tube for 30 min. The silica
poraneously, the volatiles from the samples continued to evolve
precipitate was aged 3 h at room temperature, and then filtered by
with increasing activated temperature. The develotilization process
a pump. The silica precipitate was washed by distilled water and
further developed the rudimentary pore structure in the char,
dried at 120  C for 24 h to obtain silica powder. The filtrate was
concentrated and crystallized to prepare K2CO3 powder for recycle
and reuse as the reactant to activated rice husk ash.

2.4. Characterization

The specific surface area and pore size of activated carbons are
measured at 77 K by means of a standard BrunauereEmmetteTeller
(BET) procedure N2 adsorption (Quantacerome AUTOSORB-1C).
Prior to gas adsorption measurement, the carbon was degassed at
300  C under vacuum for 3 h. The BET surface area was calculated
from N2 adsorption isotherms by using the BET equation. The total
pore volumes were estimated at a relative pressure of 0.995.
Infrared (IR) spectra of silica were carried out on a Bruker IFS 66 vs1
spectrometer employing the KBr pellet method. The structure and
the composition of samples were analyzed by the X-ray diffraction
(XRD), using Cu Ka (k ¼ 1.54056) radiation on an SHIMADZU-6000
X-ray diffractometer.

3. Results and discussion

The comprehensive utilization of rice husk ash principally Fig. 1. Effect of activated temperature on the yield of silica and the pore volume of
consisted of two consecutive steps: activation and dissolution. The activated carbon.
206 Y. Liu et al. / Journal of Cleaner Production 32 (2012) 204e209

whereas the C-K2CO3 reaction enhanced the existing pores and

created new porosities (Adinata et al., 2007; Hayashi et al., 2002).
The extraction rate of silica increased with the activated tempera-
ture increased, and reached maximum value of 90.48%. This shown
that the activated temperature of 1000  C was close to optimum for
preparing activated carbon and silica.

3.2.2. Activated time

The effect of activated time on the pore volume of activated
carbon and the yield of silica is illustrated in Fig. 2. Activation time
was shown to have dramatic effect on the pore volume of activated
carbon. With activated time increased, the K2CO3 obtained suffi-
cient contact with rice husk ash, and the pore volume of activated
carbon was gradually increased. After reaching the maximum
value (1.65 mL/g), the prolonged activated time leaded to increase
“burn-off” of rice husk ash. Finally, the structure of pore was
destroyed, and the pore volume was decreased. Additionally, the
extraction rate of silica obtained by varying activated time from 15
to 105 min was not significantly different (in the range of
Fig. 3. Effect of impregnation ratio on the yield of silica and the pore volume of
87.59e94.8%). Thus, 90 min was chosen as the optimum activated
activated carbon.
time.

3.2.3. Impregnation ratio 3.2.4. Volume of water

The impregnation ratio has been found to be one of the most In this work, K2CO3 reacted with rice husk ash initially, during
important parameters in preparing activated carbon using chemical which process, part of potassium silicate existed in the carbon
activation (Ahmadpour and Do, 1997). A series of activated carbon porosity, and then it was removed from carbon during water
and silica prepared at 1000  C for 90 min using different impreg- dissolution to form pores, at the same time, silica is separated.
nation ratios of K2CO3 are shown in Fig. 3. It indicated remarkable Therefore, the dissolution of potassium silicate has a great influence
effects on both the pore volume of activated carbon and the yield of on the pore volume. In this process, the potassium silicate obtained
silica. With increasing impregnation ratio from 1:1 to 1:1.25, the was dissolved into water, and the water volume was considered.
pore volume increased initially, reached maximum at 1:1.5 and A series of water volume ranging from 60 to 160 mL were
then decreased. The extraction rate of silica reached maximum at studied at 100  C for 30 min. Fig. 4 shows the variation of the pore
1:3 with the increase in impregnation ratio. The pores were created volume of activated carbon and the yield of silica at different water
due to the evolution of gaseous carbonization products and cata- volumes. As seen in Fig. 4, with the water volume significantly
lytic oxidation of carbon surface by potassium metallic salt. At high increased, resulting in both the pore volume of activated carbon
ratio of K2CO3, the pore development was mostly due to the and the yield of silica increased. When the water volume reached to
intercalation of potassium metal in the carbon structure 120 mL, the curves rise slowly and present a platform.
(Sudaryanto et al., 2006). Experimental results suggested appro-
priate impregnation ratio should be selected for the production of 3.3. Characterization of silica, activated carbon and recovered
the activated carbon with the optimal pore volume and the sodium carbonate
extraction rate of silica. Thus, in order to obtain the optimal pore
volume and extraction rate of silica, the impregnation ratio should With this method, we have prepared activated carbon and silica
be around 1:1.5. from rice husk ash, and the optimal experimental conditions

Fig. 2. Effect of activated time on the yield of silica and the pore volume of activated Fig. 4. Effect of water volume on the yield of silica and the pore volume of activated
carbon. carbon.
 Y. Liu et al. / Journal of Cleaner Production 32 (2012) 204e209 207

stretching vibration and bending vibration. The band at 1670 cm1

belonged to HeOeH bending vibration.
The average diameter of the silica particles was about
40e50 nm. The adsorption of dibutyl phthalate which is a kind of
rubber ingredients is 3.0 mL/g. The silica had been synthesized into
surface hydrophobic silica with long-chain alcohols in water phase
at low temperature (An et al., 2010a, b). It showed the better
physical and mechanical properties after the hydrophobic silica
added to macromoleclar polymer. This amorphous SiO2 can be
changed to tridymite, which has better chemical and optical
properties by treatment with glycol liquid at comparatively low
temperature (Ren et al., 2008).
A useful indication of the pore structure of activated carbon
could be obtained by visual inspection for the shape of the
isotherm. The result was determined by the adsorption isotherms
of nitrogen. The structural heterogeneity of porous material was
generally characterized in term of the pore size distribution. The
pore size distribution was closely related to both kinetic and
equilibrium properties of porous materials used in industrial
application. The pore size distribution of activated carbon at the
optimal condition is given in Fig. 7. From this figure, it seemed to be
a mixed-type of I þ II (El-Hendawy, 2003), which indicated that the
carbon was mainly micro and mesoporous in character with
Fig. 5. XRD of silica obtained at the better condition.
a minor presence of wider pores, where capillary condensation
occurred.
Fig. 8 shows the nitrogen adsorptionedesorption isotherms of
(activated temperature, activated time, impregnation ratio, and
activated carbon at the optimal condition. At low values of P/P0, the
water volume) were determined. A series of characterization of
isotherm was similar to microporous adsorbents. Then adsorption
silica and activated carbon were depicted as follow.
increased markedly at P/P0 above 0.4 where pore condensation
The X-ray spectra and characteristic absorption peak of silica
took place and the isotherm exhibited a hysteresis loop, which
have been obtained and shown in Fig. 5, no pre-treatment has been
suggested that the existence of mesopores in the carbon and the
performed on the sample. The sample is completely amorphous as
size distribution of pores became wider, and the average pore size
indicated by the featureless diffractograms and the appearance of
concentrated in 4 nm. The BET surface area of activated carbon
a diffuse maximum at 2q of 22.5 typical for amorphous silica. The
could achieve 1713 m2/g, which showed the higher surface area
result confirmed the absence of any ordered crystalline structure.
than other studies. The comparison of utilization performance of
Infrared spectra of the silica is recorded by FT-IR spectrometer
the as-prepared activated carbon and the commercial activated
and presented in Fig. 6, and the major chemical groups of silica are
carbons are shown in Table 1, it indicates that they have proximal
identified. The predominant absorbance peaks of silica are dis-
surface area. It can be found that the micoporosity plays an
played in the low frequency region bands at 1200e1000 cm1,
important role for adsorption of methylene blue, and the capaci-
807 cm1 and 475 cm1 due to asymmetric stretching, symmetric
tance value mainly due to contribution of mesoporosity. Therefore,
stretching and bending modes of bulk SieOeSi. The band located at
the activated carbon produced in our route has rich micopores and
3366 cm1 and 955 cm1 was ascribed to the SiOeH asymmetry

Fig. 7. Differential pore size distribution of activated carbon obtained from rice husk
Fig. 6. FT-IR spectra of the silica. ash.
208 Y. Liu et al. / Journal of Cleaner Production 32 (2012) 204e209

Fig. 8. Nitrogen adsorptionedesorption isotherms measured on synthetic activated

carbons.

Fig. 9. XRD of K2CO3 obtained from the filtrate of carbonation reaction.

mesopores, and possesses the extensive applications. The activated

carbon in this work presented optimal adsorption capacities for
which had been confirmed in the experiment, and it could be used
methylene blue adsorption (210 mg/g) compared with other
as the initial reactant.
researches (49e333.3 mg/g) (Miguel et al., 2002; Rozada et al.,
2003; Singh and Srivastava, 2001; Bestani et al., 2008; Deng et al.,
2011; Ryu et al., 2002; Lata et al., 2007). We had amplified the 4. Conclusions
experiment in 5 and 10 times, the yield of silica was 97.10% and
97.5%, and the BET surface area of activated carbon could achieve In this work, an alternative approach for preparing activated
1600e1700 m2/g. carbon and silica from rice husk ash was developed. The traditional
preparation method was simplified and improved. Compared with
3.4. Recycling of potassium carbonate commercial products, the application prospect of the activated
carbon prepared in this work was much more promising due to its
The X-ray spectra and characteristic absorption peak of the high adsorptive capacity. The performances of the simultaneously
recovery of potassium carbonate, and comparison with the stan- prepared activated carbon and silica were similar to the separately
dard potassium carbonate is shown in Fig. 9. The XRD peaks were prepared ones.
indexed in terms of the potassium carbonate structure according to
the standard JCPDS files no. 49-1093. All diffraction peaks were Acknowledgements
quite similar to the pure potassium carbonate, and the determined
unit cell parameters were in good agreement with the standard This work was supported by Key Project of the National Eleventh
values. No characteristic peaks of impurities, such as KHCO3 and Five-Year Research Program of China (2008BAE66B00), Scientific
other unreacted compounds were observed. Thus, the results and Technological Planning Project of Jilin Province (20075009 and
showed that the as-prepared product was pure potassium 20100326), and the Interdisciplinary Research Project of Jilin
carbonate. The recovery rate of potassium carbonate was 94.2%, University (201003030).

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