b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4

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A study on the consecutive preparation of silica powders and

active carbon from rice husk ash

Dongmin An, Yupeng Guo, Bo Zou, Yanchao Zhu, Zichen Wang*

College of Chemistry, Jilin University, Qianjin street 2699, Changchun 130012, China

article info abstract

Article history: Rice husk ash (RHA) is an abundant agricultural by-product. The present research work
Received 2 July 2010 deals with the production of silica powders and active carbon from RHA with a consecutive
Received in revised form method. The RHA is firstly treated with acid leaching to remove mineral composition, and
12 November 2010 then is boiled with base to leach silica. The filtrate is used to synthesize silica powders with
Accepted 10 December 2010 CO2 precipitator and solid residue is used to prepare active carbon. The optimum condi-
Available online 15 January 2011 tions of preparing silica powders are as follows: the concentration of Na2CO3 is 25 wt.%, the
base-leached time is 4 h, and the impregnation ratio of Na2CO3 solution to RHA is 6:1. The
Keywords: yield of silica leached from RHA is 84.57 wt.%. The synthesized silica powders are hydrated
Rice husk ash with amorphous structure, moreover, with a relative smooth surface and high purity. The
Silica powders residue is activated with potassium hydroxide (KOH) after base-leached. The activated
Active carbon carbons are found to be a mixture of micropore and mesopore pore structures. The
Consecutive preparation maximum pore volume, BET surface area and iodine adsorption capacity of as-prepared
Morphological feature active carbon can reach 1.22 cm3/g, 1936.62 m2/g and 1259.06 mg/g, respectively. Field
emission scanning electron microscopy (SEM) is used to characterize the morphological
features of the ash after step by step treatment.
ª 2011 Elsevier Ltd. All rights reserved.

1. Introduction RHA has been widely used as a construction material to

Rice husk is an agricultural waste material abundantly avail-
able in rice-producing countries. In recent years, the applica-
tion of rice husk as fuel in power plant is increasing, due to its
high calorific power. In this combustion, rice husk ash (RHA) is
produced [1]. RHA usually has a light weight, therefore, the
disposal of bulky RHA could be a problem. In some areas,
a large amount of RHA is treated as waste and disposed at
landfill site, leads to air and water pollution. The airborne
particles have been linked to respiratory disease in humans
[2]. RHA usually contains over 60% silica, 10e40% carbon and
minor other mineral composition. More researchers become
interested in how to use this industrial waste, because RHA is
available in plenty and almost free of cost.
product concrete [3e5], or as a adsorbent to adsorb organic
dye, such as indigo carmine dye [6], and inorganic metal such
as lead, mercury [7], Cd2þand Zn2þ metal ions [8]. However,
the final disposal of the RHA after adsorption has not been
reported. Due to its high silica content, RHA can be an
economically viable raw material for the production of sili-
cates and silica in recent years [9,10]. Some researchers have
synthesized ZSM-5 zeolite or MCM-48 from RHA [11,12], but
long time (generally about several days) and high temperature
(generally at 150  C) to synthesize these materials have limited
this method to utilize RHA. Amorphous silica from RHA is
usually extracted with alkali, such as sodium hydroxide
[13,14], and sodium carbonate. The residue is obtained with
above 50% carbon content after silica leached RHA and the

* Corresponding author. Tel./fax: þ86 431 8515 5358.

E-mail address: wangzc@jlu.edu.cn (Z. Wang).
0961-9534/$ e see front matter ª 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biombioe.2010.12.014
1228 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4

disposal of the residue has not been mentioned in these
papers.
Production of activated carbon from rice husk has also
attracted people’s attention. Active carbon, which is a versa-
tile adsorbent because of its good adsorption property, can be
produced from a variety of raw materials, such as packing
papers, plastic bottles, by-products of the timber industry (e.g.
sawdust), straw, rice husk, seeds or fruit shell can be
mentioned. In recent years, there is an increasing interest in
the production of activated carbon from agricultural by-
products and residual wastes. Production of activated carbon
from rice husk is achieved through activation with chemical
or physical means. Chemical impregnation with KOH or NaOH
of pyrolysed rice husk followed by activation at 650e850  C
results in activated carbons with extremely high surface areas
(1413e3014 m2/g)[15]. The aim of using KOH or NaOH is to
remove the silica so as to increase the pore in the rice husk. As
far as we know, the content of amorphous silica in rich husk is
around 20%, and more in pyrolysed rice husk. The disposal of
these silica or silicate is not mentioned when active carbon is
prepared from rich husk or pyrolysed rice husk, either. The
RHA is high in silica content and the loose wet structure of rice
husk is destroyed after rice husk combustion in high
temperature. While silicon dioxide is extracted from the RHA,
the carbon content is increased greatly in the residue, which is
more economical for active carbon preparation in order to
realize the farthest value of the agricultural waste.
In this paper, the research work deals with the production
of silica powders and active carbon from RHA with a consec-
utive method. The RHA is firstly treated with acid leaching to
remove mineral composition, and then is boiled with sodium
carbonate to leach out silica, while sodium carbonate is
usually used to smelt quartz sand at 1300  C in industry
[16,17]. The filtrate is used to synthesize silica powders and
solid residue is used to prepare active carbon. The main
influencing parameters on the silica leaching yield from RHA
and on the pore volume, BET surface area of obtained active
carbon are investigated, respectively. The adsorption capacity
of active carbon is investigated by adsorbing iodine. In all
previous studies [18e21], the produced carbon has significant
surface areas and adsorption capabilities, in many cases
comparable with the commercially available carbons.
However, their production method involves several stages of
preparation, long retention times for pyrolysis of rice husk.
The method we used can produce silica powders and active
carbon at the same time.
carbon and other impurities. The composition of RHA is given
in Table 1. Distilled water is applied for all synthesis and
treatment processes.
2.2. Acid pretreatment of RHA
The aim of acid pretreatment is to improve the purity of silica
product. Many authors [22e26] have concluded that prelim-
inary leaching of rice husk with a solution of HCl, HNO3,
H2SO4, NaOH and NH4OH, boiled before thermal treatment,
proves to be an effective way in substantially removing most
of the metallic impurities and producing ash silica
completely white in color. A typical procedure is as follows:
the dried RHA is refluxed with HCl solution in a flask within
a thermostat for 30 min. After the acid solution is drained,
the RHA is washed repeatedly with hot distilled water until
the filtrate is free from the acid, and then is dried at 120  C for
12 h.
2.3. Preparation of silica powders
30.00 gof the acid pretreated RHA is put into a flask, and 150 ml
of 25 wt.% Na2CO3 solution is then poured into the reactor. The
suspension is boiled for 4 h under reflux condenser, and
vigorous stirring is applied during the whole reaction process.
The suspension is filtered and solid residue is washed with hot
water. Finally, the filtrate is moved to another reactor and
5.00 wt.% PEG is added into the filtrate under stirring. Mixed
gases with N2/CO2 are then introduced into the reactor. The
resulting slurry is kept aging for 3 h at room temperature after
carbonation for 60 min, and then is filtered. The precipitate is
washed by distilled water and then dried at 120  C for 24 h. The
solid residue is directly dried at 120  C for the use of prepa-
ration of active carbon.
2.4. Preparation of active carbon
The process of preparing active carbon from residue after
silica extraction is depicted as follows: the carbon residue is
impregnated with KOH at various ratios. The impregnated
ratio is the mass of the activating agent compared with the
mass of the dried carbon residue depending on the ratio of
Table 1 e The composition of the RHA.
Composition Value

2. Materials and methods K2O 1.952 wt.%

CaO 0.592 wt.%
Na2O 0.078 wt.%
2.1. Materials
MgO 0.221 wt.%
Al2O3 0.606 wt.%
All chemicals are analytical grade and used without further ZnO 0.015 wt.%
purification. Anhydrous sodium carbonate (Na2CO3), hydro- Fe2O3 0.423 wt.%
chloric acid (HCl), iodine (I2), potassium hydroxide (KOH) and MnO2 0.101 wt%
polyethylene glycol 10000 (PEG 10000) are purchased from the CuO 432 ppm
Beijing Reagent Factory of China. N2 and CO2 are chemical TiO2 8 ppm
SiO2 66.12 wt.%
grade (at a purity of 99%).The rice husk ash (RHA) is from
C 29.64 wt.%
a power plant of Jilin Province in China. The gross weight of Others 0.25 wt.%
silicon dioxide in the RHA is 66.12 wt.%, and the residual is
 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4
activating agent/carbon residue (A/C) used (1:1, 2:1, 3:1 or
4:1).The impregnated residue is set in a crucible at 200  C for
30 min in order to remove the excess water, and then the
resulting mixture is used for carbonization. The carbonization
is carried out in a horizontal furnace and the samples are
heated (20  C/min) from room temperature to the final
carbonization temperature. Samples are kept at the final
temperature for 1.0 h before cooling down to room tempera-
ture. The samples are washed repeatedly with distilled water
until the activating agent is removed, and then the product is
dried at 110  C for 12 h.
2.5. I2 adsorption experiments
Experiments are conducted according to the China National
Standards GB/T 12496.7e1990. The obtained active carbon is
first triturated and then filtered through a 200 mesh-sieve.
Accurate 0.50 g of porous carbon and I2 solution are shaking in
a thermostatic shaker for 15 min. The mixture is filtered with
filter paper and the residual I2 concentration in the filtrate is
determined by titration.
2.6. Characterization of the silica powders and active
carbon
Minerals composition of the RHA and as-obtained silica
powders are determined by atomic emission measurements
using ICP emission spectroscopy (PerkineElmer Optima 3300
DV). Morphology and size of the silica powders are observed
by scanning electron microscopy with a filed-emission-scan-
ning electron microscope (JEOL JSM-6700F, 10 kV). The crys-
talline phase of the synthesized silica powders is
characterized by the X-ray diffraction (XRD), using Cu Ka
(l ¼ 1.54056 Å) radiation on an SHIMADZU-6000 X-ray
diffractometer. Fourier transform-infrared spectroscopy
(FTIR) experiments are carried out on a Bruker FT 5DX (Nicolet)
spectrometer employing the KBr pellet method. The specific
surface area and pore diameter of the active carbon samples
are measured by N2 adsorption at 77 K using an ASAP 2010
Micromeritics instrument and the BET method. Micropore
volumes are calculated by use of the DubininePadushkevich
equation and mesopore volume are calculated by the Barrett-
Joyner-Halenda (BJH) method (ASTM D4641-94). The average
pore diameter is estimated from the surface area and pore
volume.
3. Results and discussion
3.1. Effect of reaction condition on the yield of silica
powders
Extraction of silica from RHA is mainly affected by the
concentration of Na2CO3, the extraction time, impregnation
ratio (Na2CO3/RHA, ml/g). Therefore, those factors are inves-
tigated respectively. In order to depict the degree of silica
extraction, the yield of silica powders is defined as the percent
of Ms/Mr, in which Ms represents the mass of synthesized
silica powders and Mr represents the mass of silica in RHA.
1229
3.1.1. Effect of concentration of Na2CO3 on the silica yield
Fig. 1a shows the effect of Na2CO3 concentration on the yield
of silica. When the other two factors (the extraction time,
impregnation ratio) are fixed at 4 h and 5:1, the yield of silica
increases with the increment of Na2CO3 concentration and
reaches the maximum value (81.05 wt.%) when Na2CO3
concentration is 25 wt.%. However, the silica yield decreases
to 74.30 wt.% when Na2CO3 concentration increases to
30 wt.%. It can be explained as follows: the reactions (a, b and
c) occur in the suspension solution, and the concentrations of
HCO 
3 and OH increases with the concentration of Na2CO3
increasing. The increment of OH leads to more silica leached,
which promotes the reaction c to carry through, so the yield of
silica increases. But the solubility of NaHCO3 (The maximum
solubility of NaHCO3 is 9.6 g at 30  C) is weaker than the
Na2CO3 (The maximum solubility of Na2CO3 is 21.5 g at room
temperature), while the amount of liquid is decreased sharply
when the suspension is filtered because of the strong moisture
absorption of ash residue, besides, the temperature of the
suspension decreases when filtered, all of these factors result
in the concentrations of HCO 3 and H4SiO4 are supersatura-
tion, therefore, the increased Na2CO3 concentration leads to
the separating out of silica entered solid ash residue when the
suspension is filtered, as leads to the yield of silica decreasing
when the concentration of Na2CO3 solution is 30 wt.%. On the
other hand, the reenter of silica results in the silica content in
carbon residue increased, as certainly will affect the quality of
the preparation of active carbon. So the optimal concentration
of Na2CO3 is 25 wt.%.
CO2
3 þ H2 O ! HCO
3 þ OH

(a)
2OH þ SiO2 ! SiO3
2
þ H2 O (b)
4HCO
2 2
3 þ SiO3 ! H4 SiO4 þ CO3 (c)
3.1.2. Effect of the reaction time on the silica yield
To find the effect of extraction time on the yield of silica
powders, the extraction time is varied from 2 to 6 h, when the
concentration of Na2CO3 is fixed at 25 wt.% and impregnation
ratio is 5:1. The yield of product increases with reaction time
increasing as shown in Fig. 1b. However, no significant
increment of silica yield (83.20 wt.% at 6 h) is observed at
longer reaction time than 4 h (81.05 wt.%), so 4 h is confirmed
as the optimal reaction time.
3.1.3. Effect of the impregnation ratio on the silica yield
The impregnation ratio is investigated from 4:1 to 9:1 When
the concentration of Na2CO3 is fixed at 25 wt.% and reaction
time is 4 h. When the impregnation ratio is 4:1, the yield of
silica is 76.38 wt.%, and the yield increases to 84.57 wt.% as the
impregnation ratio increases to 6:1. Continual increment of
impregnation ratio is just given a limit increasing of silica
yield (85.55 wt.% at 8:1 and 86.16 wt.% at 9:1) as shown in
Fig. 1c, from which, we can see that the yield of silica is not
obvious from 76.38 wt.% to 86.16 wt.% although impregnation
ratio increases from 4:1 to 9:1. However, considering low
impregnation ratio (5) will bring inconvenient operation (the
ash is not easy moved from reactor due to few liquid in the
system) and high impregnation ratio will bring high cost, so
impregnation ratio of 6:1 is chosen in our study.
1230 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4

3.2. Morphology and structural features of synthesized

silica powders

The as-prepared silica powders are investigated by SEM

(Fig. 2a), FTIR (Fig. 2b) and XRD (Fig. 2c) respectively. The purity
of the obtained silica powders is investigated by ICP
measurement. The results are shown in Table 2. Data in Table
2 shows that the metal oxides in RHA are removed efficiently
under acid pretreatment. The morphology of the obtained
silica powders is shown in Fig. 2a. The silica particles about

Fig. 1 e The effect of concentration of Na2CO3 (a); the

reaction time (b); and the impregnation ratio of Na2CO3 to
RHA (c) on the yield of silica leaching from RHA.
Fig. 2 e The SEM (a), FTIR (b), and XRD (c) of as-prepared
silica powders.
 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4 1231

Table 2 e The elements content analysis of as-obtained

silica powders.
Composition Value (wt.%)

K 2O 0.0038
CaO 0.0092
Na2O 0.0128
MgO 0.0012
Al2O3 0.0022
ZnO 0.0000
Fe2O3 0.0015
MnO2 0.0005
CuO 0.0000
TiO2 0.0000
SiO2 99.6000
C 0.0000

100e200 nm is interlinked together. PEG as surfactant can play

a certain dimensional hindrance effect as can control the
dispersibility of silica powders [27]. Two kinds of hydrophilic
groups (hydroxyl group and ether linkage) are in PEG mole-
cules, therefore, the PEG is a good water soluble surfactant. In
aqueous solution, it looks like a snake, so it can easily be
adsorbed on the surface of the particles to form a macromol-
ecule protection layer, that’s why our obtained silica particles
has a slippery surface and better dispersibility. The adsorption
peaks at 3540 and 1640 cm1 in Fig. 2b are assigned to the
HeOeH stretching and bending modes of the adsorbed water,
respectively. The strong peaks at 1101, 944, 789, and 470 cm1
correspond to asymmetric, symmetric and the bending modes
of SiO2 respectively. There are no CeH absorption peaks at
2910 and 1500e1300 cm1. Therefore, the FTIR confirms that
the powder is silica without the contamination of PEG. The
XRD pattern in Fig. 2c confirms that the powders are amor-
phous silica.

3.3. Preparation of active carbon from solid residue

The effect of different activated conditions variables on

physical and chemical characteristics of the active carbon
products will be discussed in this section. The main influ-
encing factors on the BET surface area and iodine adsorption
capacity of active carbon samples are investigated. Moreover,
the morphologies of samples after different treatment are also
investigated to explain the adsorption property of samples.
Fig. 3 a shows pore volume change of active carbon
samples with different activated temperature at various
impregnation ratios. The pore volume of active carbon
increases with the raise of the activated temperature. For the
boiling point of potassium is 758  C, the potassium can enter
into the interior of carbon structure and make the activation
freely above 758  C, the active reaction improves and the
number of pores in the rice husk ash increase, thus the pore
volume increases. On the other hand, when the activated
temperature reach 900  C, according to our previous study[15],
the white and blue compound will be obtained at 900  C with Fig. 3 e The effect of impregnation ratio and activated
KOH treatment and no porous carbon will remain, here, the temperature on the pore volume of active carbon (a);
same phenomena occurred in our experiment. The pore adsorptionedesorption isotherm (b), and the pore size
volumes of active carbons reach their maximum value when distribution of active carbon samples obtained at
the impregnation ratio is 2:1 at all investigated temperatures. impregnation ratio of 2:1 and 850  C (c).
However, the pore volume is relatively small when the
1232 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4

impregnation ratio is 1:1. This may be because activation

occurs only at the exterior of the RHA, and decreases the
formation of pores. An increase in the activating agent
promotes the contact area between RHA and activating agent,
therefore, increases the pore volume of active carbon, but the
pore volume of activated husk ash samples decreases, when
the impregnation ratio exceeds 2:1, as shows that these pore
volume values are sensitive to impregnation ratio. The
observation can be explained as follows: the porosity of the
carbon structure can be created by leaching out silica and
removing the chemical activating agents in the carbonized
samples by washing. However, with the increasing of active
agent KOH, the excess KOH reacted with C for the low silica
content in solid residue [28], some pores may become larger
because of the collapse of some micropore, as a result, low
total pore volume is obtained finally.
Nitrogen adsorption isotherms at 77 K for active carbon
prepared at 850  C of activated temperature and 2:1 of
impregnation ratio are shown in Fig. 3b. The isotherm displays
a sharp knee at the relative pressure (P/Po) < 0.01, which is
typical to microporous systems [29]. When the adsorption
increases markedly above 0.4, the isotherms show apparent
hysteresis loops. This may be caused by a capillary conden-
sation in the mesoporous structures of the activated carbon.
This implies that samples have both micropore and mesopore
pore structures [30]. A typical pore size distribution of the
obtained porous carbon is shown in Fig. 3c, as further
confirms that active carbon sample has both micropore and
mesopore pore structures but mainly mesoporous.
Fig. 4 shows the BET surface area and iodine adsorption
capacity of active carbon activated with different temperature
at various impregnation ratios. As can be seen in Fig. 4a, the
minimum BET surface area and iodine adsorption capacity Fig. 4 e The effect of impregnation ratio (a); and activated
occurs in the sample that is carbonized at impregnation ratio temperature (b) on the BET surface area and iodine
of 1:1. With the increment of impregnation ratio, the BET adsorption capacity.
surface area and iodine adsorption capacity gradually
increases, as the pore volume varies depicted in Fig. 3a, the
BET surface area and pore volume of samples reach their Fig. 5a shows the morphological features of the raw mate-
maximum values at impregnation ratio of 2:1 at the temper- rial RHA. It can be seen in Fig. 5a, most ash is with fragments
ature of 850  C, and the iodine adsorption capacity reaches its morphology although some ash is well organized in structure
maximum at the same time. The increase in iodine adsorption that resembles rolling hills which remains the morphology of
capacity is most likely related to the maximum surface area rice husk. Fig. 5b shows the morphology of RHA after acid
created and the availability of more adsorption sites for the leaching. With the leaching of mineral composition, the RHA
bulky organic group, while the BET surface area and iodine was broke into pieces and the surface of the outer epidermis is
adsorption capacity decrease with the continual increment of peeled off, and a few big pores are presented. The morphology
impregnation ratio, as is for the total pore volume decreasing of base-leached RHA is shown in Fig. 5c. The silica in RHA reacts
when impregnation ratio exceeds 2:1, which lead to less with sodium carbonate and is then removed after base-leach-
adsorption sites for iodine. The effect of activated tempera- ing of the RHA. As a result, a few small pores are left in the ash’s
ture on the BET surface area and iodine adsorption capacity is inner part. Fig. 5d shows the morphology of as-obtained active
shown in Fig. 4b. When the activated temperature is lower carbon similar to the ash after base-leached, more mesopores
than 850  C, the reactants are only partial activated, as lead to and micropores are created by the etching of KOH within the
low total pore volume so as to low BET surface area and iodine carbon residue. The change of pore volume shown in Fig.5e
adsorption capacity. When the activated temperature reaches also indicates the description above. The total pore volume of
900  C, no porous carbon is obtained. It is clearly shown that raw RHA only is 0.06 cm3/g, the pore volume gradually
850  C is the optimum temperature to produce activated increases to 0.12 cm3/g and 0.162 cm3/g when raw RHA is
carbon from carbon residue through KOH treatment, and the leached by acid and base, respectively, but the increment of
resulting active carbon has BET surface area of 1936.62 m2/g pore volume is feeble. When the carbon residue is activated
and iodine adsorption capacity of 1259.06 mg/g respectively, with KOH, the total pore volume quickly increases to 1.22 cm3/
which shows comparable adsorption capacity with the g, which is further confirmed that the pores are mainly created
commercial activated carbon. by KOH eroding at higher temperatures.
 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4 1233

Fig. 5 e The SEM of samples: the raw RHA (a); the acid pretreatment RHA (b); the RHA after base leaching (c); the active carbon
obtained at impregnation ratio of 2:1 and 850  C (d).

84.57 wt.% by base-leaching at 25 wt.% of Na2CO3 concentra-

4. Conlusions
The studies show that the silica powders and active carbon
are successfully obtained through a consecutive preparation
method from RHA. The silica extraction yield can reach
tion, 6:1 of impregnation ratio and 4 h of reaction time. Active
carbon produced from carbon residue has good iodine
adsorption capacity. The optimal experimental conditions are
2:1 of impregnation ratio, 850  C of activated temperature. The
results obtained in this study suggest that the RHA is
1234 b i o m a s s a n d b i o e n e r g y 3 5 ( 2 0 1 1 ) 1 2 2 7 e1 2 3 4

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