Preparation of high-surface area activated carbons from Paulownia wood

by ZnCl
2
activation
Sait Yorgun
*
, Naile Vural, Hakan Demiral
Department of Chemical Engineering, Engineering and Architecture Faculty, Eskis ehir Osmangazi University, 26480 Eskis ehir, Turkey
a r t i c l e i n f o
Article history:
Received 17 September 2007
Received in revised form 16 February 2009
Accepted 18 February 2009
Available online 9 March 2009
Keywords:
Paulownia wood
Activated carbon
Chemical activation
Textural characterization
a b s t r a c t
In this study, an activated carbon with high-surface area was prepared from Paulownia (P. tomentose)
wood by chemical activation with ZnCl
2
. The inuences of carbonization temperature and impregnation
ratio on the pore structure of the activated carbon were investigated. Activation temperatures and
impregnation ratios were selected in the range of 400700 C and 0.54.0, respectively. Under the exper-
imental conditions investigated, a carbonization temperature of 400 C and impregnation ratio of 4.0
were found to be suitable for producing high-surface area activated carbon. It was shown that ZnCl
2
works effectively as dehydration reagent below 500 C. The obtained carbons were characterized by
nitrogen adsorptiondesorption isotherms at 77 K. The results showed that the surface area and micro-
pore volume of activated carbons, which were determined by application of the BrunauerEmmettTeller
(BET) and t-plot methods, were achieved as high as 2736 m
2
/g and 0.69 cm
3
/g, respectively. The chemi-
cally activated carbons were found to be mainly type I carbons. The microstructures of the char and acti-
vated carbons were also examined with scanning electron microscopy (SEM).
2009 Elsevier Inc. All rights reserved.
1. Introduction
Biomass is a renewable resource that can be better managed
and utilized to provide a wide range of useful chemicals, materials
and energy. A possible utilization of biomass resources is convert-
ing it into activated carbon.
The environmental constraints and a growing demand in
adsorbing materials need to intensify research works on activated
carbon produced fromnon-fossil sources. In this perspective, ligno-
cellulosic wastes from agriculture and forestry are of great interest
[1]. In recent years, evaluation of agricultural and forestry wastes
as raw materials for the production of activated carbons has in-
creased remarkably due to their low cost and large supply.
Activated carbon is predominantly an amorphous solid with a
large internal surface area and pore volume. It consists of a basic
structural unit building up of condensed aromatic rings. The pores
in the carbon contribute to the increase in its surface area and to
textural properties before and after activation [2]. Activated carbon
is one of the most important adsorbents used in industry. This
adsorbent is mainly used for separation and purication of gaseous
and liquid mixtures [36]. The nature of the precursor, activation
method, and activation conditions determine the characteristics
of porosity in activated carbons, including pore size distribution,
pore shape and surface chemistry [2,6,7].
Activated carbons can be produced basically by two methods:
physical activation or chemical activation. The former involves pri-
mary carbonization of the raw material (below 700 C) followed by
controlled gasication at higher temperatures (>850 C) in a
stream of an oxidizing gas (steam, CO
2
, air or a mixture) [810].
Chemical activation is known as a single step method of prepara-
tion of activated carbon in the presence of chemical agents which
are normally alkali and alkaline earth metal containing substances
and some acid such as KOH, K
2
CO
3
, NaOH, Na
2
CO
3
, AlCl
3
, ZnCl
2
,
MgCl
2
, H
3
PO
4
and H
2
SO
4
[2,9]. Chemical activation is the process
that normally takes place at a lower temperature and shorter time
than those used in physical activation. Moreover, the development
of a porous structure is better for the chemical activation. The car-
bon yield in chemical activation is usually higher than in physical
activation since the chemical agents are substances with dehydro-
genation properties that inhibit the formation of tar and reduce the
production of other volatile substances [5,1012]. Among the
chemical activating agents, in particular, zinc chloride is the most
widely used chemical in the preparation of activated carbon [13].
Zinc chloride activation has been applied to different materials
[6,11,1323].
Woods are one of the most important materials for preparing
activated carbons, which have particular porous characteristics
and are appropriate for the adsorption of solute in liquid-phase
[5]. There are many studies in the literature relating to preparation
and characterization of activated carbon from forest wastes [24].
Paulownia is scrophulariacease, with nine species of the very
adaptable and fast-growing timber trees. Paulownia, which is
1387-1811/$ - see front matter 2009 Elsevier Inc. All rights reserved.
doi:10.1016/j.micromeso.2009.02.032
* Corresponding author. Tel.: +90 222 239 37 50x32 76; fax: +90 222 239 36 13.
E-mail address: [email protected] (S. Yorgun).
Microporous and Mesoporous Materials 122 (2009) 189194
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j our nal homepage: www. el sevi er . com/ l ocat e/ mi cr omeso
indigenous to China, has been naturalized in Japan, Australia, Bra-
zil, Europe and USA [25]. In recent years, Paulownia is receiving
increasing attention as a genus suitable for use as a short-rotation
woody crop in Turkey. The climate of Turkey is suitable for Pau-
lownia plantation. If appropriate conditions are provided, the tree
can reach about 1525 m high in a 5-year period [26,27]. Paulow-
nia trees have been used for different purposes such as to produce
leaves useful as fodder or fertilizer, ower for honey production,
and wood for solid products over the years [25,28,29].
In this study, the use of Paulownia wood to produce activated
carbon has been considered. For this purpose, activated carbons
were prepared from Paulownia wood (P. tomentose) by chemical
activation with zinc chloride, and the inuences of carbonization
temperature, and impregnation ratio on the pore structure (spe-
cic surface area, pore volume, and pore size distribution) were
investigated. In addition, scanning electron microscopy (SEM) has
been used to visually observe the differences in the development
of the microstructure of the activated carbons.
2. Experimental
2.1. Materials
Paulownia wood used in this study as a raw material was ob-
tained from orum, Black Sea region in Turkey. Prior to use, sample
was air dried, grounded in high-speed rotary cutting mill and then
screened to give the fraction of 0.6 < Dp < 1.8 mm particle size for
use in the chemical activation experiments. Elemental analyses
of the raw material and activated carbon were performed on a Car-
lo Erba Model EA 1108 elemental analyzer. ASTM standard test
procedures were applied for ash content, ASTM D 1102-84; volatile
matter content, ASTM E 897-82; higher heating value, ASTM D
3286 and moisture content, ASTM D 2016-74. Fixed carbon was
calculated from the difference. The proximate and ultimate analy-
ses of the raw material and activated carbon are given in Table 1.
2.2. Preparation of activated carbon
In this study, the impregnation ratio was calculated as the ratio
of the weight of ZnCl
2
in solution to the weight of the used Paulow-
nia wood. The impregnation ratio was varied between 0.5 and 4.
Chemical activation of Paulownia wood was performed using zinc
chloride. Ten to eighty grams of ZnCl
2
were dissolved in 200 mL of
distilled water, and then 20 g of the raw material was mixed with
the ZnCl
2
solution and stirred at approximately 80 C for 7 h to en-
sure a complete reaction between ZnCl
2
and wood particles. The
mixtures were then ltered and the remaining solids were dried
at 110 C for about 12 h.
Carbonization of the impregnated sample was carried out in a
316 stainless steel tubular reactor with a length of 104 mm and
an internal diameter of 70 mm, with a sweep gas (N
2
) connection.
The xed-bed reactor was externally heated by an electrical fur-
nace. In the carbonization system, heating rate and nal carboniza-
tion temperature were controlled. The temperature was measured
with a NiCr thermocouple inside the bed. More detailed descrip-
tions of the carbonization procedure can be found elsewhere [30].
About 10 g of the impregnated sample was placed on a metal mesh
in the reactor and heated up to the nal carbonization temperature
under the nitrogen ow (150 cm
3
/min) at heating rate of 10 C/min
and held for 1 h at this nal temperature. The nal carbonization
temperature was varied from 400 to 700 C. The resulting solids
after carbonization were boiled at about 90 C with 100 mL of
1 N HCl solution for 30 min to leach out the activating agent, l-
tered and rinsed by warm distilled water several times to remove
excess acid. They were then dried at 110 C for 12 h, and weighed
to calculate the yield.
2.3. Characterization of the prepared activated carbon
The pore structure characteristics of the resulting activated car-
bons were determined by nitrogen adsorption at 77 K using an
automatic adsorption instrument (Quantachrome, Autosorb-1 C).
Prior to gas adsorption measurements, the samples were degassed
at 300 C in a vacuum condition for 3 h. Adsorption data were ob-
tained over a relative pressure, P/P
o
, ranging from approximately
10
6
to 1. The surface area, pore volume and pore size distribution
of the activated carbons were determined by the application of the
BrunauerEmmettTeller (BET) and t-plot analysis software avail-
able with instrument, respectively. The BET surface areas were as-
sessed by applying relative pressures ranging from 0.01 to 0.15 [8].
The total pore volumes (V
t
, cm
3
/g) were estimated to be the liquid
volumes of N
2
at a high relative pressure near unity (0.99). The t-
plot method was applied to the micropore volume and mesopore
surface area, and the mesopore volume was obtained by deducting
the micropore volume from the total pore volume. Pore size distri-
bution of the activated carbons was obtained by applying the
micromeritics density functional theory (DFT) method to the nitro-
gen adsorption isotherms using the software supplied by Auto-
sorb-1 C [31]. The microstructures of char and activated carbons
produced from Paulownia wood were examined using scanning
electron microscopy (JEOL JSM-5600 LV Model SEM).
3. Results and discussion
3.1. Yield of activated carbon
The high volatile matter and low ash content of a biomass re-
source make it a good starting material for preparing activated car-
bon [31]. As can be seen from Table 1, the raw material Paulownia
wood used in this study has low ash and high volatile matter con-
tents. The yield of activated carbon was calculated from the weight
of resultant activated carbons divided by the weight of dried Pau-
lownia wood [7,21]. The nal carbonization temperature and
impregnation ratio play an important role on the yield of activated
carbon. As seen in Fig. 1, it is observed that the activated carbon
yields are higher than those of chars with no impregnation in the
carbonization temperature range of 400700 C. The activation of
Paulownia sawdust without ZnCl
2
impregnation resulted in a rela-
tively low active carbon yield in the range of 28.321.9% since a
large amount of carbons were removed as CO, CO
2
, CH
4
and tar
coupling with O and H atoms [32]. The activating agent in the inte-
Table 1
Proximate and ultimate analyses of Paulownia wood and an activated carbon
(prepared at impregnation ratio of 3.0 and carbonization temperature of 400 C).
Analysis Raw material (wt%) Activated carbon (wt%)
Proximate
Moisture 6.50 3.20
Ash 1.06 2.65
Volatile matter 71.80 13.80
Fixed carbon 20.64 80.35
Ultimate
Carbon 44.73 71.36
Hydrogen 6.12 2.25
Oxygen
a
48.28 25.93
Nitrogen 0.87 0.46
H/C molar ratio 1.64 0.38
O/C molar ratio 0.81 0.72
Caloric value (MJ/kg) 20.6 25.3
Empirical formula CH
1.64
O
0.81
N
0.02
CH
0.38
O
0.27
N
0.005
a
By difference.
190 S. Yorgun et al. / Microporous and Mesoporous Materials 122 (2009) 189194
rior of particles produces a dehydrating effect on the already trans-
formed components (cellulose, hemicellulose, and lignin) during
the heat treatment. It is very possible that cross-linking reactions
are predominant in this step with the subsequent reduction in
the exit of volatile matter and tars, leading to high active carbon
yield observed [10,11,23,33,34]. On the contrary, activation with
low ZnCl
2
impregnation ratio resulted in a higher yield range of
38.129.3% since ZnCl
2
selectively stripped H and O away from
the impregnated sample as H
2
O and H
2
rather than hydrocarbons,
CO or CO
2
[32].
In each carbonization temperature, activated carbon yields are
decreasing with increasing impregnation ratio. The behaviour in
the weight loss between 0.5 and 3 impregnation ratios is due to
the larger evolution of volatiles. A similar trend has been reported
in the literature [23,31]. In each impregnation ratio, the yield of
activated carbon also decreased with the increase of nal carbon-
ization temperature because of the promotion of tar volatilization
by higher temperature [21]. This result is in good agreement with
that reported by Qian et al. In their study, the carbonization of cat-
tle-manure compost impregnated with ZnCl
2
was investigated
[21].
From the view of activated carbon yields, ZnCl
2
Works effec-
tively, as an activating agent especially at low carbonization tem-
peratures and impregnation ratios.
3.2. The effect of carbonization temperature on the surface area and
pore volume
In the chemical activation, the nal carbonization temperature
is an important process parameter in determining the surface area
and the pore volume of the activated carbon. The effects of temper-
ature on the surface areas (BET, micropore and mesopore) and pore
volumes (total, micropore, and mesopore) of the activated carbons
are shown in Table 2.
The surface areas and pore volumes of the activated carbons
gradually decreased with increasing nal carbonization tempera-
ture from 400 to 700 C. When the nal carbonization temperature
was raised to 700 C, the S
BET
, S
mi
and S
me
were found as 1264 m
2
/g,
817 m
2
/g and 447 m
2
/g, respectively; and the V
tot
, V
mi
and V
me
were found as 0.6 cm
3
/g, 0.33 cm
3
/g and 0.27 cm
3
/g, respectively.
Qian et al. studied the activation of manure compost by using
ZnCl
2
. They observed a decrease in the surface area and pore vol-
ume with increasing temperature [21]. This decrease can be attrib-
uted to the heat shrinking [35]. Another similar trend has been also
reported by Hayashi et al. in their study of carbonization of lignin
with ZnCl
2
[35].
The effect of ZnCl
2
was also investigated at the nal carboniza-
tion temperatures. ZnCl
2
worked as dehydration reagent and re-
stricted the formation of the tar and promoted charring of carbon
below the nal carbonization temperature of 500 C. Consequently,
the carbon structure was modied and the surface area increased
below 500 C. The maximum surface area of 2620 m
2
/g and the to-
tal pore volume of 1.331 cm
3
/g were obtained at 400 C. However,
above 500 C, ZnCl
2
does not work as an activation reagent, and the
surface area and pore volume decreased because of heat shrinkage
[35]. The micro and mesoporosity percentages at the studied tem-
peratures are also given in Table 2. As can be seen from Table 2, the
micro and mesoporosities also change with the increasing carbon-
ization temperature. The microporosity increased from 50.3% to
61.8% and mesoporosity decreased from 49.7% to 38.2% as temper-
ature increased from 400 to 600 C. After 600 C carbonization
temperature, the microporosity was decreased to the value of
55%. At all nal carbonization temperatures, mixed (micropo-
rous/mesoporous) activated carbons were obtained. Williams
et al. obtained microporous, mesoporous and mixed micropo-
rous/mesoporous activated carbons from activation of bre waste
with ZnCl
2
[34]. Zinc chloride used as the activating agent lowers
the carbonization temperature. According to the obtained results,
activated carbon having high-surface areas (S
BET
, S
mi
, and S
me
)
and pore volumes (V
tot
, V
mi
, and V
me
) was obtained at nal activa-
tion temperature of 400 C.
The nitrogen adsorptiondesorption isotherms for the activated
carbons obtained at various nal carbonization temperatures and
their pore size distributions were investigated. Fig. 2 shows the
adsorptiondesorption isotherms of the activated carbons pre-
pared under different carbonization temperatures. As can be seen
from Fig. 2, at low relative pressures, a rapid increase in the
adsorptiondesorption isotherms is observed, which is followed
by a nearly horizontal plateau at higher relative pressures, indicat-
ing type I of isotherm based on the classication of the Brunauer,
Deming, Deming and Teller (BDDT). The type I isotherm represents
a material with microporous structure. The major uptake occurs at
low relative pressures indicating the formation of highly porous
materials with narrow pore size distribution as shown in Fig. 3.
3.3. The effect of impregnation ratio on the surface area and pore
volume
The surface areas and the pore volumes of the activated carbons
prepared at 400 C carbonization temperature using various
impregnation ratios are shown in Table 3. Paulownia wood char
Fig. 1. The effects of carbonization temperature and impregnation ratio on the yield
of activated carbon.
Table 2
Surface areas and pore volumes of activated carbons at different nal carbonization temperatures (impregnation ratio = 3.0).
Temperature (C) S
BET
(m
2
/g) S
mi
(m
2
/g) S
me
(m
2
/g) V
tot
(cm
3
/g) V
mi
(cm
3
/g) V
me
(cm
3
/g) V
mi
(%) S
mi
(%)
400 2620 1684 934 1.331 0.670 0.661 50.3 64.3
500 2150 1497 653 1.038 0.600 0.438 57.8 69.6
600 1816 1251 565 0.809 0.500 0.309 61.8 68.9
700 1264 817 447 0.600 0.330 0.270 55 64.6
S
BET
: BET surface area, S
mi
: micropore surface area, S
me
: mesopore surface area, V
tot
: total pore volume, V
mi
: micropore volume, V
me
: mesopore volume, V
mi
% = (V
mi
/V
tot
) 100,
S
mi
% = (S
mi
/S
BET
) 100.
S. Yorgun et al. / Microporous and Mesoporous Materials 122 (2009) 189194 191
prepared at the carbonization temperature of 400 C without ZnCl
2
activation had surface area of 257 m
2
/g. The impregnation ratio has
been found to be one of the important parameters in preparation of
activated carbon using chemical activation. The chemical activa-
tion experiments were carried out by applying various impregna-
tion ratios. ZnCl
2
increases the degradation of the carbon
containing raw material structures. Thus, during carbonization, a
dehydration of the raw material occurs, which results in charring
and aromatization of the carbon skeleton and creation of the por-
ous structure [8,23,36]. The surface areas and pore volumes of the
activated carbon increased rapidly with increasing the impregna-
tion ratio up to 3.0. Similar results were obtained from the chem-
ical activation experiments of bre waste and cattle-manure
compost raw materials with ZnCl
2
[21,34]. The pore volumes of
activated carbon increase at larger values of increasing impregna-
tion ratio, where the attack of the chemical is larger [23]. The V
tot
,
V
mi
and V
me
were found as 1.387 cm
3
/g, 0.69 cm
3
/g and 0.697 cm
3
/
g, respectively, for impregnation ratio of 4.0. Results show that
activated carbon includes micropores and mesopores. The percent-
ages of micropore and mesopore surface areas are varied between
73.3%63.1% and 26.7%36.9%, respectively. In this respect, the
activated carbons with BET surface areas from around 400 m
2
/g
to more than 2700 m
2
/g have been prepared. Such high-surface
areas are comparable to commercially produced activated carbons
which typically range from 500 to 2000 m
2
/g [34]. The nitrogen
adsorptiondesorption isotherm and pore size distribution for acti-
Fig. 2. Nitrogen adsorptiondesorption isotherms for prepared activated carbons
with variable temperature (impregnation ratio = 3.0).
Fig. 3. Pore size distribution of prepared activated carbons with variable temper-
ature (impregnation ratio = 3.0).
Table 3
Surface areas and pore volumes of activated carbons at different impregnation ratios (T
carb
= 400 C).
Impregnation ratio S
BET
(m
2
/g) S
mi
(m
2
/g) S
me
(m
2
/g) V
tot
(cm
3
/g) V
mi
(cm
3
/g) V
me
(cm
3
/g) V
mi
(%) S
mi
(%)
0 257
0.5 424
1.0 977 716 261 0.516 0.27 0.246 52.3 73.3
2.0 1312 901 411 0.685 0.36 0.325 52.5 68.7
3.0 2620 1684 936 1.331 0.67 0.661 50.3 64.3
4.0 2736 1727 1009 1.387 0.69 0.697 49.7 63.1
S
BET
: BET surface area, S
mi
: micropore surface area, S
me
: mesopore surface area, V
tot
: total pore volume, V
mi
: micropore volume, V
me
: mesopore volume, V
mi
% = (V
mi
/V
tot
) 100,
S
mi
% = (S
mi
/S
BET
) 100.
Fig. 4. Nitrogen adsorptiondesorption isotherms for prepared activated carbons
with variable impregnation ratio (T
carb
= 400 C).
Fig. 5. Pore size distribution of prepared activated carbons with variable impreg-
nation ratio (T
carb
= 400 C).
192 S. Yorgun et al. / Microporous and Mesoporous Materials 122 (2009) 189194
vated carbons prepared by applying various impregnation ratios
are given in Fig. 4 and Fig. 5, respectively.
From Fig. 4, all of the isotherms are essentially type I in the
BDDT classication, which is characteristic of adsorption on a
microporous adsorbent. From Fig. 5, it is obvious that the impreg-
nation ratio gives signicant effect on the pore structure of acti-
vated carbon.
3.4. SEM examinations of char and produced activated carbon
The SEM micrographs of a char and two activated carbons are
given in Fig. 6. As can be seen from Fig. 6a, there is no enough
and successful pore development in the char obtained at 400 C
without activation. However, there is a good and successful pore
development in the activated carbon obtained at 400 C with
impregnation ratio of 3.0. In addition, the effect of pore develop-
ment was also reected to the surface area. The activated carbon
obtained at 400 C had a regular and highly porous surface, indicat-
ing higher surface area. The lower surface area of the char (257 m
2
/
g) was increased to the 2620 m
2
/g in the case of activated carbon.
According to Fig. 6b, a fully developed pore structure similar to
honeycomb voids, was observed in the activated carbon obtained
at 400 C. The corner lines of the hole openings can be clearly
shown [6]. Therefore, the ZnCl
2
is an effective activating agent to
obtain activated carbon having high-surface area. The effect of acti-
vation temperature at the constant impregnation ratio is clearly
shown in Fig. 6b and c. According to Fig. 6b and c, the pore struc-
ture of the activated carbon obtained at 600 C is irregular with re-
spect to the activated carbon obtained at 400 C. It can be
attributed to the collapsing of pore and heat shrinking [21,35] with
the increasing activation temperature. As a result of pore collaps-
ing and shrinking, the surface area and total pore volume were re-
duced from 2620 to 1816 m
2
/g and from 1.331 to 0.809 cm
3
/g,
respectively.
4. Conclusion
Paulownia wood (P. tomentose) was used as a raw material to
prepare activated carbons by chemical activation method with
ZnCl
2
. Carbonization experiments were conducted at various
impregnation ratios (0.54.0) and nal carbonization temperatures
(400700 C). The chemically activated carbons are found to be of
mainly type I which are essentially microporous structure materi-
als. The prepared activated carbons have both a high pore volume
and a very large BET surface area. It was found that the specic sur-
face area and total pore volume of the activated carbon were
2736 m
2
/g and 1.387 cm
3
/g, respectively, at a nal carbonization
temperature of 400 C and at an impregnation of 4.0. The activation
agent, ZnCl
2
, worked affectively below 500 C. The effect of the in-
crease in the impregnation ratio on the surface area and total pore
volume of the activated carbon is stronger than that of the rise in
the nal carbonization temperature. According to the results of this
study, it can be said that the Paulownia wood can be effectively
used as a raw material for the preparation of activated carbon
using chemical activation procedure. In addition, the raw material
is found in abundance and therefore the carbon cost is expected to
be economical. As a result, the activated carbon product with high-
surface area obtained in this study can be used as a very promising
adsorbent for pollution control and other applications.
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