Applied Surface Science 299 (2014) 86–91

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Applied Surface Science

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

Preparation and characterization of activated carbon fiber (ACF) from

cotton woven waste
Jieying Zheng, Quanlin Zhao, Zhengfang Ye ∗
Department of Environmental Engineering, Peking University, The Key Laboratory of Water and Sediment Sciences, Ministry of Education,
Beijing 100871, China

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

Article history: In this study, the activated carbon fibers (ACFs) were prepared using cotton woven waste as precursor.
Received 28 October 2013 The cotton woven waste was first partly dissolved by 80% phosphoric acid and then was pre-soaked in
Received in revised form 7.5% diammonium hydrogen phosphate solution. Finally, carbonization and activation were proceeded
18 December 2013
to get ACF. The optimum preparation conditions, including carbonization temperature, carbonization
Accepted 30 January 2014
time, activation temperature and activation time, were chosen by orthogonal design. Nitrogen adsorp-
Available online 6 February 2014
tion/desorption test was conducted to characterize the prepared ACF’s pore structure. Fourier transform
infrared spectroscopy (FTIR) analysis, X-ray photoelectron spectroscopy (XPS) and environmental scan-
Keywords:
Cotton woven waste
ning electron microscope (ESEM) were employed to characterize its chemical properties and morphology.
Activated carbon fiber Adsorption of oilfield wastewater was used to evaluate its adsorption properties. The results show that
N2 adsorption test the prepared ACF is in the form of fiber, with the sectional diameters of 11.7 × 2.6 ␮m and the surface area
XPS of 789 m2 /g. XPS results show that carbon concentration of the prepared ACF is higher than that of the
commercial ACF. When the prepared ACF dosage is 6 g/L, over 80% of COD and over 70% of chrominance
can be removed after 24 h of adsorption at 18 ◦ C.
© 2014 Elsevier B.V. All rights reserved.

Introduction
Activated carbon fiber (ACF) is considered a kind of promis-
ing adsorption material, which can be widely used for treatment
of organic wastewater [1–4] and the recovery of noble metals or
metal adsorption [5,6]. It shows excellent adsorption performances
because of its nano-structure, abundant micrometer porosity, high
specific surface area and narrow pore size distribution. Currently,
the major precursors for producing ACF are rayon, acrylic, polyacry-
lonitrile (PAN), novoloid (novolac resin) and viscose rayon fibers,
etc. ACF can be made from them by pretreatment and subsequent
carbonization and activation [7]. In the traditional technologies, the
high cost of precursor hinders its large-scale application [8]. So it
is essential to find a cheap substitute material for ACF production.
In recent years, great amount of cotton woven waste are pro-
duced, which need to be recycled or disposed effectively. Such
researches have been focused on landfill, incineration, compost-
ing and recycling [9,10]. Since cotton woven waste is composed of
cotton fiber, it may be a potential substitute material for precursor
to produce ACF [11]. In our present work, we investigated the feasi-
bility of cotton woven waste to be used as precursor for production
∗ Corresponding author. Tel.: +86 10 62755914; fax: +86 10 62756526.
E-mail addresses: zhengfangye@163.com, yezhengfangiee@163.com (Z. Ye).
of ACF. Phosphoric acid was used to dissolve cotton woven waste
partly to slightly loose the fibrils bundled together, which makes
its character closer to that of individual cotton fibrils.
The aim of the present work was to prepare ACF using cotton
woven waste as precursor. The pore structure of the prepared ACFs
were evaluated by nitrogen adsorption/desorption test. Fourier
Transform Infrared (FTIR) spectroscopy analysis and X-ray photo-
electron spectroscopy (XPS) were conducted to determine its
chemical properties. Environmental scanning electron microscope
(ESEM) was used to observe its surface morphology. Furthermore,
its adsorption efficiency for treatment of oilfield wastewater was
also evaluated, with commercial ACF as comparison.
Experimental
Materials
In this study, cotton woven waste was collected from tailor’s
shop. It was cut to produce pieces of size 5 × 2.5 cm, washed several
times with deionized water, and then dried at 80 ◦ C for 24 h. High
purity (99.999%) nitrogen gas and carbon dioxide gas (90%) were
purchased from Hengyuantong Gas Co. Ltd. (Beijing, China). Other
chemicals were analytical grade. A commercial ACF (BEGF 1000)
provided by Sutong Carbon Fiber Corporation (Jingsu Province,
China) was used as reference, with the surface area of 950 m2 /g.

0169-4332/$ – see front matter © 2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.apsusc.2014.01.190
 Jieying Zheng et al. / Applied Surface Science 299 (2014) 86–91 87

Preparation of ACF Table 1

Factors and levels of orthogonal design.

The pre-weighed amount of cotton woven (CW) was put into Level Factor
phosphoric acid (80%) solution with the solid loading of 10% (w/v),
(A) (B) (C) Activation (D) Activation
and stirred for 5 min. After 1 h aging, it was taken out and washed Carbonization Carbonization temperature time (min)
by distilled water several times to remove residual solution. The temperature (◦ C) time (min) (◦ C)
pretreated cotton woven (PCW) was dried in an oven at 80 ◦ C for 1 500 30 700 30
24 h, then put out and cooled under ambient temperature for 12 h. 2 600 60 800 60
The cooled PCW was soaked in (NH4 )2 HPO4 solution (7.5%) at room 3 700
temperature for 3 h and then squeezed and dried at 80 ◦ C for 24 h. 4 800

After cooling to ambient temperature, it was transferred to an alu-

mina boat and put into a muffle furnace. The N2 gas was used as
was 6.70 × 10−8 Pa and the take off angle was 90◦ . Survey scans in
protective gas with the flow rate of 600 mL/min. The temperature
the range 0–1000 eV with step size 1 eV and high-resolution scans
raised from 25 ◦ C to 500–800 ◦ C with the rate of 5 ◦ C/min and was
with step size 0.1 eV for C 1s was recorded. The binding energies
kept for 30–60 min to proceed carbonization. Then it was heated
were corrected by referencing to the hydrocarbon component at
to 700–800 ◦ C with the rate of 10 ◦ C/min and kept for 30–60 min
284.8 eV.
to process activation under CO2 atmosphere with the flow rate of
0.5 L/min. After the temperature decreased to 300 ◦ C under N2 flow
naturally, the product was removed from the furnace and cooled to ESEM analysis
ambient temperature. Then it was washed by distilled water until The surface morphology of the prepared ACFs was observed by a
a neutral pH was reached. Finally it was dried at 80 ◦ C for 24 h to Quanta 200FEG environmental scanning electron microscope (FEI,
get ACF. USA).The accelerating voltage was 20 kV and the pressure of the
chamber was 60 Pa.
Characterization of ACFs
Results and discussion
Nitrogen adsorption measurement
Nitrogen adsorption/desorption test was conducted on an ASAP Optimization of ACF’s preparation conditions
2010 gas sorption analyzer (Micromeritics, USA). The N2 apparent
surface area was calculated using the BET equation in the relative Orthogonal design was utilized to optimize the preparation con-
pressure range of 0.07–0.20. The total pore volume was estimated ditions of ACF. L8 (41 × 24 ) orthogonal design (Table 1) was used to
from the amount of N2 adsorbed at p/p0 = 0.99. optimize the preparation conditions, such as carbonization tem-
perature (A), carbonization time (B), activation temperature (C) and
Iodine value measurement activation time (D). The adsorption properties of the prepared ACFs
Iodine value of the prepared ACF was determined according to were evaluated by measuring iodine value, which was determined
Chinese standard GB/T 12496.8-1999. An amount of 0.5 g dried ACF according to Chinese Standard GB/T 12496.8-1999.
was weighed and transferred to a 100 mL iodine flask equipped Table 2 lists the iodine values and range analysis. It can be
with a ground glass stopper. Then 10 mL HCl (10 wt%) was added seen that the sum of iodine value KC2 (3978.8 mg/g) is bigger
to fully wet the sample. The mixture was heated to boil and main- than KC1 (2941.9 mg/g). For other factors, KA3 > KA4 > KA2 > KA1 ,
tained for 30 s. After cooling to room temperature, 50.0 mL iodine KB1 > KB2 , KD1 > KD2 . Thus the optimum preparation conditions are
standard solution (0.1 mol/L) was put into the flask. The flask was as followed: carbonization temperature 700 ◦ C, carbonization time
stoppered and the contents were vigorously shaken for 15 min. 30 min, activation temperature 800 ◦ C, activation time 30 min.
Then the mixture was quickly filtered into a beaker. 10.0 mL filtrate Under this condition, the iodine value of the prepared ACF is
was pipeted into a 250 mL iodine flask and 100 mL water was added. 1146.0 mg/g.
The standardized Na2 S2 O3 solution (0.1 mol/L) was used to titrate F-test was employed to evaluate the influence of the four fac-
until the solution turned to pale yellow. Then 2 mL starch indicator tors. Since carbonization time has little influence on the result, it
solution was added and the titration was continued until the solu- is treated as error term. As can be seen in Table 3, activation tem-
tion became colorless. The iodine value (mg/g) can be calculated perature (with 72.75% contribution) is the most significant factor
according to the following equation: (FC = 35.24 > F0.05 (1, 2) = 18.51). Activation time, carbonization tem-
perature and carbonization time have less influence, respectively.
5 × (10c1 − 1.2c2 V2 ) × 127
iodine value = ×D (1)
m
Table 2
where c1 (mol/L) and c2 (mol/L) are the concentrations of
L8 (41 × 24 ) orthogonal test results.
iodine standard solution and sodium thiosulfate standard solution,
respectively. V2 (mL) is the consumed volume of sodium thiosulfate Sample no. A (◦ C) B (min) C (◦ C) D (min) E Iodine value
(mg/g)
standard solution and m (g) is the mass of ACF. D is the correction
coefficient. 1 500 30 700 30 1 721.6
2 500 60 800 60 2 917.7
3 600 30 700 60 2 680.6
FTIR analysis 4 600 60 800 30 1 999.4
The surface functional groups were investigated by FTIR analysis 5 700 30 800 30 2 1146.0
using a Magna-IR750 spectrometer (NICOLET, USA), with 128 scans 6 700 60 700 60 1 700.1
and a resolution of 8 cm−1 . 7 800 30 800 60 1 915.7
8 800 60 700 30 2 839.6
K1 (mg/g) 1639.3 3463.9 2941.9 3706.6 3336.8
XPS analysis K2 (mg/g) 1680.0 3456.8 3978.8 3214.1 3583.9
XPS analysis was conducted using an Ultra Axis X-ray photo- K3 (mg/g) 1846.1
electron spectrometer (SHIMADZU, Japan) equipped with an K4 (mg/g) 1755.3
R 206.8 7.1 1036.9 492.5 247.1
achromatic Al K␣ X-Ray source. The pressure during the analysis
88 Jieying Zheng et al. / Applied Surface Science 299 (2014) 86–91
Fig. 1. Effect of activation temperature on iodine value.
Since the effect of activation temperature is prominent, we fur-
ther investigated the effect of activation temperature on iodine
value (Fig. 1). When the activation temperature increases from
700 ◦ C to 800 ◦ C, the iodine value increases from 698.4 mg/g to
1146.0 mg/g. However, it decreases to 837.76 mg/g when the
activation temperature increases to 850 ◦ C. This is because CO2
activation can produce pores under high temperatures by reac-
tions between carbon and activating agents. The amorphous carbon
is removed from the network, which causes the change of pore
structure and characters. When the activation temperature further
increases (higher than 800 ◦ C), it may destruct the micropores and
turn them into larger pores, reducing the adsorption ability [12,13].
N2 adsorption/desorption isotherm
The pore structure and specific surface area of an adsorbent can
be obtained by constructing an adsorption–desorption isotherm
of N2 . Fig. 2 shows nitrogen adsorption–desorption isotherms of
the prepared ACF and the commercial ACF. It can be seen that
for the prepared ACF, the volume adsorbed increased quickly
with increasing pressure at low pressure ranges, meaning that
the adsorption isotherm is type I adsorption/desorption, where
microporous adsorption is the prominent adsorption. The volume
adsorbed leveled off when the relative pressure was greater than
0.1. For the commercial ACF, adsorption–desorption hysteresis can
be observed, suggesting that the isotherm is type IV. It proceeds via
multilayer adsorption followed by capillary condensation, which is
resulted from the presence of mesopores embedded in a matrix
[14]. The onset of the hysteresis loop (where p/p0 is about 0.4)
indicates the beginning of the capillary condensation in the pores
[15].
Table 3
F test results.
Sum of squares
(A) Carbonization temperature (◦ C) 12,389
(B) Carbonization time (min) 5.987
(C) Activation temperature (◦ C) 134,343
(D) Activation time (min) 30,304
Error 7619
Error∼ 7625
Sum 184,661
*
Means F > F0.05 .
Fig. 2. N2 adsorption–desorption isotherms.
The results obtained from analyzing the isotherm of ACF with
BJH method [16] show that the specific surface area of the pre-
pared ACF is 789 m2 /g, with the mean diameter of 1.93 nm. The
micropore surface area and mesopore surface area are 502 m2 /g
and 53 m2 /g, respectively. And the micropore volume and meso-
pore volume is 0.224 cm3 /g and 0.0387 cm3 /g, respectively. The
Vmic /Vmes ratio in the prepared ACF is 5.77, which is much higher
than that in commercial ACF (2.69), meaning that more micropores
exist in the prepared ACF than commercial ACF.
FTIR analysis
FTIR is a sensitive technique for surface analysis [17]. It was used
to characterize the surface chemical structure changes of cotton
woven in the preparation process. Fig. 3 shows the spectra of CW
and the prepared ACF.
For CW, eight adsorption peaks can be observed. The peak
at 3336 cm−1 is assigned to intra and intermolecular hydrogen
bonded –OH stretching vibration [18]. The band at 2915 cm−1 cor-
responds to stretching vibration of C–H bond in methylene groups
[19].The peak at 1428 cm−1 is assigned to –CH2 – scissoring vibra-
tion. The band at 1317 cm−1 could be attributed to the deformation
vibration of –OH [20]. The sharp and intense peak at 1161 cm−1
corresponds to the asymmetric stretching vibration of C–O bond
in ester group [21]. The peaks at 1109 cm−1 and 1057 cm−1 corre-
spond to –OH stretching vibrations in polysaccharide molecules.
The peak at 1033 cm−1 is assigned to C–O–C symmetric stretching
vibrations in lactone. These peaks are conformed to the character-
istic of typical cellulose structure.
After carbonization and activation, the peaks at 3336 cm−1
and 2915 cm−1 disappear, and some new peaks appear. The peak
at 1720 cm−1 is assigned to the stretching vibration of C=O in
DOF Variance F-ratio Critical value of F Pure sum Percent (%)
3 4130 1.08 F0.05 (1, 2) = 18.51 F0.05 (3, 2) = 19.16 12,389 6.71
1 5.987 – – –
1 134,343 35.24* 134,343 72.75
1 30,304 7.95 30,304 16.41
1 7619
2 7625 7625 4.13
7 184,661 100
 Jieying Zheng et al. / Applied Surface Science 299 (2014) 86–91
Fig. 3. FTIR spectra of cotton woven and the prepared ACF.
C=C–COO– [22], and the peak at 1580 cm−1 is assigned to the
stretching vibration of C=C [23]. The band at 1080 cm−1 is asymmet-
ric stretching vibration of C–O–C. The peak at 981 cm−1 is assigned
to the wagging vibration of =CH2 in trans vinyl-compounds. The
peaks at 786 cm−1 and 707 cm−1 are characteristic of the out-of-
plane bending vibration of C–H in alkene [24]. This is because –OH
groups are removed in gaseous form by pyrolytic decomposition of
CW during thermal treatment, which are oxidized to C=O groups
and COO– groups [25].
XPS analysis
The XPS technique was used to analyze the atomic concentra-
tion in the surface layer (1–2 nm) of the prepared ACF and the
commercial ACF. For the prepared ACF, the O/C ratio is 0.0845,
which is lower than that of the commercial ACF (0.1590), indicating
that more unsaturated carbon atoms are left on the surface of the
prepared ACF. The surface unsaturated carbon atoms are likely to
attract foreign molecules, as there are imbalanced forces compared
to those within the solids, which can be balanced by interaction
with foreign molecules [26].
High resolution XPS spectra was performed to explore the sur-
face functional and their relative content of ACFs, as seen in Fig. 4
The binding energy of C 1s high-resolution spectra is acquired over
278–302 eV. For the prepared ACF (Fig. 4a), the C 1s spectra can
be fitted to four components corresponding to the C=C (284.8 eV),
C–OH/C–O–C (285.5 eV), C=O(288.0 eV) and COOR (290.0 eV), with
the relative percentages of 40.98%, 25.80%, 9.74% and 23.47%,
respectively. The presence of C=C, C–OH/C–O–C, C=O and –COOR
could be attributed to the carbonization and activation stage. Since
no hydroxy group is observed in the FTIR spectra, it can be inferred
that the peak at 285.5 eV is assigned to C–O–C groups rather than
C–OH groups.
For the commercial ACF (Fig. 4b), the C 1s spectra can be fitted
to three components corresponding to the C=C (284.7 eV), C–O–C
(285.4 eV) and –COOR (288.6 eV), with the relative percentages of
42.64%, 25.11% and 32.24%. No carbonyl groups are detected, mean-
ing that the kinds of groups containing oxygen are less than the
prepared ACF.
Surface morphological observation
Fig. 5 shows the whole morphology of the prepared ACF and
the magnified morphologies of cotton woven, PCW, the prepared
ACF and the commercial ACF. It can be seen that the woven
89
Fig. 4. High resolution C 1s spectra of (a) prepared ACF and (b) commercial ACF.
structure of the prepared ACF (Fig. 5a) remains unchanged, com-
pared with that of the cotton woven. For cotton woven (Fig. 5b), the
surface is smooth and the structure is orderly and compact. After
partly dissolved, the surface became uneven and rough (Fig. 5c).
The structure of the prepared ACF (Fig. 5d) is similar to that of the
commercial ACF (Fig. 5e). It is in the form of fiber, where some long
or short irregular and discontinuous slits can be observed. The sec-
tional dimensions of prepared ACF is about 11.7 × 2.6 ␮m, while the
sectional dimension of commercial ACF is 12.4 × 4.5 ␮m.
Treatment of oilfield wastewater by ACF
In order to assess the adsorption properties of the prepared ACF,
it was used to treat oilfield wastewater generated from Huabei oil-
field [27]. The pre-weighed amount of adsorbent (0.30 g) was put
into a 250 mL flask containing 50 mL water samples. The flasks were
sealed and shaken at 18 ± 1 ◦ C for 24 h. Then the solution was with-
drawn and filtered and the COD was determined. Commercial ACF
was also used for comparison. The COD of the water samples were
determined using potassium dichromate oxidation method (Hach
Heating system, Hach Corporation, USA). The UV–vis spectra of
wastewater samples were determined in the range of 190–1100 nm
by using a UV–Vis spectrophotometer (UV-1800, Shimadzu, Kyoto,
Japan) with a 1 cm quartz cell. The pH of water samples before
and after treatment was measured with pH meter (pH-201, Hanna
Corporation, Woonsocket, RI).
Table 4 lists the change of water qualities before and after
adsorption. It can be seen that the adsorption performance of the
prepared ACF is superior to that of commercial ACF. After adsorp-
tion by the prepared ACF, the color turns from pale yellow to
90 Jieying Zheng et al. / Applied Surface Science 299 (2014) 86–91

Fig. 5. Whole morphology of the prepared ACF (a) and magnified morphologies of (b) cotton woven, (c) PCW, (d) prepared ACF and (e) commercial ACF.

paler (Fig. 6), and the COD decreases from 327.6 mg/L to 54.3 mg/L. pared ACF. Under the same conditions, commercial ACF can only
The COD removal ratio is 83.4%, which is much higher than that reduce the chrominance from 60◦ to 45◦ .
using commercial ACF (18.8%). The chrominance is also reduced Fig. 7 shows the absorption spectra of oilfield wastewater sam-
obviously. It decreases from 60◦ to 10◦ after treatment by the pre- ples before and after adsorption. It can be observed that the
absorbance in UV and visible region changes a little after adsorption
by commercial ACF, meaning that the pollutants containing chro-
Table 4 mophores and auxochromous groups are hardly removed. After
Change of water qualities before and after adsorption. adsorbed by the prepared ACF, the adsorption decreases promi-
Parameters Before After After adsorption nently. The absorbance at 260 nm decreases from 2.58 to 0.589,
adsorption adsorption by by commercial indicating the removal of most pollutants from oilfield wastewa-
prepared ACF ACF ter. It maybe because that the prepared ACF has smaller pore
COD (mg/L) 327.6 54.3 266.0 size (1.93 nm vs. 2.03 nm) and higher ratio of micropore volume
Chrominance (◦ ) 60 10 45 (58.8% vs. 39.9%), which is helpful for increasing adsorption energy
pH 7.8 7.1 7.7 [28].
 Jieying Zheng et al. / Applied Surface Science 299 (2014) 86–91
Fig. 6. Photographs of oilfield wastewater samples before and after adsorption by
ACFs. (For interpretation of the references to color in this figure legend, the reader
is referred to the web version of this article.)
Fig. 7. Absorption spectra of oilfield wastewater samples before and after adsorp-
tion.
Conclusions
In this work, ACFs were prepared using cotton woven waste
as precursors. The optimum preparation condition is determined
as: carbonization at 700 ◦ C for 30 min and activation at 800 ◦ C
for 30 min, where the iodine value of optimum prepared ACF is
1146.0 mg I2 /g C. The sectional diameters of the prepared ACF is
11.7 × 2.6 ␮m and the surface area is 789 m2 /g. For treatment of
industrial wastewater, such as oilfield wastewater, the adsorption
performance of the prepared ACF is superior to that of commercial
ACF. When the ACF dosage is 6 g/L, over 80% of COD and over 70% of
chrominance can be removed after 24 h of adsorption at 18 ◦ C. The
raw material cost is lower than that of commercial ACF, indicating
that cotton woven waste can be used as precursor for producing
ACF.
Acknowledgments
The authors are grateful for the financial support from
International (Regional) Cooperation Projects of the National Nat-
ural Science Foundation of China, whose registered number is
91
20877001. The authors also gratefully acknowledge the refer-
ees for their comments and constructive suggestions, which have
improved the quality of the paper.
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