25
ADSORPTION OF BTX VAPORS ON ACTIVATED CARBON PELLETS
PREPARED FROM WASTE CASHEW NUT SHELL
Vani Daptardar,
Department of Chemical Engineering,
M.V.J. College of Engineering,
Bangalore, India
Vani.sd26@gmail.com
Abstract— Activated carbon was produced from
Anacardium occidentale (Cashew nut) shell waste by
chemical impregnation and later the material was
carbonized using microwave irradiation at
optimized carbonization conditions. Activated
carbon obtained by carbonizing at 500 ºC for 90
minutes showed better pore development which was
confirmed by SEM(Scanning Electron Microscope)
image, iodine number and methylene blue number.
The proximate and ultimate analysis was carried out
for quantitative analysis of components in activated
carbon. Freundlich isotherm was found to agree
with the equilibrium data in the removal of BTX
(Benzene, Toluene, Xylene) vapors and the fit was
best suited for absorption of benzene. The effect of
change in bed height, particle size of adsorbent,
molecular size of adsorbate and the inlet
concentration of the gas stream on the removal of
BTX vapors were studied by plotting breakthrough
curves.
Keywords- Activated Carbon, Adsorption, Cashew Nut
Shell, H3PO4 Impregnation, Microwave Irradiation,
BTX.
I. INTRODUCTION
BTX vapors which are categorized as Volatile
organic compounds are critical toxic gases which have
significant effects on the eyes, nose and long-term
exposure may even cause cancer. Some of the BTXs are
toxic, potentially carcinogenic and mutagenic at high
concentration levels, found in urban environment.
Environment authorities are particular concerned about
BTX vapors emissions because of their potential to
contribute to the formation of ground level ozone and to
global warming due to its photochemical reactivity.
At a low-concentration level, adsorption of BTX
vapors on active carbon is the most employed method
for the removal of BTX vapors [1]. Cashew nut is
abundantly grown in Western Ghats of India. The nuts
are separated from the shell and cashew nut shell liquid
Vani Daptardar, Deepti Koti, Dr. Rajmohan
JEST-M, Vol 4, Issue 4, Jan-2015
Deepti Koti, Dr. Rajmohan
Department of Chemical Engineering,
NITK, Surathkal,
India
(CNSL) is extracted from the waste cashew nut shells.
After extracting the cashew oil from the cashew nut
shells, the waste shells after extracting oil are burnt in
incinerators, which causes many environmental
problems by emission of particulate and gaseous waste.
The study is carried out to prepare activated carbon from
these shells and use the prepared activated carbon to
adsorb the BTX vapors at artificially generated gaseous
source.
Conventional methods of carbonization which made
use of furnaces do not ensure a uniform temperature for
different shapes and sizes of chars because of surface
heating from the hearth wall. This generates a thermal
gradient from the hot surface of the char particle to its
interior and impedes the effective removal of gaseous
products to the ambient, thereby resulting in a
detrimental effect on the quality of the activated carbons
prepared. Microwave-induced chemical reactions can be
used to solve the above problems associated with
conventional surface heating because microwave
heating is both internal and volumetric heating.
Therefore, the tremendous thermal gradient from the
interior of the char particle to its cool surface allows the
microwave-induced reaction to proceed more quickly
and effectively at a lower bulk temperature, resulting in
energy savings and shortening the processing time [2].
The objectives of present study is to produce and
characterize the activated carbon prepared from cashew
nut shell waste and to optimize the operating conditions
like carbonization temperature and time. The pellets are
formed with the prepared activated carbon which are
used to adsorb BTX vapors. Finally characteristics of
breakthrough curve for the adsorption BTX vapors are
analyzed in packed bed by varying the parameters like
bed height, particle size of adsorbent, molecular size of
adsorbate and the inlet concentration of the gas stream.
Cashew nut shell waste used in the present study
was obtained from ACHAL INDUSTRIES,
Baikampady Industrial Estate, Mangalore. Cashew nut
26
shell liquid was extracted from the shells in Soxhlet
apparatus using acetone as an extraction solvent.
II. EXPERIMENTAL
A. Preparation of activated carbon
The cashew nut shells are washed with distilled
water and dried. The dried material was impregnated at
room temperature in 2:1 H3PO4 for 24 hours. The
sample was washed and dried at 110 ºC in hot air oven.
Later it was subjected to carbonization to form activated
carbon under inert gas environment. The carbonization
temperature is varied from 500oC to 700oC and holding
time is varied from 60 min to 120 min to optimize the
conditions to obtain the activated carbon with well
developed pores. Nitrogen gas was used as inert gas at
flow rate of 150 ml/min. The carbonized product was
powdered and activated carbon pellets of 5mm and 9mm
diameter are formed using hot bitumen as a binding
agent.
B. Characterization of the produced activated carbon
1) Proximate and Ultimate analysis
The proximate analysis for activated carbon
was carried out according to ASTM D 3172-3175
standards and the results were expressed in terms of
moisture, volatile matter, ash and fixed carbon contents.
The ultimate analysis was calculated theoretically using
empirical formulae [3] as given below:
Carbon % = 0.97FC + 0.7 (VM- 0.1A) – M (0.6-0.01M)
Hydrogen, % = 0.036FC + 0.086 (VM- ).1A) – 0.0035M2 (1- 0.02M)
Nitrogen, % = 2.10 – 0.020VM
Oxygen, % = 100 – (C+ H+ N+ ash)
where FC = fixed carbon content, VM = volatile matter content, A =
ash content, M = moisture content.
2) Iodine number
The iodine was carried out according to ASTM D 4607-
94. Iodine number is a indicator of porosity in activated
carbon. It is used as an approximation for surface area of
activated carbon. Iodine number is defined as the
amount of iodine adsorbed (mg) from aqueous phase by
1 g of activated carbon. Higher iodine number indicates
the higher adsorption capacity of iodine molecules by
the AC prepared.
Vani Daptardar, Deepti Koti, Dr. Rajmohan
JEST-M, Vol 4, Issue 4, Jan-2015
3) Methylene blue number
Methylene blue (MB) adsorption tests were conducted
by mixing 0.3 g of the prepared activated carbon with
100 mL of 1000 mg/L MB solution. After agitation for
24 h, the suspension was filtered and the MB residual
concentration was measured at 660 nm, using Hitachi
UV/Vis spectrophotometer.
C. Experimental set-up
The experimental set up consists of a vapor
generation unit and a fixed bed column for adsorption.
Adsorption experiments were conducted at room
temperature. A synthetic gas stream containing BTX ,
vapors are produced by passing air from compressor
through air pre-heater. The hot air was then passed to an
aspirator bottle containing BTX liquid. The flow rate of
the stream was controlled by an air rotameter. The
synthetic gas effluent thus produced was fed at the
bottom (inlet) of the column
The packed bed was filled with activated carbon
pellets. Sampling ports were provided at the inlet and
outlet of each bed for drawing the gaseous samples at
regular intervals of time.
Adsorption experiments were carried out for
different particle size of the adsorbent, different inlet
concentrations of inlet gas stream in continuous mode
with a single stage and multistage adsorption for three
different BTX vapor streams.
D. Analytical measurement
Analysis of gas samples was carried out in Shimadzu
Gas Chromatography using flame ionization detector.
GC was operated in split mode with split flow of 30
ml/min. The injector and detector temperatures were
maintained at 200 and 250 ºC respectively. The
temperature of the oven was gradually increased from
40 ºC at 2 ºC/ min. to 350 ºC for 20 min. Nitrogen gas at
2 mL/min. was used as a carrier gas.
III. RESULTS AND DISCUSSION
A. Analysis of pore structure using SEM
The Pores of various sizes could be observed on the
surface, indicating homogeneous and to some extent of
heterogeneous nature of the activated carbon. Figure 1
shows the SEM image of prepared activated carbon
indicating development of the pores on the surface of
the AC.
27 JEST-M, Vol 4, Issue 4, Jan-2015

Table 2 shows the results of proximate and ultimate

analyses. The result of proximate analysis of the sample
is compatible to ASTM D 3176.

Table 2: Proximate and Ultimate analyses of raw CNSH and activated

carbon sample
Parameters Raw CNSH Activated carbon

Moisture (%) 8.87 1.7

Ash (%) 1.82 3.5
Volatile matter (%) 53.59 28.9
Fixed carbon (%) 35.71 65.9
C (%) 67.49 83.88
H (%) 5.65 4.81
N (%) 1.02 1.52
O (by difference, %) 25.84 9.78
Figure 1: SEM image of activated carbon prepared

B. Iodine number and Methylene blue number D. Freundlich Isotherm

Table 1 shows the iodine number and methylene The experimental adsorption data for benzene,
blue number for all the activated carbon samples toluene and xylene vapors fit to an isotherm was given
prepared at different temperatures and holding time. by Freundlich and Kuster. That is
Activated carbon prepared at 700 ºC carbonization
temperature, with holding time of 90 min, Sample No. 8, log q = log k + (1/n)log C
BTX K n R
Table 3 shows Freundlich parameters for adsorption
Benzene 20 3.52 0.99 of BTX vapors. It can be seen from the value of R that
Toluene 5.16 1.33 0.98 Freundlich equations provides an adequate fit to the
adsorption data for for benzene vapors.
Xylene 10.99 1.49 0.99
Table 3: Freundlich isotherm constants for BTX vapor adsorption
shows the highest iodine number and methylene blue
number.
E. Effect of bed height of adsorbent on breakthrough
Table 1: Iodine number of AC with respect to time and
temperature curve

Sample AC Sample Iodine number MB number Figure 2 shows effect of bed height on adsorption
no. specification (mg/g) (mg/g) process. The residence time of the gaseous effluent
1 500o C, 60 min. 756.81 178.5 increases with increase in the amount of adsorbent in the
2 500o C, 90 min. 736.91 178.1
bed. Thus, increasing the contact time between the
3 500o C , 120 min. 705.55 190.0
4 600o C, 60 min. 893.70 191.0 benzene molecules and adsorbent, and increase in the
5 600o C, 90 min. 909.38 191.0 availability of active sites for adsorption has favored the
6 600o C, 120 min. 705.55 189.5 adsorption process.
7 700o C, 60 min. 689.87 189.0
8 700o C, 90 min. 1003.45 193.5
9 700o C, 120 min. 799.63 182.5
10 800o C, 60 min. 705.55 183.0
11 800o C, 90 min. 674.20 188.5
12 800o C, 120 min. 564.44 178.5
13 500o C, 60 min. 736.91 178.0

C. Proximate and Ultimate analyses

Vani Daptardar, Deepti Koti, Dr. Rajmohan

28
Figure 2: Breakthrough curves for the adsorption of toluene vapors on
activated carbon of 5 mm pellets for different bed heights
F. Effect of particle size of adsorbate on breakthrough
curve
Figure 3 shows that the adsorption is stronger when
smaller molecules of adsorbate are involved, that means
when pores are just large enough to permit the adsorbate
molecules to enter into them. In addition smaller
molecules move at greater velocity and diffuse much
faster into pores than the larger molecules. Benzene
vapor being smallest among the three BTXs considered
here has least saturation time and xylene vapor has
highest saturation time.
Figure 3: Breakthrough curves for the adsorption of benzene, toluene
and xylene
G. Effect of particle size of packing material on
breakthrough curve
Figure 4 shows that benzene vapors were saturated
in 6.5 hours when the size of the activated carbon pellets
of 5 mm were considered. While it took 4 hours for
when activated carbon pellets of 9 mm were considered.
This is attributed to the fact that 5 mm particle size
pellet is having larger surface area than that for 9 mm
Vani Daptardar, Deepti Koti, Dr. Rajmohan
JEST-M, Vol 4, Issue 4, Jan-2015
pellet. Hence, the adsorption capacity also increases in
case of 5 mm pellet size.
Figure 4: Breakthrough curves for the adsorption of benzene vapors on
adsorbent of different pellet sizes and bed height of 5 cm.
H. Effect of inlet concentration of Benzene vapors on
breakthrough curve
Figure 5 shows that higher the concentration of
adsorbate, faster is the breakthrough time. Also, the
slope of the breakthrough curve was gradually
increased. As the inlet concentration of benzene vapor
was increased from 181.29 ppm to 637.88 ppm, the
saturation time was decreased from 10 hours to 5 hours.
This is explained by the fact that allowable adsorbate
molecules are increased as inlet concentration was
increased. Also, adsorption is faster when there is
increase in diffusion velocity and adsorption velocity
into pores of activated carbon. At any given inlet
concentration the outlet concentration increases with
increase in time after breakpoint is reached. Therefore,
the saturation of the adsorbent bed is delayed and occurs
in relatively longer time.
Figure 5: Breakthrough curves for the adsorption of benzene on 5 mm
pellets and 5 cm bed height for various inlet concentrations
29 JEST-M, Vol 4, Issue 4, Jan-2015

IV. CONCLUSIONS
Activated carbon was produced and optimized from
cashew nut seed husk by impregnating with 2:1 H3PO4
and then carbonizing using microwave irradiation. SEM
images indicated that pore development was better in
case of activated carbon prepared at 700 ºC for 90 min.
which was indicated by the values of Iodine Number
and Methylene Blue Number. Adsorption equilibrium
data were fitted to Freundlich isotherm, which described
satisfactorily. The study on the effect of packed bed
height in MSPB column on breakthrough curve yielded
longer breakthrough time with increase in bed height
which means, with increase in mass loading of
adsorbent, the breakthrough time was extended. Increase
in mass loading increases the number of active sites for
adsorption there by increasing the adsorption followed
by longer breakthrough time in MSPB column. On the
basis of the experimental data, CNSH can be used to
remove BTX vapors from gaseous effluent. The method
is simple, economic, eco-friendly and can be used for
minimization of the waste management problem.
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Vani Daptardar, Deepti Koti, Dr. Rajmohan