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Production of Activated Carbon from Raw Date Palm Fronds by ZnCl2 Activation

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GENERAL AND PHYSICAL J.Chem.Soc.Pak., Vol. 37, No. 06, 2015 1081

Production of Activated Carbon from Raw Date Palm Fronds by ZnCl2 Activation
Ashfaq Ahmad, Hassan Mohammed Al-Swaidan* and Ahmad Hamed Alghamdi
Chemistry Department, College of Science, King Saud University, P.O. Box, 2455,
Riyadh-11451, Kingdom of Saudi Arabia.
hswaidan@ksu.edu.sa*

(Received on 27th January 2015, accepted in revised form 23rd July 2015)

Summary: Annually a large volume of date palm frond waste is produced in Saudi Arabia as a
result of the pruning of date palm trees. In this research activated carbon (AC) was prepared from
date frond through a single step chemical activation method by ZnCl2. The influence of ZnCl2
concentrations (in the range of 0, 20, 40, 60 and 80%) on the surface areas, pore volumes and carbon
yield of ACs prepared from raw date frond (RDF) was studied with various analytical techniques.
The RDF and ACs were characterized by Thermogravimetric Analysis (TGA), nitrogen adsorption
Brunauer-Emmett-Teller (BET) for surface areas and pore volumes, Scanning Electron Microscopy
(SEM) and Energy Dispersive X-ray (EDX) for surface morphology and elemental composition
respectively. In the present study we have obtained the highest BET surface area 1581.67 m2g-1 and
total pore volume 0.629 cm3g-1 at 60 % ZnCl2 concentration. The % yield of ACs increased with
increase in ZnCl2 concentration and reached to 39% at 60 % ZnCl2 concentration. The surface area
obtained in the present study is highest amongst the results report in literature.

Keywords: Activated carbon, Date Palm Fronds, Zinc Chloride Activation, Surface area.

Introduction

Agricultural wastes are important starting

material for the production of ACs. Agro waste Physical and chemical activation methods
produced AC have large surface area and high are used for preparation of ACs. In physical method,
content of carbon materials. ACs is porous, solid and the carbonization of the carbonaceous materials is
black carbonaceous materials [1, 2]. ACs is excellent carried out at high temperature range of 700-1100 ºC
adsorbents because they have high porosity, in inert atmosphere followed by activation with
extremely high surface area, surface reactivity, large oxidizing gases (activating agents) such as oxygen,
adsorption capacity and ease of regeneration [3-5]. steam and CO2. However, in chemical activation the
ACs are widely used in various fields such as carbonization of the precursor materials is carried out
environmental (for gas and air treatment, and at comparatively low temperature (400-700 ºC) in the
wastewater purification), medical (in presence of a chemical activating agent.
pharmaceutical), food (for the decolorization and
purification of vegetable oil and fats) and chemical The carbonization and activation during
(for the recovery of solvents and as catalyst support) chemical activation method occurs at the same time.
industries [6, 7]. ACs are available in three different The advantages of chemical activation method over
forms e.g. powder, granular and fibrous. The most physical activation are: (i) it is a single step process,
frequently used precursor materials for the synthesis (ii) it is carried out at lower temperature and usually
of ACs are coals, polymers, agro biomass (RDF have a better effect on pores development, and (iii)
(lignocellulosic)) and some petroleum based products high carbon yields and low energy cost [24-30].
[8]. The properties of ACs are largely dependent on
the methods of activation and type of the precursor Many researchers have used chemical
materials. Lignocellulosic biomass wastes are very activation method for the production of ACs. In
important as these are abundant in nature and cheaply chemical activation the biomasses are impregnated in
available precursor materials for ACs. Many various chemical activating agents such as
researchers have reported the production of ACs from phosphoric acid (H3PO4) [31], zinc Chloride (ZnCl2)
various sources of lignocellulosic waste materials [32], potassium hydroxide (KOH) [33], sulfuric acid
including coconut shell and husk, [9,10] palm oil (H2SO4) [34], hydrochloric acid (HCl) [35], nitric
shells, [11] cotton stalks [12] durian shell [13] rice acid (HNO3) [36], pyrophosphoric acid (H4P2O7)
husk, [14] jackfruit peel [15], pomegranate seeds [16] [37], sodium hydroxide (NaOH) [38], sodium
sugar cane bagasse [17], hazelnut shell [18], almond chloride (NaCl) [39], potassium carbonate (K2CO3)
shell [19], Woods [20], Olive stone [21], date stone [40], ammonium chloride (NH4Cl) [41], sodium
[22], Walnut shell [23] etc. carbonate (Na2CO3) [42], ferric chloride (FeCl3) [43],
hydrogen peroxide (H2O2) [44] etc.
*
To whom all correspondence should be addressed.
Ashfaq Ahmad et al., J.Chem.Soc.Pak., Vol. 37, No. 06, 2015 1082

The plenty cultivating plant and cash crop in water to eliminate the remaining chemicals. This
Saudi Arabia are the date palm. According to the filtration and washing were continued until the
recent Figures, over 20 million date palm trees are in effluent became neutral. The pH was determined by
Saudi Arabia. During the pruning process around Thermo Scientific (Orion 2 Star) pH meter. The
fifteen branches of frond from each date palm tree are washed ACs samples were dried at 110°C in an oven.
pruned (trim) annually by the cultivator. The weight The charcoal prepared from RDF at 400°C
of each branch of frond is approximately 1 Kilogram. carbonization temperature for 3 h with 20°C min-1
These estimates show that around 300,000 tons of ramp rate without chemical activation was indicated
RDFs are produced annually in Saudi Arabia [45, as RDF 400-3-20. The ACs prepared from RDF at
46]. 400°C carbonization temperature for 3 h with 20°C
min-1 heating ramp rate and various concentration of
KOH was used as an activating agent for
ZnCl2 such as 20%, 40%, 60% and 80% were
preparation of ACs from RDF in our previous
designated as AC20 400-3-20, AC40 400-3-20,
research article [6]. In continuation to our previous
AC60 400-3-20 and AC80 400-3-20 respectively.
study, in the current research work the synthesis of
ACs from RDF were carried out by ZnCl2 activation.
Analysis and Characterization
The influences of various concentration of ZnCl2 on
the surface areas, pore volumes, % yields,
The surface areas and pore volumes
morphological and elemental composition of the ACs
properties of ACs and RDF samples were determined
were investigated.
through the adsorption of nitrogen (N2) gas (at 77K)
Experimental using Micromeritics (Gemini VII, 2390 Surface Area
and Porosity analyzer). The samples were degassed
Materials
under nitrogen flow for 1 h at 150°C to eliminate
RDFs were collected from date plants moisture and gasses before analysis. TGA (TA/TGA
garden in Riyadh (KSA). RDFs were cut it into Q50) was used for thermal behavior of RDF with
pieces of 1 to 3 cm. The pieces were thoroughly heating rate 20°C min-1 under N2 atmosphere until
washed first with tap water and then with distilled 1000°C. The surface morphology and elemental
water to remove the dust, fibers and impurities, etc. composition of RDF and ACs at different ZnCl2
The washed RDFs were dried, at 105°C for 5 h in solutions were analyzed by scanning electron
oven (Gallenkamp size one BS oven), to remove the microscope (SEM) and Energy Dispersive X-ray
moistures content. The dried RDFs were crushed into (EDX) by using JEOL (JSM–6380 LA).
powder and sieved by 0.160 mm mesh (Retsch 4188
type prufsieb/Sieve). Analytical grad chemical such Result and Discussion
as ZnCl2 97% (BDH England) and hydrochloric acid
37 % (Riedel-de Haen USA) were used for activation Thermogravimetric (TGA) analysis
and washing respectively in this research. Double
distilled water was used in the solution preparation TGA was used to measure the amount of
and distilled water was used for washing. weight loss of the RDF with respect to temperature.
Fig. 1 shows the TGA plot of RDF in N2 atmosphere.
Preparation of Activated Carbon The first stage of weight loss start from 50 to 189.67
°C temperature range, which correspond to the loss of
ACs were prepared by first impregnating water and some light volatile compounds. The %
RDFs in ZnCl2 solution followed by carbonization at weight loss at this temperature range is about 4.38%.
400oC for 3 h. Various concentrations such as 20, 40, The temperature range of the second stage start from
60 and 80% of ZnCl2 solutions were prepared by 210-347°C and about 54.40% weight loss occurred.
dissolving ZnCl2 in distilled water [47]. The powder The decomposition of lignocellulosic structure
RDFs (11g) were separately socked in 40 mL ZnCl2 usually starts above 200°C [48]. The high weight loss
solutions at room temperature and allowed for 24 h. occurred in this step was attributed to the swift
The samples were filtered to remove the excess ZnCl2 transformation of hemicelluloses and cellulose to
solution and dried in air circulated oven for 6 h at gases and tars. On the contrary lignin conversion to
120°C. The dried samples were carbonized at 400°C gases and tar was slow. Further, the formation of
for 3 h in muffle furnace (XY-1200 XinYu). The carbon also begins in this step [49, 50]. The weight
Prepared ACs were cooled at room temperature and loss in the 3rd step gradually decreased. Most of the
then washed with 0.5 mol.L-1 HCl solution to remove lignin decomposes above 350°C and up to 1000°C in
the excess chloride ions. All the samples were this step. Thermogravimetric analysis TGA reveals
washed several times with hot water and distilled that carbonization RDF occurs at~ 400°C.
Ashfaq Ahmad et al., J.Chem.Soc.Pak., Vol. 37, No. 06, 2015 1083

Yield of Activated carbon

Fig. 2 shows the % yields of ACs prepared

with ZnCl2 concentrations of 20%, 40%, 60% and
80%. The % yield of ACs is calculated using
equation 2. Similar to the BET, mesoporous surface
area and mesopore volume, the % yield of the ACs
increased with increase in the concentration of ZnCl2
until 60%, however, further increase in the ZnCl2
concentration results in the decrease of the % yield.
This decrease in the % yield is attributed the increase
in dehydration, degradation and condensation
reaction in lignocellulosic precursor with increase in
ZnCl2 concentration. These reactions result in
increased evolution of gaseous products from the
Fig. 1: Typical TGA diagram of Date Fronds in a hydroaromatic structure of carbonized char.
nitrogen atmosphere.
Yield (%) = WAC / WR *100 (2)
BET Surface Areas, Pore Volumes
where WAC is the dry weight (g) of final AC and WR
The BET, micro and mesopore surface area, is the dry weight (g) of RDF.
total pore volume (Vtotal) and micropore Volume 4
0
(Vmicro) of ACs prepared at different ZnCl2
3
8

concentrations and RDF measured by N2 adsorption

3
6

are given in Table-1. RDF showed low surface area

4.5 m2g-1, which revealed that RDF has a highly
)
3
4

compact structure with almost no porosity. The BET, %

mesopore surface area and mesopore volume of ACs (
3
2

d
l
increased with increase in the ZnCl2 concentration e i
3
0

Y
until 60%. Further increase in the ZnCl2
2
8

concentration to 80%, the mesopore volume

2
6

(calculated using equation1) [16] and the BET

0

2Z
0n

4e
0n

6
0%

8
0
surface area of ACs are decreased. This shows that
C
l2
C
o
n
c
t
r
a
t
i
o
n
(
)
until 60% a well porous structure is formed which is,
however, destroyed when the concentration was
increased to 80%. The maximum BET, mesopore Fig. 2:Effect of ZnCl Concentration on yield of ACs.
2
surface area and mesopore volume obtained for AC
2 -1 2 -1
at 60% ZnCl2 are 1581 m g , 1507 m g and 0.610 SEM Analysis
cm3g-1, respectively. Fig. 3 shows the SEM micrographs of RDF
(a) and AC60 (b) at optimum concentration of ZnCl2
Vmeso = Vtotal – Vmicro (1) (i.e. 60%). Significant changes among the surface
morphologies of RDF and AC60 can be observed.
where Vmeso is the mesopore volume, Vtotal is the total The micrograph in Fig.3a shows a wavy or curvy
pore volume and Vmicro is the micropore volume. surface for RDF. This curvy surface was attributed to
the presence of cellulose, hemicellulose and lignin.
The BET surface area and total pore volume Further no pores and cracks were observed on the
of the present work were compared with ACs surface of RDF. The surface morphology of RDF is
prepared from different raw materials and activated found similar to that of common lignocellulosic
by physical and chemical methods in Table-2. It materials. On the contrary, AC60 exhibited several
could be observed that the AC produced in this large pores and cracks on the surface. The
research work indicated a high BET surface area of development of these pores is attributed to release of
1581 m2g-1 as compare to the values reported in volatile organic and inorganic compounds (Fig. 3 b).
literature. Based on the above results, ZnCl2 is a The high BET surface area of the AC prepared with
promising activating agent for AC preparation from 60% ZnCl2 is attributed to the presence of these pores
RDF. and cracks.
Ashfaq Ahmad et al., J.Chem.Soc.Pak., Vol. 37, No. 06, 2015 1084

Table-1:BET, Surface Areas, Pore Volumes of RDF and ZnCl2 ACs.

BET Surface Micropore Surface Mesopore (External) Total Pore Vol. Micropore Vol. Mesopore Vol.
Label
Area(m2g-1) Area(m2g-1) Surface Area(m2g-1) (cm3g-1) (cm3g-1) (cm3g-1)
RDF
4.6 1.93 2.67 0.003 0.001 0.002
400-3-20
AC20a
572 267 304 0.237 0.114 0.123
400b-3c-20d
AC40
1494 85 1409 0.595 0.025 0.570
400-3-20
AC60
1581 74 1507 0.629 0.019 0.610
400-3-20
AC80
753 235 518 0.309 0.099 0.210
400-3-20
Note: RDF-Raw Date Frond, AC- activated carbon, a-ZnCl2 concentration, b- activation temperature (°C), c- activation time (h), d-ramp rate (°C /min)

Fig. 3: SEM of (a) RDF (b) AC60.

Table-2:Comparative data of the various adsorbent activated by physical and chemical methods
Activation Activating BET Surface Total Pore Vol. Micropore Vol. Mesopore Vol.
Raw Materials Refs.
Method Agent Area (m2g-1) (cm3g-1) (cm3g-1) (cm3g-1)
Palm shell CO2 984 0.76 - - 51
Almond shell Steam 1234 0.90 0.36 - 52
Coconut shell Steam 1054 0.517 0.092 0.019 53
Physical Date stone CO2 604 0.34 0.29 - 22
Activation Date palm
Steam 560 0.292 0.259 0.068 54
branches
Date palm leaves Steam 525 0.309 0.199 0.089 54
Raw Date Frond CO2 1094 0.438 - - 55
Tea Fruit Peel H3PO4 1024 0.746 0.285 0.463 31
Pomegranate
ZnCl2 978 0.563 0.283 0.280 16
seeds
Palm kernel
Chemical KOH 217 0.12 0.11 - 56
shell
Activation
Date stone ZnCl2 951 0.456 0.355 - 57
Date palm stem H3PO4 1100 1.15 - - 58
Grape stalk ZnCl2 1411 0.723 - - 32
Raw Date Frond KOH 250 0.082 - - 6
Chemical Current
Raw Date Frond ZnCl2 1581 0.629 0.019 0.610
Activation Paper

EDX Analysis Carbon and Oxygen contents are the major and
mainly observed elements in both samples. The
The elemental composition of RDF and carbon content in AC60 is 95.03%, which is greater
AC60 was carried out by Energy Dispersive X-ray than the RDF 59.17% and Oxygen percentage in
(EDX) analysis. The elemental analysis of RDF and RDF 34.66%, which is greater than AC60 2.19%.
AC60 prepared at optimal concentration of 60 % The high Carbon% and low Oxygen % in AC60 are
ZnCl2 are shown in Table-3. The carbon, oxygen and attributed to the volatilization of Oxygen and
some other elements contents were determined. Hydrogen atoms.
Ashfaq Ahmad et al., J.Chem.Soc.Pak., Vol. 37, No. 06, 2015 1085

Table-3:Elemental Analysis of (RDF) and AC60. Chemical Activation, Asian J. Chem., 26, 7833
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