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Synthesis and Characterization of Composite of

TiO2/Activated Carbon from Activated Carbon Bunch by


Hydrothermal Method
Meidita Kemala Sari1, Feby Rahmawati2, Afra Najiyah Amatullah3, Allwar4,
Chemistry Department, Faculty Mathematics and Natural Sciences
Universitas Islam Indonesia
Jl. Kaliurang KM. 14,5 Sleman Yogyakarta, Indonesia
Corresponding author: 15612065@students.uii.ac.id

Abstrack--Composite of TiO2/activated carbon (TiO2/AC) Composites are a new type of engineered material
has been successfully synthesized by hydrothermal method. comprising two or more materials in which the properties
Composite of TiO2/AC was synthesized from activated of each material differ from each other whether chemical
carbon by mixing with TiO2 powder in liquid phase using or physical and remain separate in the final product.
ethanol and treated with hydrothermal at a temperature of Therefore, it needs the addition of wetting agent as a
250oC for 3 hours. Comparison study of surface area binder [4]. Composite applications are numerous as
between activated carbon and composite of TiO2/AC reinforcing agents, catalysts and adsorbents. In this study,
indicate that surface area decrease from 67.658 to 30,615 composite of TiO2/AC was each composed of activated
m2/g. However, XRD analysis shows that there is slight
carbon mixed with TiO2 powders.
different hkl phase. Characterization using FTIR show that
the composite of TiO2/AC has similar functional group with
activated carbon.
The use of hydrothermal method is by dissolving the
mixture of carbon and solvent-given activator. The
hydrothermal principle is to reduce the stress value of the
Keywords--Activated Carbon, Composite, Hydrothermal, material by breaking the bonds of the amorphous
TiO2.
compound in the material with water vapour at a certain
I. INTRODUCTION temperature so that it is expected to increase the particle
size [3]. In the study of Zhang (2011) He said that the
Carbon is the constituent of plant body. Almost all solvent can be used in controlling the morphology of the
parts of plant body contain carbon such as lignin, surface of a material to be synthesized. The mixed carbon
cellulose and hemicellulose. These three compounds are mixture and activator are then heated at high temperatures
the most abundant type of carbohydrate derived polymer causing good mixing so that the composite is perfectly
in plants. Lignin is a polymer compound which have formed.
much composed of carbon, hydrogen and oxygen, but the
proportion of carbon is much higher than other In Abussaud's (2015) study, the production of
carbohydrate compounds. So the plants can be taken the chemically activated carbon with Aluminium nitrate
carbon and applied to adsorbent, catalyst and mixture to activator forming C-Al and titanium isopropoxide
become a new compound. The most plant part of plant forming C-Ti for the application of phenol degradation,
contains lignin is palm shell. In palm oil, cultivation Al and Ti which is carried on carbon capable of absorbing
process generally produced a lot of palm oil shell waste. phenol well in solution form. In previous study, the
So it is necessary to utilization the palm oil shell. activated carbon was bonded with many types of surface
Research on the utilization of palm shell made into active functional groups such as hydroxyl, carbonyl C=C on the
carbon was done by [2], oil palm shell treated by furnace surface Allwar (2014).
at a temperature of 900oC and then activated with HNO 3
and used as heavy metal adsorbent. The goal of this study is to synthesize of TiO 2/AC
composite from waste of oil palm shell and study its
One of carbon function is as a good absorbent characterization. Characterizations were carried out by
material, therefore the necessary for increased use of the FTIR to see the functional groups, XRD to see the
carbon as an adsorbent is one form of utilization of solid composite crystals and SAA phases to determine the
waste processing of oil palm. However indirect carbon in composite surface area. The process of composite of
oil palm shell can be used as an adsorbent. Preparation of TiO2/AC was prepared by the chemical process.
activated carbon needs physical and chemical treatment
such as carbonization, hydrothermal, chemical activation, II. MATERIALS AND METHODS
inert gas [7]. The addition of activator can improve its
porous structure quality by increasing surface area. The A. Materials
carbon that is powered up through activation is called A set of Herma and Iwaki Glassware, Porcelain
activated carbon. Grille, Glass Stirrer, Spatula, Purple Spoon, Memmert
Oven, Magnetic Stirrer Labinco, Sartorius Analytic
Balance. Perkin-Elmer, X-Ray Diffraction (XRD), and being N2. The data obtained by the adsorption and
Surface Area Analysis (SAA) Quantachrome. desorption process and the calculation of BET to obtain
the Composite surface area.
Activated carbon, TiO2 Merck powder, Ethanol pa
Merck, distilled water and aquatridest. III. RESULTS AND DISCUSSION
A. Hydrothermal method
B. Preparation of composite of TiO2/AC This hydrothermal process helps the composite
A total of 290 grams of activated carbon mixed with formation process under low temperature and pressure.
TiO2 powder as much as 58.5 grams and given a solvent The mixture of activated carbon and metal oxide was
of ethanol pa until completely immersed while stirring carried out into aquatridest (triple-distilled water) media
slowly using a glass stirrer. Then stirring and heating and heated in the hydrothermal reactor at temperature of
using a magnetic stirrer for ± 1 hour, do until ethanol pa 250oC under pressure of 5-6 bar for 3h. After cooling
decreases and looks absorbed in the mixture. After that down, the composite was taken out and kept in desiccator
left until the mixture is not so hot. Add distilled water for further analysis.
until the mixture is completely submerged and left for 1
night. B. Characterization by FTIR
Characterization of composite of TiO2/AC was
After leaving 1 night throw away the distilled water conducted using FTIR to determine the functional groups
and do the washing on the mixture of activated carbon present in the composite.
and TiO2 using distilled water as much as 2 times. Then
dry the mixture in the oven at 110oC.

After that, weigh about ± 70 grams of activated


carbon mixture and TiO2 in a hydrothermal tool and add
aquatridest until submerged. Leave about ± 10 cm of
space from the hydrothermal cap. In order to mix the
composite and metal oxide process is perfect. Perform
hydrothermal process for 3 hours at a temperature of
250oC.

After that, composite of TiO2/AC was washed with


distilled water of 50 mL for 3 times or until the water
washed clear. Then dry for 1 hour in the oven at 110 oC.
Weigh the final result after cool. Obtained the results is
286 grams.

C. Characterization of composite of TiO2/AC


Characterization aims to determine the conditions of
the composites that have been made. In this research,
characterization is done using FTIR, XRD and SAA.

As a comparison of the untreated activated carbon


added metal oxide do characterization with FTIR, XRD
and SAA.

Characterization of composite of TiO2/AC using B


FTIR to see functional groups retained in the composite
[9]. Taken sufficiently each composite ± 1 spoon of and
directly analyzed using FTIR U200 Diamond. Read the
peak generated and specify the functional group.

Characterization of composite of TiO2/AC using


XRD to know the crystal phase formed [4]. Taken
sufficiently each composite and placed in a small vial
bottle. The composites were analyzed using XRD with Cu
cathode ray source. Diffractogram data are matched to
existing standards and JCPDS so that the crystal phase
can be known.

Characterization of composite of TiO2/AC using


surface area analyzer (SAA) to determine the composite
surface area formed [5]. Taken sufficiently each Fig 1. Spectra IR A. Activated carbon C-600 and B. Composite of
composite and placed in a small vial bottle. The TiO2/AC.
composite was analyzed using SAA with the flowed gas
TABLE I. FTIR spectra of activated carbon TiO2/Activated carbon
Wavenumber
N Functional
Activated Composite of
o groups
carbon (cm-1) TiO2/AC (cm-1) a. Activated Carbon
1 2323,76 2330,7 C≡C Based on diffractogram data of activated carbon can
2 1987,41 1982,87 C=C be known that the phase is highly amorphous structure.
3 1002 1561,7 C-C For 2θ which has a high intensity of 22.875 o; 26,516o; and
4 450-471 443,45 C-Ti-O 50.069o. The hkl values of each order of 2θ are [1,2,1]:
[1,1,1]: [1,-1,1]. Amorphous can be known from the
process of irradiation by x-rays, where the greater the
Characteristic found in the activated carbon is the angle 2θ the irradiation beam is more irregular so that the
diversity of bonds between carbons. In Wave Numbers result will be unreadable peak. Amorphous is a solid
2323,76 cm-1 is characteristic of C≡C, the wave number which constituent particles have no perfect order.
1987,41 cm-1 is characteristic of C=C, at wave number
1002 cm-1 is characteristic of C-C, and at wave number b. Composite of TiO2/AC
450-471 cm-1 is characteristic of short alkyl bonds [8]. Based on diffractogram data it can be seen that the
Short alkyl is characteristic of the Activated carbon where composite of TiO2/AC phase is amorphous. For 2θ which
only short-bonded C atoms form cyclic and irregular has a high intensity of 25,307 o; 38,445o; 47,919; 54,913;
acyclic. and 62,597o. The hkl values of each order of 2θ are
[1,1,1]; [-1,1,1]; [-1,1,-1] ; [-1,-1,-1]; and [1-,1,1].
A functional group of C≡C absorbed by composite However, amorphous structure can be known from the
of TiO2/AC attached to the composite of TiO2/AC is process of irradiation by x-rays, where the greater the
found, the C≡C group in this case is found in the 2330,7 angle 2θ the irradiation beam is more irregular so that the
cm-1 range. In wave number 1982,87 cm -1 is characteristic result will be unreadable peak.
of C=C, at wave number 1561,7 cm-1 is characteristic of
C-C. While the characteristic of composite of TiO2/AC is D. Characterization by SAA
found composite of TiO2/AC bond at wave number
443,45 cm-1.

C. Characterization by XRD
Characterization of composite of TiO2/AC using
XRD aims to determine the composite phase and unit cell
dimension. Based on data obtained diffractogram:

Fig 3. Curve adsorption of activated carbon and composite TiO2/AC

Characterization of composite of TiO2/AC using


SAA was determined to study its pore structure. In the
curve we know Composite TiO2/AC have monolayer.
Fig 2. Diffractogram A. Activated carbon and B. Composite of TiO2/AC Carbon that has been activated both chemically and
physically will change shape, one of which is a change in
the surface area of the pore on carbon. Surface area of [3] Arief, M. “Sintesis dan Karakterisasi Nanopartikel Seng Oksida
(ZnO) dengan Metode Proses Pengendapan Kimia Basah
activated carbon and composite of TiO2/was evaluated by dan Hydrothermal untuk Aplikasi Fotokatalis,” [Skripsi].
the Brunauer, Emmet, and Teller (BET) Methods. The Program Studi Teknik Metalurgi dan Material Fakultas
values of surface area of activated carbon and composite Teknik Universitas Indonesia, hal. 1-81. 2011.
of TiO2/AC are 67,6584 m2/g and 30,6159 m2/g,
respectively. The decreasing of surface area could be [4] Callister, W.D. “Materials Science and Engineering : An
Introduction,” 7nd ed, John Wiley & Sons Inc, New York,
from the additional of TiO 2 attached on the activated 2007.
carbon.
[5] Lakhera, S.K., and Suman, S. “Synthesis and Characterization of
E. Differences of active carbon and composite of TiO2/AC 13X Zeolite/Activated Carbon Composite,” International
Journal of ChemTech Research, 7(3), pp. 1364-1368, 2015.
Based on the results of the carbonization of C-600
carbon, the activated carbon used as the matrix composite [6] Rovikavitch, “Characterisation of Micro-Mesoporous Material from
of TiO2/AC is the activated carbon prepared with Nitrogen and Toluene Adsorption : Experimend and
physically activated carbon process under nitrogen gas at Modelling Langmuir”, Journal of Surface Area, ACS
Publications, 2000.
600oC. Seen from FTIR result with functional group
2323,76 cm-1 C≡C ; 1987,41 cm-1 C=C ; and 1002 cm-1 C- [7] Saragi, T., dan Purba, T.R.” Karakterisasi Nanopartikel ZnO : Studi
C and the 450-471 cm-1 finger region is characteristic of Efek Pelarut Pada Proses Hydrothermal,” Jurnal Material
the short alkyl present in the activated carbon. The dan Energi Indonesia, 6(1), pp. 31-35, 2016.
resulted XRD shows that the phase of the activated [8] Septiani, M. “Pembuatan dan Karaterisasi Katalis TiO 2/Karbon Aktif
carbon is amorphous. Activated carbon has a surface area dengan Metode Solid State,” Jurnal Riset Kimia, 9(1), pp.
of 67.6584 m2/g. Through BET calculations and it is 34-38, 2015.
known that activated carbon is monolayer.
[9] Silverstein, “Penyidikan Spektrometrik Senyawa Organik”. Penerbit
Erlangga, Jakarta, 1981.
Composites made in this study is composites C-
TiO2. The C-TiO2 Composite is a Carbon Metallic [10] Zhang, Y., Chung, J., Myoung, J., Lim, S., “Synthesis of ZnO
Composite, in which the Matrix (main constituent) on the Nanospheres with Uniform Nanopores by a Hydrothermal
composite is carbon and reinforcement (reinforcement) process,” Journal of Physics and Chemistry of Solids, 7(2),
pp. 1548-1553, 2011.
Metal oxide (TiO2) which is embedded in activated
carbon.

Based on the result of characterization of composite


of TiO2/AC showed that the composite was successfully
seen from FTIR result with functional group of 2330,7
cm-1 group C≡C; 1982,87 cm-1 C=C; 1561,7 cm-1 C-C and
the fingerprint area of 443,45 cm-1 indicates C-Ti-O. The
fingerprint region indicates the metal oxide binds to the
activated carbon. Based on the XRD results show that the
TiO2/AC composite phase is amorphous and the surface
area of the composite becomes smaller than the C-600
active carbon that is 30,6159 m2/g is monolayer.

IV. CONCLUSION
In summary, the results of synthesis and
characterization with FTIR, XRD, and SAA instruments
proved that the composite of TiO2/AC was successfully
synthesized from the waste of oil palm shell. The
TiO2/AC composite has an amorphous phase and its
surface area is 30,6159 m2/g relating with monolayer
structure. In the formation of the TiO2/AC composite
hydrothermal process has no effect because ethanol is not
suitable as solvent.

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