Synthesis And Characterization N-TiO2-Chitosan Photocatalyst And The

Application As Purification Of Air Embung Unnes

Emas Agus Prastyo Wibowo*, Navela Rahma Aji, Resti Ujiningtyas, Tri Maya Sari, Rahmawati

Chemistry Department, Faculty of Mathematics and Natural Sciences, Semarang State University, Sekaran Gunung
Pati, Semarang, Indonesia

*e-mail: emasagus@ymail.com

Abstract— Nowadays, the condition of water reservoir is alarming because it looks more cloudy and
dirty caused by contamination of waste. So, it can’t be used as the first function as a rain shelter by Unnes
and its surroundings. The purpose of this research is to provide a solution as an effort to return the
function of water ponds with a purifier based on photocatalysts N-TiO2-chitosan, which when exposed to
the UV rays and a visible ray will produce OH radical compounds which serve as degrading organic
pollutants and superoxide compounds functioning kill bacteria. Based on the results of SEM (Scanning
Electron Microscopy), TiO2 can be concluded that: In the SEM magnification 100x, 250x, 500x, and 1000x
seen that the coated material has not been good. It is still lumpy and uneven while based on the results of
XRD, TiO2 crystal size is 13.54 nm. The result of COD and BOD using photocatalyst TiO2-chitosan
decrease from20 ppm to 16.55 ppm and 60.70 ppm to 49.37 ppm (Wibowo et al., 2016). In this research is
added doped N on TiO2-chitosan. So, the using of photocatalyst N-TiO2-chitosan hoped can give the better
result to degrade organic pollutants in water and reduce both COD and BOD.

Keywords—N-TiO2 –chitosan; Photocatalysts; Water reservoir

to hold interaction with at least one reactant molecules to

I. INTRODUCTION
Unnes declared as conservation university on March
12, 2010 by the minister of education and culture, M.Nuh.
Conservation concept is also based on Permendiknas No.
8 of 2011 on the Statute of the Semarang State University.
Conservation has become a very important part for Unnes.
This is demonstrated by the integration of conservation
into the vision and mission of Unnes by statute, namely
university of the conservation of the international are
healthy, superior, and prosperous. In order to realize the
vision of conservation, Unnes has formed a water
reservoir named Embung.At the beginning of
construction, the reservoir is expected to have a primary
function as a rainwater, but in fact the reservoir is also
used as a recreation area of local people and the academic
community Unnes. Therefore, the water reservoir now
appears green because of mossy and appeared unkempt
(Wibowo et al.,016).
In order for optimal function of reservoir needed an
attempt to overcome this problem is by N-TiO2-chitosan
photocatalyst. Photocatalyst is a combination process
between the photochemical process and catalyst.
Photochemical itself is a process of chemical
transformations with the help of light as a trigger. While
the catalyst is a substance that can accelerate the reaction
rate but not to react during the process and at the
beginning until the end of the reaction catalyst amount
remains the same. This is due to the catalyst has the ability
produce more reactive intermediates. The catalyst in this
process as a photocatalyst, so it has an ability to absorb
photons (Prambasto, 2013).
Titanium dioxide has a valence band (VB) is filled and
the conduction band (CB) is empty. If the temperature
rises or the presence of excitation optical (light) energy
that exceeds the energy of Eg, electrons will rise to CB
leaving VB, then there was a hole or a positive charge at
VB.In TiO2 its gap of band is proportional to the light
radiation 388 nm (3.23 eV) in the area near UV (Noqueira
etal.,1993).
Chitosan is a natural polymer types that have the form
of a linear chain, as a product of deacetylation of chitin
through a chemical reaction using a strong base
(Muzzarelly, 1985). Chitosan is poly-D-Glucosamine
(composed of more than 5000 units of glucosamine and
acetylglucosamine) with a molecular weight of more than
one million Dalton, a dietary fiber (fiber that can be eaten)
second after cellulose (Simunek et al., 2006).
A. Objective
The purpose of this paper is to provide a water
purification solution air embung Unnes by purification
with N-TiO2-chitosan photocatalyst.
 II. METHODS
The method used in this paper is a qualitative
descriptive study based literature. Selection of this
approach is expected to describe accurately the state or
certain symptoms of the object of study. In this case I tried
to create an overview of the concept of water purification
through the N-TiO2-chitosan photocatalyst using a water
purifier.
A. Making the solution N-TiO2-chitosan (adopting
research Wibowo et al., 2016)
First, the synthesis of TiO2 nanosol using sol-gel
method with H2O: Ti mole ratio which is 4:1, which is the
ratio of hydrolysis in the synthesis is 30 ml of ethanol,
then added HNO3 to pH 3,5. The ambiance is quite acidic
solution maintained so that hydrolysis does not occur at an
early stage and the precursor solution added (dropped) is
not changed to white (indicative precursor changed and no
longer nanometer sized). Furthermore, the solution is
stirred using a magnetic stirrer for ± 10 minutes so HNO3
added evenly distributed into the solution. Then 3.98 gram
of TIPP added by putting Erlenmeyer containing the
solution and magnetic bar up the digital scales with a scale
of 0 and shed TIPP slowly until the scale figure of 3.97
grams. Then 5 ml of ethanol in beaker glass is placed on
digital scales and added 0,063 rams of distilled water.
Then shed ethanol in the beaker dropwise and shed urea
5% into the solution with stirring for ± 5 hours to become
nanosol. The second step is dissolving the N-TiO2 into
100 ml of 1% acetic acid, and then stirred continuously
and constantly for ± 2 hours. After dissolved, add 0.4
grams of chitosan, stirred quickly for ± 2 hours until clear
sol obtained. Then added 1 M NaOH solution dropwise
into the sol until solution reached pH = 10. And then
continued with the formation of the gel at a temperature of
110-120oC for 15 hours. Gel calcined at a temperature of
450oC for 3 hours to obtain N- TiO2-chitosan powder.
B. Procedure Creation Tool
The tools used is saw.
And the materials used are 7 pieces of plywood
boards, cables, plugs, glass, rope, and lamp.
Fig. 1. Design Process Water Purification of Air Embung Unnes
III. DISCUSSION
A. Mechanism of TiO2 in Decreasing Organic Pollutans
TiO2 can catalyze the reduction and oxidation
reactions. Oxidation reactions can occur due to positive
holes formed during the activation of the photocatalyst
will oxidize the hydroxyl ion or water on the surface of
the catalyst to produce hydroxyl radicalsHO•. These
radicals will oxidize organic compounds in the
wastewater. The mechanism of decreased levels of BOD
and COD using photocatalyst TiO2 and TiO2-N is a redox
reaction where the release and the capture of electrons
were occurred caused by the photon energy of visible
light. Photocatalytic reaction of TiO2 is a combination of
photooxidation reactions and photoreduction preceded by
the adsorption of substrate to the surface of
semiconductor. Photooxidation or photoreduction can
occur because TiO2 is a semiconductor with typical
electronic structure which has a valence band and the
empty conduction band so that when subjected to visible
light it will experience e- excitation from the valence band
to the conduction band (generating e-cb) which led to the
vacancy or hole (h + vb) in the valence band which can
act as a positive charge. The next hole will react with H2O
contained in the solution to form the hydroxyl radical
(•OH), this hydroxyl radical is a powerful oxidant that can
degrade organic compounds into CO2 and water. The
electrons in the semiconductor surfaces can react with the
existing e- catcher in the solution that is O2 forming
superoxide radical (•O2-) which can also degrade organic
compounds in solution (Hoffman et al., 1995).
Radical (•OH) and (•O2-) are formed continuously
during the visible light was still on photocatalysts and will
degrade organic compounds into CO2 and H2O. The
effectiveness of photocatalytic reaction depends on the
competition between the recombination of charge carriers
with the donation of electrons from the substrate to the
hole (h + vb). Recombination of the charge carriers can be
prevented by providing e- catcher in the form of O2that
are adsorbed and become superoxide anion radicals •O2
will oxidize organic compounds. According to Okamoto
et al., (1985) TiO2 photocatalytic mechanism is as
follows:
TiO2 + hv TiO2 (h+ + e-) (1)

H2O + h+ •OH + H+ (2)

OH- + h+ •OH (3)

O2 + e- •O2 (4)

TiO2 (e- + h+) + bahan organik CO2 + H2O (5)

That mechanism be strengthened by Sonawane and

dongare (2006), which describes the mechanism of TiO2 Fig. 3. SEM morphology of TiO2 Magnification 500 x
photocatalyst with the stages as follows :
Based on the results of SEM (Scanning Electron
- + Microscopy) above it can be concluded that : In the SEM
TiO2 + hv TiO2 (e + h ) (6)
magnification 250x and 500x seen that the coated material
has not been good and still lumpy and uneven . This is
because less mixing and aging time that will affect the
h+ + OH-ad •Ohad (7) morphological structure of TiO2 produced.
Based on research of Wibowo et al., 2016 the time
+
h + H2Oad •OHad + H +
(8) required to degrade organic pollutants in this case is the
BOD and COD using TiO2-chitosan are for 30 minutes,
where the levels of BOD has decreased from 20 ppm to
e- + Mn+ M (9) 16,55 ppm while the COD decrease from 60 ppm to 49,37
ppm. In this research is added doped N on TiO2-chitosan.
So, the using of N-TiO2-chitosan photocatalyst hoped can
Hydroxyl radical •OH produced has an important role
give the better result to degrade organic pollutants in
to oxidize organic compounds. The higher the formation
water and reduce both COD and BOD.
of hydroxyl radicals, the greater the photocatalyst ability
to oxidize organic compounds.
C. Superiority
B. Analysis Characteristics of TiO2-Chitosan with Innovation photocatalyst thin layer of nanoparticles of
Scanning Electron Microscopy (SEM) N-TiO2-chitosan as an antibacterial and reducing heavy
metals of air embung Unnes has several advantages,
including:
1. Responsive to visible light
By doping N and chitosan to semiconductor TiO2 will
increase performance of light activation. Before doped
TiO2 is only responsive to UV light, but after doped iw
will increase photorespond of TiO2 to visible light
wavelength region that is for applications solar light (λ >
UV-A, 320 nm) and visible light (> 400 nm)
2. It can improve water quality
Activities semiconductor photocatalyst N-TiO2-
chitosan has anti-bacterial activation in the water
purification process.
Fig. 2. Morphology of TiO2 SEM Magnification 250 x 3. Sustainable
The availability of natural ingredients for
semiconductor TiO2, nitrogen and chitosan in Indonesia
are abundant, so the application of technology
photocatalyst thin layer of semiconductor N-TiO2-chitosan
can take place continously.
4. Optimizing the availability of clean water.
5. Provide solutions to problems of air embung
Unnes.
 IV. CONCLUSION
By using this water purifier hopes can help the problem of
air embung Unnes through photocatalytic process that will
produce superoxide compounds that can degrade organic
pollutants in the water.
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