7

Photocatalytic Decolorization of
Two Remazol Dyes Using TiO2
Impregnated Pumice Composite as
Catalyst
Deniz İzlen Çifçi, Sema Terzi, Süreyya Meriç
DEPARTME NT OF ENVIRONMENTAL ENGINEERING, FACULTY O F ÇORLU ENGINEERING,
NAMIK KEMAL UNIVERSITY, TEKIRDA Ğ, TUR KE Y

7.1 Introduction
Dyes are widely used in textiles, pulp mills, leather, dye synthesis, printing, painting, photog-
raphy, food and plastics industries and most of them display resistance to removal with bio-
logical treatment systems (Çifçi and Meriç, 2015). There have been more than 100,000
commercial dyes and more than 7 3 105 tons of paints registered per year in the world
(Malakootian et al., 2014). Most of the dyes are known to be toxic or carcinogenic, and they
reduce light transmittance in the aquatic environment, thus, advanced treatment methods
are required to remove color and toxic content before discharge (Kanakaraju et al., 2015;
Mahmoun et al., 2013). Photocatalysis is a promising method among the advanced oxidation
processes (AOPs) for the removal of the toxic dyes to carbondioxide and water (Çifçi and
Meriç, 2015). Because TiO2 is not a good adsorbent, the use of TiO2 in combination with a
porous adsorbent, which is owning the high surface area that improves the photocatalytic
activitiy by preventing electron/hole recombination, enhances the aggregation of TiO2 (Li
et al., 2014; Zabihi-Mobarake and Nezamzadeh-Ejhieh, 2015). In addition, other studies have
shown that photocatalytic activity increases with catalysts such as TiO2 supported chitosan,
activated carbon and TiO2 supported zeolite (Wang et al., 2015; Afzal et al., 2017; Bagheri
et al., 2016; Gomez et al., 2013; Omri et al., 2014). However, there have any studies with TiO2
supported pumice up to date. Pumice, which is a volcanic stone, is an intensive porous
material with an average porosity of 90% (Calabrò et al., 2012). As a cheap adsorbent, pum-
ice has become popularly used in the adsorption of heavy metals and dyes (Çifçi and Meriç,
2016). However, there are still few studies on its use as catalyst, in particular, there is no
study reported on TiO2 impregnated pumice yet. This study is a first attempt to evaluate the
decolorization of photocatalysis using TiO2 impregnated pumice composite as catalyst under

Nanotechnology in Water and Wastewater Treatment. DOI: https://doi.org/10.1016/B978-0-12-813902-8.00007-1

© 2019 Elsevier Inc. All rights reserved.
125
126 NANOTECHNOLOGY IN WATER AND WASTEWATER TREATMENT

UV-A illumination. The reusability and stability of composite synthesized was evaluated for
three times. Toxicity of oxidation by-products to Daphnia magna was tested following the
standardized test.

7.2 Materials and Methods

7.2.1 Materials
Titanium isopropoxide (TTIP, 97% CAS#546-68-9) was purchased from Sigma Aldrich.
Ethanol (CAS#102371), HNO3 (CAS#100456) and NaOH (CAS#106462) were purchased from
Merck and used as analytical grade. Distilled water was used in all the experiments. The
pumice was obtained from a company working in Cappadocia region (Nevşehir city,
Turkey), where a large pumice reserve as is present. The particle size of pumice powder ran-
ged from nano to micron (0
125 μm). Remazol red (RR) and remazol brilliant blue (RB)
were purchased from a dye producer industry in Turkey.

7.2.2 Synthesis of TiO2 Impregnated Pumice Composite

TiO2 supported pumice composite was synthesized following the literature with the applica-
tion of some modifications (Kanakaraju et al., 2015; Afzal et al., 2017). Briefly, 10 mL TTIP
was dropped slowly into the 100 mL anhydrous ethanol under continuous stirring at room
temperature. Meanwhile, concentrated nitric acid was dilluted with distilled water with a vol-
ume ratio of 1:5. This solution was added dropwise into the TTIP solution and stirred for
1 hour. After that, pumice was added to the solution at a mass ratio of 2% between TiO2 and
pumice. Than, the solution of pH was adjusted to 4 using concentrated nitric acid and stirred
for 24 hours for the ageing step. Latter, it was dried at 105 C for 24 hours and calcinated at
550 C for 2 hours.

7.2.3 Photocatalytic Degradation Experiments

A photoreactor equipped with sixteen UV-A light lamps (Philips, 8 W, 350 nm wavelength)
was used during photocatalytic experiments carried out in 200 mL sample volume at 30 C
constant temperature. pH was adjusted to the desired values by dosing 1 M NaOH and 1 M
HNO3. The effect of the composite amount (0.5
2.5 g/L) and the effect of pH (3
11) on
both dye removal were evaluated in this study. Experiments were run for 2 hours and a 3 mL
of sample were collected at different time intervals. The samples were centrifuged for 5 min-
utes at 4000 rpm speed before analysis. The experiments were repeated at optimized condi-
tions to collect samples for toxicity tests. To determine the reusability and stability the
composite was centrifuged, washed with distilled water and dried at 105 C each time before
reuse experiments run for three times. During reuse studies, a solution containing 50 mg/L
of dye solution was submitted to photocatalysis at pH 3 using a 2.0 g/L of composite amount
for RR and 2.5 g/L for RB dye. The color removal of RR and RB dyes was calculated on the
basis of their peak absorbance values measured at 520 nm (Mahmoodia and Aramib, 2009)
and at 610 nm (Dong et al., 2011) respectively prior and post photocatalytic oxidation.
 Chapter 7 • Photocatalytic Decolorization 127

7.2.4 Analysis
The synthesized composite was submitted to electron scanning microscopy (SEM)-energy
dispersive X-ray analyzer (EDX) (Fei-Quanta FEG 250) and Fourier transform infrared spec-
troscopy (FTIR) (Bruker Vertex 70 ATR) analysis to obtain its surface properties. SEM-EDX
was operated at 5 kV accelerating, 60 Pa pressure and 3 spot at 20000 3 and 40000 3 magni-
fication. FTIR was obtained in the range of 400 to 4000 cm21. Absorbance of the dyes was
scanned using a spectrophotometer (Shimadzu UV-2401).

7.2.5 Acute Toxicity

Newborn Daphnia magna (,24 hours) was exposed to dye solutions for 24 and 48 hours. at
50% and 25% dilution ratios (ISO 6341, 2012). D. magna were inoculated in a temperature
constant vivarium at NKU Environmental Engineering Department’s Laboratory. The pH of
the feeding and test solutions was kept at 8.0. Toxicity tests were performed in the dark at
temperature constant room (20 C). Experiments were performed as quadruplicate and 5
daphnids were tested in each replicate. Acute toxicity was assessed by means of immobiliza-
tion percentage determined by dividing the total number of immobilized organisms in four
replicate to total number of test organisms to be 20.

7.3 Results and Discussion

7.3.1 Characterization of TiO2 Impregnated Pumice Composite
SEM analysis illustrating surface morphology of TiO2 impregnated pumice composite
showed that pumice has an irregular shape with a porous surface that is heterogeneous
(Fig. 7-1). While the TiO2 film layer is mostly coated on the external surface of the pumice, it
can be also coated on the inner surfaces due to the pore structure (Zhang et al., 2016;
Nagarjuna et al., 2015). This leads to increase the active surface area of TiO2 thin layer but it
is, in any case, limited by the pore size (Pires et al., 2015; Liu et al., 2015). Chemical compo-
sition of pumice is mostly composed of silisium and oxygen. It numerically contains 23.81%
O, 2.00% Na, 9.74% Al, 64.45% Si and trace amount of Fe. After TiO2 impregnation the com-
position of pumice was characterized by 1.6% Ti as well as 22.85% O, 1.72% Na, 10.22% Al,
63.61% Si and trace amount of Fe.
As seen in Fig. 7-2, the FTIR spectrum of TiO2 impregnated pumice composite showed a
peak near 600 cm21 representing the stretching of Ti-O bond which is different from the FTIR
spectrum of pumice alone (Singh et al., 2016; Bagheri et al., 2016; Farhadian and Kazemzad,
2016; Zhang et al., 2012). The vibrations at 1650and 3400 cm21 assigned to 2OH vibration. The
peaks appeared at 450, 785, and 1030 cm21 are the characteristic bands of silisiums as Si-O,
Si-O-Si or O-Si-O bonds (Jardim et al., 2017). The absorption band at 450 cm21 could be
attributed to bending of Si
O vibration and the intensity of this band for TiO2 impregnated
pumice composite is higher than the band of pumice alone. The peak which appears at
1030 cm21 slightly shifted to 1058 cm21 for TiO2 impregnated pumice composite.
128 NANOTECHNOLOGY IN WATER AND WASTEWATER TREATMENT

FIGURE 7-1 SEM image of TiO2 impregnated pumice composite.

FIGURE 7-2 FTIR spectra of TiO2 impregnated pumice composite and pumice powder.
 Chapter 7 • Photocatalytic Decolorization 129

7.3.2 Effect of the Amount of TiO2 Impregnated Pumice Composite on

Decolorization
The effect of the amount of TiO2 impregnated pumice composite used as a catalyst during
photocatalytic oxidation on the decolorization of RB and RR dyes is given in Fig. 7-3.
Increasing the amount of the catalyst enhanced decolorization of RB and RR dyes due to the
presence of TiO2 nanoparticles promoting the formation of OH radicals. As the amount of
the catalyst increased from 0 to 2.5 g/L, the decolorization of RB shifted from 36.1% to

FIGURE 7-3 Decolorization of the dyes versus oxidation time using different concentrations of TiO2 impregnated
pumice composite as catalyst (pH:7).
130 NANOTECHNOLOGY IN WATER AND WASTEWATER TREATMENT

FIGURE 7-4 Effect of TiO2 impregnated pumice composite dose on the decolorization of the dyes (pH:7, oxidation
time: 120 minutes).

89.7%, while decolorization of RR dyes increased from 64.7% to 96.2% (Fig. 7-4). The degra-
dation of RR dye did not significantly change during 90 and 120 minutes oxidation. While
the degradation of RB dye continued during 120 minutes illumination. Maximum degrada-
tion of RB was obtained using 2.5 g/L catalyst, while the removal of RR did not significantly
change when a 2.0 and 2.5 g/L of catalyst was used. Pseudo first (Eq. 7.1) order kinetics fitted
the data as given in the following the equation:

lnC=C0 5 2 kt ð7:1Þ

Where C is the initial dye concentration (mg/L), C0 is the concentration of the dye at the end
of the reaction (mg/L), t (min) indicates the reaction occurring at any time, k1 (1/min) is the
equilibrium rate constant of pseudo first order adsorption. Accordingly, the reaction rate
constant (k1) is calculated from the intercept of the plot of 2 ln (C/C0) against time t. The
decolorization rates of dyes using the synthesized catalyst are given in Table 7-1. The kinetic
constant of RB dye increased with increasing catalyst dose up to 2.5 g/L. However, the kinetic
constant of RR decreased as the amount of the catalyst increased from 2.0 g/L to 2.5 g/L.
Highest kinetic constant was calculated to be 17.28.1023 min21 at 2.5 g/L catalyst dose for
RB and 27.19.1023 min21 at 2.0 g/L catalyst dose for RR dye.

7.3.3 Effect of pH on the Color Removal

The pH is important for the color removal of dyes as the adsorption of dye molecules on the
catalyst surface is affected by the change of surface charge with pH varying (Gupta et al.,
2012). The effect of pH on the color removal of both RB and RR dyes is given in Fig. 7-5.
Table 7-1 Pseudo First Order Kinetic Rates for Photocatalytic Decolorization of Dyes
Studied Using Different Amounts of the Composite (pH:7)
RB RR

Composite k1 (min21) k1 (min21)

Concentration (g/L) Removal % ( 1023) R2 Removal % ( 1023) R2

1.0 69.4 11.07 0.8297 73.9 11.75 0.9527

1.5 74.2 12.16 0.7705 86.7 16.60 0.9308
2.0 79.7 13.54 0.9490 91.3 27.19 0.9472
2.5 89.7 17.28 0.9686 96.2 25.02 0.9808

FIGURE 7-5 Effect of pH on the decolorization of the dyes (catalyst concentration: 2.0 g/L for RR and 2.5 g/L for RB,
oxidation time: 120 minutes).
132 NANOTECHNOLOGY IN WATER AND WASTEWATER TREATMENT

FIGURE 7-6 Effect of pH on the decolorization of the dyes (catalyst concentration: 2.0 g/L for RR and 2.5 g/L for RB,
oxidation time: 120 minutes).

Table 7-2 Pseudo First Order Kinetics for Photocatalytic Decolorization of Dyes at
Varying pH Values (Composite Amount: 2.0 g/L for RR and 2.5 g/L for RB)
Remazol Blue Remazol Red

pH k1 (min21) ( 1023) R2 k1 (min21) ( 1023) R2

3.00 28.29 0.9652 29.84 0.9866

5.00 15.74 0.9116 20.92 0.9092
7.00 17.28 0.9686 27.19 0.9472

Higher catalytic activity obtained at acidic condition for both dyes and the removal efficiency
decreased by the increase of pH of the solutions. Specifically, decolorization of RB and RR
dyes were found to be 97.8% and 97.6% at pH 3, respectively whereas those color removal
percentages decreased to 57.4% and 53.9%, respectively at pH 11 after 2 hours of photocata-
lytic oxidation (Fig. 7-6). When pH was adjusted from 5 to 3, the k1 enhanced from
15.74.1023 to 28.29.1023 min21 for RB dye and from 20.92.1023 to 29.84.1023 min21 for RR
dye (Table 7-2).

7.3.4 Toxicity of Photocatalytic Oxidation By-Products

As it was reported for the other advanced oxidation processes, oxidation by products can
form in photocatalysis process that can also cause more toxic effluent than prior to the treat-
ment (Lofrano et al., 2016; Ozkal et al., 2016). In this study, photocatalytic treated all samples
resulted in 100% immobilization of Daphnia magna when they were tested without dilution.
 Chapter 7 • Photocatalytic Decolorization 133

FIGURE 7-7 Toxicity evolution of photocatalytic treated samples on Daphnia magna for 24 h exposure time and
tested at 75% dilution ratio (catalyst concentration: 2.0 g/L for RR and 2.5 g/L for RB, pH:3).

The treated samples were also tested after dilution at which the samples resulted in 100%
toxic at 50% dilution ratio after 24 hours exposure time. As a further dilution, the samples
were tested at 75% dilution at which both photocatalytic treated dye solutions resulted in
100% toxic after 30 and 60 minutes of irradiation. Toxicity to Daphnia magna decreased
below 50% immobilization after 90 and 120 minutes of irradiation for both dyes (Fig. 7-7).
This decrease is found promising for the effectiveness of photocatalytic treatment, however
there is an urgent need to prolong the treatment duration and/or for increasing catalyst dose
to completely remove toxicity in the undiluted samples.

7.3.5 Reuse and Stability of TiO2 Impregnated Pumice Composite

A slight decrease in the photocatalytic color removal was observed for both dyes when TiO2
impregnated pumice composite was reused. This reduction of removal efficiency was proba-
bly due to the adsorption of dyes on the surface of the composite (Yener et al., 2017). Dye
molecules accumulate in the pores of pumice leads to inhibition of the photocatalytic degra-
dation. The degradation efficiencies of RB dye were found to be 97.8%, 82.7%, and 75.3%
whereas a 97.6%, 85.3%, and 84.0% degradation of RR were observed for the first, second,
and third cycles of reusing composite, respectively. Besides, k1 decreased from 28.29.1023 to
11.01.1023 min21 for RB and from 29.84.1023 to 14.03.1023 min21 for RR dye (Table 7-3).
Similar reductions in removal efficiency for reuse of catalyst was reported in the literature
(Kanakaraju et al., 2015; Yener et al., 2017; Hadjltaief et al., 2016; Gomez et al., 2013).
However, Gomez et al. (2013) found that the calcination of catalyst is important to regenerate
the catalyst for reuse. On the other hand, Zabihi-Mobarake and Nezamzadeh-Ejhieh (2015)
reported that the calcination at 450 C for used catalyst was more efficient than at 25 C and
200 C. The slight decline of degradation observed in our study could occur since calcination
is not applied for each cycle.
134 NANOTECHNOLOGY IN WATER AND WASTEWATER TREATMENT

Table 7-3 Pseudo First Order Kinetics Changes for Photocatalytic Decolorization of
Dyes Reusing Composite (Composite Amount: 2.0 g/L for RR and 2.5 g/L for RB, pH:3)
RB RR
21
Reuse of k1 (min ) k1 (min21)
Composite Removal (%) ( 1023) R 2
Removal (%) ( 1023) R2

1st 97.8 28.29 0.9652 97.6 29.84 0.9866

2nd 82.7 15.71 0.9754 85.3 15.00 0.9766
3rd 75.3 11.01 0.9924 84.0 14.03 0.9624

R, regression coefficient.

7.4 Conclusion
This study, as a first attempt, aimed to evaluate photocatalytic decolorization of of two rema-
zol dyes (blue and red) using TiO2 impregnated pumice composite catalyst. The SEM-EDX
analysis showed that TiO2 nanoparticules were mostly impregnated on the pores of pumice
with a ratio of 1.60% Ti. A 97.8% and 97.6% of color removal was achieved for RB and RR at
pH 3, respectively, whereas those color removal percentages decreased to 57.4% and 53.9%,
respectively, at pH 11 after 2 hours illumination. The color removal efficiencies of 97.8%,
82.7%, and 75.3% for RB dye and of 97.6%, 85.3%, and 84.0% for RR dye were observed after
first, second, and third cycles reuse of the synthesized catalyst. Toxicity of photocatalytic
treated samples of both dyes decreased below 50% after 90 and 120 minutes irradiation
when they were diluted at 75%. This result indicate there is an urgent need to prolong the
irradiation time and/or for increasing catalyst dose to completely remove toxicity in the
undiluted samples.

Acknowledgments
The authors thank Soylu Ltd for providing pumice. This study was inspired from the EU COST Actions
ES1202 and supported by Namik Kemal University Research funding Office (NKUBAP.06.GA.17.094).

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