J Nanotechnol Nanomaterials. 2022;3(2):67-76.
Journal of Nanotechnology and Nanomaterials Research Article
Photocatalytic Degradation of Organic Dyes Using Titanium
Dioxide (TiO2) and Mg-TiO2 Nanoparticles
Sandesh Jaybhaye1, Nikita Shinde1,2, Shrutika Jaybhaye3, Himanshu Narayan4*
1
NTRL, Department of Chemistry, B.K. Birla College of Arts, Science & Commerce, Kalyan 421 304, India
2
Department of Biotechnology, B.K. Birla College of Arts, Science & Commerce, Kalyan 421 304, India
3
Department of Architecture and planning, Vivekanand Global University, Jaipur, India
4
Usha Martin University, Ranchi 835 103, India
*
Correspondence should be addressed to Himanshu Narayan, [Link]@[Link]
Received date: March 15, 2022, Accepted date: April 12, 2022
Citation: Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
Copyright: © 2022 Jaybhaye S, et al. This is an open-access article distributed under the terms of the Creative Commons
Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author
and source are credited.
Abstract
Titanium dioxide (TiO2) based nano-sized photocatalysts (NPCs) were synthesized following a green method from the extract of Peepal (Ficus
religiosa) leaves and titanium tetrachloride as precursors. Doping of TiO2 with Magnesium (Mg) was done using magnesium chloride through
the method of chemical precipitation. Size of the NPC samples were estimated and characterized by CPS Disc Centrifuge, Diffracted Light
Scattering (DLS) and Field Emission Gun Scanning Electron Microscopy (FEG-SEM) techniques. UV-visible spectroscopy was employed in the
study of photocatalytic properties of the NPCs. A low-cost, simple photo-reactor was fabricated and photocatalytic degradation of Methyl
Orange (MO) and Methylene Blue (MB) dye solutions was investigated. Reasonable degradation of the dyes was observed in the presence of
the NPCs. It was therefore concluded that the NPCs studied in this work can be promising nanomaterials for the degradation of MO and MB
dyes under visible light irradiation. Nevertheless, a detailed investigation of various factors influencing the processes involved will be required
to optimize the conditions in order to achieve the best degradation efficiency.
Keywords: Titanium dioxide nanoparticles, Ficus religiosa, Photocatalytic degradation, Organic dyes
Introduction minerals. However, for it to be used more efficiently and
effectively, certain properties, such as, particle size and shape,
Titanium oxide (TiO2), or titania, is a very important crystallinity, etc. can be modified. Moreover, incorporation (or,
semiconducting material that has attracted great interests doping) of metal ions into host TiO2 has also been investigated
due to its unique physical and chemical properties. TiO2 extensively as a method to improve the photocatalytic activity
exists in three major crystalline phases, namely, anatase, [1-5].
rutile and brookite. Out of these three, the brookite phase
is not practically beneficial because it is stable only at low Out of several applications associated with photocatalysis,
temperatures. On the other hand, relatively high chemical the treatment of wastewater is perhaps the most notable
inertness of the rutile phase makes it a suitable choice in one. Numerous verities of pollutants emitted as industrial
applications where stability is critical. wastewater can possibly be degraded through photocatalysis
making it reusable [4-9]. Water being one of the most vital
Chemically the anatase phase of TiO2 is the one with commodities, there is no wonder so many materials scientists
best response, especially in catalytic applications. Under around the globe are investigating photocatalytic remediation
appropriate excitation, it is generally capable of degrading of polluted water mediated by TiO2 based materials.
common pollutants of water, such as, carboxylic acids and
alcohols completely to carbon dioxide, water and simpler Nanomaterials have a larger surface-to-volume ratio
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Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
Kingdom: Plantae
Division: Magnoliophyta
Class: Magnoliopsida
Order: Rosales
Family: Moraceae
Genus: Ficus
Species: F. religiosa
Scientific Name: Ficus religiosa
Figure 1: Peepal tree leaves (Ficus religiosa) and Scientific Classification.
compared to their bulk counterparts. This has important For plant leaf extract-based synthesis of nanoparticle,
consequences for all those processes that occur at the the extract is mixed with metal precursor solutions at
surface of a material, such as, catalysis and detection. different reaction conditions. The parameters determining
Therefore, nano-sized TiO2 particles usually show improved the conditions of the plant leaf extract (such as types and
photocatalytic activity. However, pure TiO2 is a wide bandgap concentration of phytochemicals, metal salt concentration,
semiconductor that absorbs in the UV region of spectrum. As pH, and temperature) can be adjusted and tuned to optimize
a result, the photocatalysis with TiO2 can occur only under UV the rate of nanoparticle formation, their yield and stability.
irradiation making it an expensive affair. A possible solution to The leaf-extract based phytochemicals are known to usually
this could be doping the host TiO2 with a material that reduces reduce the precursor solutions into metal ions in short time,
the bandgap in such a way that photocatalysis can take place and they act also as a stabilizer for the nanoparticles produced
with inexpensive sources of visible light [6]. [10-17]. For example, Fe-, Zn- and rare earth doped TiO2 [4,5],
Mg-doped ZnO [18] and TiO2 [19] and many other pure, doped
As discussed above, the photocatalysis of TiO2 is a complex and modified nanomaterials are being investigated by a
function of its physicochemical properties, including size, number of groups.
shape, surface characteristics and inner structure. Therefore, in
order to enhance the photocatalytic efficiency, the TiO2 may be In the present study, we discuss the green-synthesis of pure,
doped with suitable ions to reduce its band gap. At the same and Mg-ions doped, TiO2 nano-sized photo catalyst (NPC)
time, appropriate methods can be employed to synthesize particles obtained from reduction of titanium tetrachloride
nano-sized particles of the catalyst [3-5,10]. precursor solution using Peepal (Ficus religiosa) leaf-extract.
Even though the magnesium doped titanium-oxide based
Many existing physical and chemical synthesis approaches nanomaterials have been studied by some groups, the method
require high radiation, highly toxic reluctant, and stabilizing of synthesis of this material through simple, inexpensive
agents, which can cause pernicious effects to the ecosystem. green route, particularly using the Peeple leaf-extract is being
In contrast, green synthesis of metallic and metal-oxide reported for the first time. Moreover, as a part of potential
nanoparticles is an eco-friendly method that involves the applications, we also report the results of photocatalytic
simple process of bio-reduction and therefore, requires degradation of Methylene Blue (MB) and Methyl Orange (MO)
relatively low energy to initiate the reaction. Consequently, it dyes using these nano-photo-catalysts, under visible light
is also cost effective also [10-13]. illumination of a tungsten lamp.
Recently, environment friendly, green, biosynthesis Materials and Methods
techniques employing plant extracts have gained added
consideration as a simple, efficient, cost effective and feasible AR grade (99.5% pure) Titanium Tetrachloride (TiCl4) was
method, and an excellent alternative mean to conventional obtained from Loba Chemicals and AR grade Sodium
methods of nanoparticles production. Many researchers have Hydroxide (NaOH) pellets were obtained from SDFCL Fine-
employed green synthesis process for preparation of metal/ Chem Limited. LR grade Magnesium Chloride hexahydrate
metal oxide nanoparticles via plant leaf extracts [10-16]. (MgCl2.6H2O) was obtained from Qualigens Company. All the
J Nanotechnol Nanomaterials. 2022
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Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
chemicals were used without further purification. Solutions of continuously. The solution was kept overnight for settling.
1 M NaOH and 1 M MgCl2 were also prepared separately using Afterwards, the brown colored precipitate was filtered and
distilled water. dried at 100°C in hot air oven for 6 h. The precipitate was then
calcinated (GRAVITY LAB INSTRUMENTS CO.) at 200°C for 6 h.
Preparation of Peepal leaf-extract The powder obtained was stored carefully for further analysis.
The resulting brown powder obtained was collected and
The Peepal leaf extract was prepared using distilled water. stored for further studies. It is a chemical way for synthesis of
Fresh leaves were taken from the campus of B. K. Birla College titanium dioxide based nanoparticles (Figure 3).
of Arts, Science and Commerce (Autonomous) Kalyan. Leaves
were thoroughly washed with distilled water and 10 g of these Prior to investigation of degradation of dyes, the Mg-TiO2
leaves was crushed in a Mortar-Pestle. Then 100 ml of distilled samples (Mg ions loaded/doped TiO2 NPCs) were pre-treated
water was added to this and the solution was boiled for 45 in two different ways. NPC sample called D1 was stirred
min. Then the leaf extract solution was cooled, double filtered continuously for 6 h, and the one called D2 was stirred for 8 h,
and centrifuged (REMI) at 5000 rpm for 5 min to remove all the followed by a 4 h sonication.
debris and to obtain a clear solution.
Characterization of samples
Green synthesis of pure titanium dioxide nanoparticles
Spectroscopic analysis was performed using an UV-Vis
TiCl4 solution was prepared by adding 10 ml TiCl4 slowly into spectrophotometer (SYSTRONICS). The samples were analyzed
100 ml of distilled water at 5 – 6°C. 100 ml of TiCl4 solution in Quartz cuvettes of 1 cm path length, scanning from 200 to
was slowly (drop wise) added to 100 ml of leaf extract on a 700 nm wavelength. Distilled water was used as reference for
magnetic stirrer (REMI 2MLH) at 500 – 600 rpm. The solution the baseline correction.
was magnetically stirred for 3 h and then sonicated for 2 h
using an ultrasonic sonicator. The solution was kept overnight Determination of particle size of samples was done using
for settling. Next day, the solution was centrifuged at 5000 rpm CPS Disc Centrifuge UHR (Model DC24000). The CPS Disc
for 10 min and supernatant was collected. The supernatant Centrifuge separated the particles by size using centrifugal
was calcinated (GRAVITY LAB INSTRUMENTS CO.) at 200°C for sedimentation in a liquid medium. Prior to measurements,
6 h. White colored powder of TiO2 was obtained which was the unit was calibrated using 8% and 24% of standard sucrose
collected and stored (Figure 2). The off-white-colored product solution. Then titanium dioxide-based NPC samples were
obtained was collected and stored for characterization. It is a injected one at a time using a syringe, and analysis was carried
simple, eco-friendly way and economical method for synthesis out.
of titanium dioxide nanoparticles.
Field Emission Gun-Scanning Electron Microscopy (FEG-SEM)
Chemical synthesis of Mg-TiO2 samples was employed to determine the size, shape and morphology
of the NPCs. These analyses were done at Sophisticated
Hundred ml of TiCl4 solution and 100 ml 1 M MgCl2 solution Analytical Instrument Facility (SAIF), IIT Bombay on JEOL JSM-
were mixed together, and 1 M NaOH solution (precipitate 7600F FEG-SEM unit.
precursor) was added drop by drop to it until the pH value
reached to 7, under continuous stirring on a magnetic stirrer DLS sample analysis was done at Mumbai University using
(REMI 2MLH). The solution was kept stirring for 6 hours MALVERN PANANALYTICAL Zetasizer Nano range. The NPC
Figure 2: Various stages of green synthesis of TiO2 nanoparticles.
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Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
Figure 3: Various stages of synthesis of Mg-TiO2 nanoparticles.
particles were dispersed in distilled water and diluted. Prior the light source dipped into the solution without touching
to analysis, the solution was sonicated for 15 min in order to directly (Figure 4). A ring attached to a stand was fitted on
make the dispersion uniform. top of the inner glass vessel to hold it in place inside the
beaker, which was placed on a magnetic stirrer-table. A 100
Fabrication of photo-reactor W Tungsten lamp (Phillips) was placed in the middle of this
vessel so that it could not touch the sides and its end was at
The visible–light photocatalytic activity was carried out in least 2 cm from the bottom of the inner vessel. Finally, the
a locally fabricated, simple and inexpensive photo reactor inner vessel was sealed with parafilm where it touched the top
[4,5,20] consisting of a 1 liter glass jar into which was placed of the beaker.
a magnetic stirring bar and a smaller glass vessel that housed
(a) (b)
Figure 4: Schematic diagram of photocatalytic reactor (a) and the photocatalytic rector (fabricated by Jaybhaye et al.) used in the present
work (b).
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Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
Figure 5: The MB [7-(dimethylamino) phenothiazin-3-ylidene]-dimethylazanium; chloride; and MO Sodium; 4-[[4-(dimethylamino) phenyl]
diazenyl]benzenesulfonate has formula C16H18ClN3S and C14H14N3NaO3S, respectively.
Study of photocatalytic activity For MB the wavelength range of recorded spectrum was
500 to 700 nm, and for MO it was 300 to 500 nm because the
Photocatalytic activity of the prepared NPC samples was respective absorption peaks (660 nm for MB and 460 nm for
examined in terms of the degradation of Methylene Blue (MB) MO) were expected within these ranges. The peak values of
and Methyl Orange (MO) dyes in solution under illumination absorption data were used as a direct indicator of the dye
with a tungsten incandescent lamp. Chemical structures of concentration and therefore used to plot the degradation
the two dyes are shown in Figure 5. curves.
Experimental solutions with 10 ppm of both dyes were The percentage of degradation was estimated in terms of the
prepared. In the reactor 500 ml of dye solution, a magnetic relative concentration (C/C0) in percent fraction, of the dye left
stirring bar and 150 mg of nanoparticles were placed. For in solution after a given time from the beginning. Here, C0 is
uniform distribution of nanoparticles throughout the solution, the initial concentration and C is the concentration at time t.
after addition of NPC sample the solution was kept stirring
for 15 min, without switching on of bulb. Then the light was The experimental procedure was carried out for all NPC
switched on to begin the processes. Stirring and lamp were samples placing the reactor in dark conditions to minimize the
both kept on continuously through the experiment. effects of various external sources of light.
Every 10 minutes, 5 ml of the experimental mixture was taken Results and Discussion
out, centrifuged, and the resulting clear solution was taken for
recording its absorbance spectra. on a UV-Vis double beam X-ray diffraction analysis
spectrophotometer (SYSTRONICS). The baseline correction
of UV-Vis double beam spectrophotometer was done using Figure 6 shows the XRD patterns for the synthesized
distilled water prior to the experiment. nanoparticles. A careful observation shows that rutile phase,
Figure 6: X-ray diffraction pattern the NPCs with PDF 00-025-1157 Mg2TiO4 peak positions shown in red.
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with (110) peak around 27.7°, is more dominant phase of TiO2 It shows that the sample is polydisperse in nature. The size
in the synthesized NPCs. Formation of a magnesium titanate of TiO2 nanoparticles is >20 nm. The Figure 7 (b) represents
phase of Qandilite, (or, Mg2TiO4) is reasonably evident from the size distribution data for Mg-TiO2 nanoparticles. Due to
the plot. The average particle size from the XRD data using agglomeration of the smaller grains of Mg-TiO2 particles, the
Debye-Scherrer formula was estimated to be around 46 nm average size of was estimated to be >500 nm. In order to
for a Gaussian peak fitting. further consolidate the observations, FEG-SEM was carried
out, which not only estimated the size but also furnished
Particle size analysis visual information about the shape and morphology of the
NPCs. The FEG-SEM image of TiO2 nanoparticle is shown in
The average particle size of TiO2 nanoparticles was Figure 8. The morphology of TiO2 nanoparticle shows that
determined using CPS Disc Centrifuge particle size analyzer. smaller particles of TiO2 NPCs have agglomerated into bigger
The procedure for analysis was set in the software and the grains. The agglomeration occurs because the TiO2 seems to
sample was processed. The particle of sample was found to be unstable in the nanoparticles form and it tends to join other
be in range of 50 to 100 nm, with more than 90% particles nearby nanoparticles until their size becomes relatively stable.
having approximately 91 nm particle size. Another estimation As evident from the pictures, the particle size of TiO2 NPCs is
of particle size was done through the DLS method, which in the range from 11.5 nm to 20 nm. Clearly, the SEM images
gives an average mean value of size of sample. The Figure 7 (a) show the particles size whereas the DLS method estimates the
represents the average size distribution for TiO2 nanoparticles. agglomerated grains size.
(a)
(b)
Figure 7: (a) DLS of TiO2 Nanoparticles; (b) DLS of Mg-TiO2 nanoparticles.
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Figure 8: FEG-SEM images of TiO2 nanoparticles.
UV-Visible Spectroscopy was found to be 1.51 × 10-2 min-1 and 0.44 × 10-2 min-1, for
degradation of MB and MO dyes, respectively. It was also
UV-Vis Spectroscopy was carried out as priliminary test to noted that before flattening-out after 50 minutes, the rate of
determine the absorption properties and characteristics degradation was marginally faster with (kobs) being 2.01 × 10-2
maxima of the samples. The absorption spectrum of pure min-1 and 0.59 × 10-2 min-1, respectively.
TiO2 nanoparticles showed a prominent peak at 377 nm and
Mg-TiO2 nanoparticles exhibited a peak around 390 nm. Degradation of dyes with Mg-TiO2 nanoparticles
Throughout the study, the formation of TiO2 nanoparticles
and Mg-TiO2 nanoparticles was confirmed by this method. As mentioned earlier, prior to degradation experiments, the
The absorption maximum was noted in the range 300-430 nm Mg-TiO2 NPC samples were pre-treated in two different ways:
for pure TiO2 nanoparticles and for Mg-TiO2 nanoparticles the While both D1 and D2 samples were kept stirred for a long
range was 250-450 nm. time, the latter was sonicated too.
The graph depicted in Figure 9 shows the comparative Figure 10 shows the degradation of MB and MO dyes in the
photocatalytic degradation of the dyes MB and MO in the presence of Mg-TiO2 NPC samples. The percent degradation
presence of pure TiO2 NPCs. It is evident that the degradation was obtained by taking the difference between initial and final
of MB dye by pure TiO2 is better than that of MO dye as the NPC optical density of solution at 660 and 460 nm, respectively, for
degrades MB by 64 %, but MO only by 28 % in approximately MB and MO dyes.
an hour time. These values also seem to be the maximum
achievable degradation as the curve flattened out after 70 On the other hand, it is observed that D1 Mg-TiO2 sample
min. produced only about 16%, whereas D2 Mg-TiO2 led to nearly
26 % degradation of MO in approximately 1 h time. It may
From the data obtained, it was determined that the rate further be noted that the degradation of MO dye with pure
of degradation follows a first-order pattern for all NPCs. The TiO2 NPC is better than both D1 and D2 types of Mg-TiO2
observed rate-constant (kobs) was estimated from the slope NPC samples. Nevertheless, compared to the un-sonicated
of a linear regression analysis of ln (C/C0) versus time, and D1 sample, the sonicated D2 Mg-TiO2 NPC sample seems to
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Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
Figure 9: Degradation of both MB and MO dyes in the presence of TiO2 NPC particles. The solid lines are just a guide to eyes.
Figure 10: Degradation of both MB and MO dyes in the presence of Mg-TiO2 NPC particles. The solid lines are just guides to eyes.
be more active, and is nearly as efficient as pure TiO2 NPCs, Stirring of solution ensured that every part of the solution
as expected. Similar analysis of data gives the values of (kobs) was exposed to the illumination from source of light for
as 0.74 × 10-2 min-1 and 1.70 × 10-2 min-1, respectively, for enhanced photo-excitation. On the other hand, the process
degradation of MB dye with D1 and D2 Mg-TiO2 NPC samples. of sonication breaks the agglomerated lumps into their
On the other hand, for degradation of MO dye with D1 and D2 constituents, smaller particles and grains, and also helps them
NPCs, the (kobs) was estimated to be 0.26 × 10-2 min-1 and 0.40 × disperse uniformly throughout the solution. Larger specific
10-2 min-1, respectively. surface area due to the smaller particles and grains supports
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Jaybhaye S, Shinde N, Jaybhaye S, Narayan H. Photocatalytic Degradation of Organic Dyes Using Titanium Dioxide
(TiO2) and Mg-TiO2 Nanoparticles. J Nanotechnol Nanomaterials. 2022;3(2):67-76.
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