Poll Res.

40 (4) : 1547-1552 (2021)

Copyright © EM International
ISSN 0257–8050

SYNTHESIS, CHARACTERIZATION AND APPLICATION OF NANO-

SIO2 AND NANO-PBO IN DYE DEGRADATION
PRIYANKA T. WADITAKE AND PRASHANT L. CHAUDHARI
Department of Chemical Engineering, Bharati Vidyapeeth (Deemed to be University),
College of Engineering, Katraj, Pune 411043
(Received 18 December, 2020; Accepted 3 February, 2021)

ABSTRACT
The precursor solutions were made by mixing Silicon Tetrachloride and Lead chloride respectively
for SiO2 and PbO nanoparticles. The detailed Microscopic and Spectroscopic characterizations of
the surface morphology for both nanoparticles were conducted by using Ultraviolet Spectroscopy
(UV), Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and X-ray Diffraction
(XRD). To study the effect of these synthesized nanoparticles, the photo catalytic reduction of
harmful azo dye – methylene blue has been investigated using SiO2 and PbO photo catalyst in
aqueous solution under irradiation. Experiments were conducted further to check phytotoxicity.
These observations indicate that all the two dyes could be degraded completely with similar time
intervals. Hence, it may be a viable technique for the safe disposal of textile wastewater into the
water streams.

KEY WORDS : Nanomaterial, Silicon dioxide, Lead oxide, Azo textile dyes,
Characterization, Phytotoxicity

INTRODUCTION issue using photocatalyst in irradiation (Manoj

Singh et al., 2011; Anastas and Williamson, 1998;
Nanoparticles have a high specific surface area, Aileen et al., ?????? ; Mohammed Mehdi et al., 2011).
interfacial dominated properties, and electrical/ The purpose of this study was to find the
optical properties that can be distinguished with degradation of harmful methylene blue dye with
respect to corresponding bulk materials and the one the photocatalytic system by using different type of
hand and individual molecules on the other. catalyst with different loading, concentration of dye,
Therefore nanoparticles find application in diverse and the role of these catalysts on the degradation
fields such as battery technology, fuel cell, efficiency with its phytotoxic effect of the recycled
wastewater treatment, electronics and sensors, etc. wastewater (Manoj Singh et al., 2011; Rajamohan
Because of the simplicity of design, low cost of and Karthikeyan, 2006).
manufacturing, reliability and relative safety there is The present work deals with the synthesis of
great use of nanomaterial in various fields. Dyes nano-SiO 2 and nano-PbO particles by using
used in textile industry are the vast source of hydrothermal method at lower temperature. The
coloured organic pollutants that increased the obtained powder was characterized by using SEM,
environmental danger. During the manufacturing XRD, UV and FTIR. Also, the photocatalytic activity
and production huge quantity of wastewater checked using Congo red dye and methylene blue
containing these toxic dyes can be introduced into dye. Further, we have also studied the phytotoxicity,
the aquatic systems. Due to the stability of these recyclability and photocatalytic activities of SiO2
modern textile dyes, convenient methods are and PbO Nano powders.
ineffective for their decolouration and toxicity
Chemicals
reduction. Recent literatures have revealed that
photocatalysis can be the viable way to mitigate this Silicon tetrachloride (SiCl 4 ) and lead chloride
1548 WADITAKE AND CHAUDHARI

(PbCl2) were used as a source of silicon and lead in make up solution of 500 ml. similar process has
the fabrication of nanoparticle. Sodium hydroxide done for the preparation of methylene blue dye.
flakes (NaOH), TRITON X100 LR (t-
Characterization
octypenoxypolyethoxyethanol) was used as
received from Sigma Aldrich Corporation. For the
A. SEM
dye preparation, methylene blue dye was used in
various amounts as received with distilled water. Table 1. EDX analysis of SiO2 nanoparticles
Procedure Element Weight% Atomic%

A. Process for synthesis of nanoparticles O K 46.18 60.10

Si M 53.82 39.90
Take 4 g of NaOH flakes and 50 mL distilled water Total 100 100
were mixed together in a beaker. Add 3.4 mL of
SiCl4 (silicon tetrachloride). Add 3.4 ml of Triton (t- Smaller rods structures have seen at the lower
octylphenoxypolyethoxyethanol). Shake well & add magnification. The Rod of flecks may be the effect of
50 ml+10ml of distilled water. Take in Teflon bottle possible agglomeration. The average particle size is
in auto clave reactor. Shake well; Keep the mixture 353.83 nm. Fig. 1 (d, e, f) represents SEM pictures of
in an oven for 24hr at 120 °C. After 24 hours remove the synthesized SiO2. The shapes of the particles are
the sample s from the oven and filter with the help similar to each other and likely become spherical in
of silica grouch crucible by water jet vacuum pump. general. In the SEM images it is also seen that the
Dry the samples in hot air oven at 120 °C for 5 synthesized SiO2 powder particles are agglomerates.
hours. Take the dry samples in alumina crucible. However, the size distribution of the powder varies
The dried samples are kept in muffle furnace for
calcinations purpose at 600 °C for 3 hours and then
Table 2. EDX analysis of PbO nanoparticles
the samples are grinded. After grinding products
are stored in vials. Similar procedure has followed Element Weight% Atomic%
for the synthesis of PbO nanomaterial. O K 18.21 74.25
B. Process for preparation of dyes Si M 81.79 25.75
Total 100 100
Take 25 mg of Congo red dye in distilled water and

(a) (b) (c)

(d) (e) (f)

Fig. 1. Scanning Electron Microscopy (SEM) of Nanoparticles
a,b,c : SEM of Lead nanoparticles(PbO); d,e,f : SEM of Silica nanoparticles (SiO2)
Fig 1(a, b, c) shows SEM images of PbO material is showing the flakes structure.
 SYNTHESIS, CHARACTERIZATION AND APPLICATION OF NANO-SIO2 AND NANO-PBO 1549

compositions. The other peaks in the graphs of PbO

nanoparticles may arise due to impurities during
the process.

Table 3. Adsorption Vs Time study for methylene blue

dye (30 ppm)
Time Adsorption in Adsorptionin
SiO2 for 30 ppm PbO for 30 ppm
0 1.987 1.987
30 1.531 1.726
60 1.164 1.495
90 0.821 0.856
120 0.596 0.367
150 0.203 0.126
Fig. 2A EDX of SiO2 nanoparticles
180 0.03 0.043

B.FTIR
FTIR provides the sample information on the basis
of physical state (solid, liquid, gas) and the chemical
composition. The FT-IR spectrum of synthesized
SiO2, dried at 1200C and that of calcined at 6000C is
shown in Fig. 3(a). The IR band at 2889.36 cm-1 could
be assigned to the stretching vibrations of Si–OH
groups in the structure of amorphous SiO 2 .
Correspondingly, the IR band at 1639.38 cm–1 is due
to the bending vibration of H2O molecules. The
Fig. 2B EDX of PbO nanoparticles very strong and broad IR band at 1066.99 cm–1 is
usually assigned to Si–O–Si asymmetric stretching
in the range for 76.3 nm to 728.34 nm. The vibrations. The IR band at 798.52 cm –1 can be
agglomeration may result from the chemical assigned to Si–O–Si symmetric stretching
treatment conditions. vibrations.
For elemental analysis of the given samples, The FT-IR spectrum of synthesized PbO, dried at
energy dispersive x-ray spectroscopy was used. The 120 o C and that of claimed at 500 o C is clearly
above Fig. 2A represents EDX of SiO2 nanoparticles represented in Fig. 3(b). The peak of 513.06 cm -1
and Fig. 2B represents the EDX of PbO indicates the formation of PbO material. The IR
nanoparticles. The elemental composition is clearly peak at 586.36 cm-1 indicates the presence of oxides.
states that, there is formation of SiO 2 and PbO Peak value 678.94 cm-1 represents Pb-O-Pb starching

(a) (b)
Fig. 3. FTIR diffraction of (a) SiO2 nanoparticles & (b) PbO nanoparticle
1550 WADITAKE AND CHAUDHARI

vibration. These two peaks are very sharp. It is angle of 29.24, 31.16, 31.54, 35.68, 44.98 corresponds
confirmed that the final product is the presence of to the reflections from the 111, 020, 200, 201 and 022
lead and oxide. The peak value 1381.03 cm -1 crystal planes respectively according to the
assigned for the presence of OH group. literature (JCPDS Card No. 38- 1477) (Fang and
Huang, ???????? ; Theivasanthi and Alagar, 2010;
C. XRD
Kikuo Okuyama et al., 2002; Schraml Marth et al.,
Fig. 4(a) shows a broad peak located approximately 1992
at 2 = 21.24°, that suggests an Amorphous
UV
characteristic of the sample and agrees with the
reported JCPDS data (card No. 01-086-1561). Fig. 1. The photo reactivity of nanostructured SiO2 is
4(b) shows the XRD pattern of Lead Oxide greatly improved by the high efficiency and wide
nanoparticles. The phase purity of the prepared range of light absorption. The sharp peak at 303 nm
tetragonal n-PbO can be clearly seen and all is due to near band edge emission in the case of PbO
diffraction peaks are perfectly indexed to the (Das Chayan and Kapgate Bharat, 2012; Rajkumar et
tetragonal PbO structure. No characteristics peaks al., ????? ; Ramesh Kumar et al., 2004).
of impurities were detected. The broadening of the
peaks indicated that the particles of nanometer RESULTS AND DISCUSSION
scale.
The XRD pattern of the PbO reveals Dye Degradation
crystallographic structure of the synthesized PbO Methylene blue using SiO22. Methylene blue using
powders. The three strongest peaks of scattering PbO

(a) (b)
Fig. 4. X-ray diffraction of (a) SiO2 nanoparticles & (b) PbO nanoparticle

(a) (b)
Fig. 5(a) UV-Vis of SiO2 nanoparticles, &(b) UV-Vis of PbO nanoparticles
 SYNTHESIS, CHARACTERIZATION AND APPLICATION OF NANO-SIO2 AND NANO-PBO 1551

Fig. 6 (a). Degradation of methylene blue by using SiO2 Nanoparticles and (b) Degradation of methylene blue by using
PbO Nanoparticles

Phytotoxicity Check The adsorption of methylene blue dye of

(intensity =30 ppm) through nano-SiO2 and nano-
Toxic effect on the growth of the plant may define as
PbO catalyst performed in UV photo chemical
phytotoxicity. This kind of damage may cause by
reactor separately. It is evident from Table that
the several variety of compounds like pesticides,
within 180 minutes the colour of dye is completely
phytotoxins, etc. The plant shows the negative
adsorbed. But the result shows that during initial 30
growth during the effect of phytotoxins. In some
minutes the dye couldn’t show any significant
instances, plants react to substances like humans
change in color in the case of PbO nanoparticles and
with food allergies react to certain foods. The
afterwards it is adsorbed by the catalyst.
substance can be applied, and within a short period,
it will become evident that the plants are intolerant
CONCLUSION
to it. The plants may be able to tolerate a substance
in smaller doses, but a grower may consciously or
The obtained result describes a simple sol-gel
unconsciously over-saturate the plants only to find
method for the synthesis of SiO 2 and PbO as a
that it poisons them. Here, the last solution of the
catalyst at lower temperature with high yields. This
methylene dyes (after 180 minutes) used to check
nanoparticles catalyst provides a new way for
the phytotoxicity. The plant seed sowed in the pots
continuous processes. Both the nanoparticles
and the effects of the degraded samples checked. It
characterized by UV-Vis, FTIR, XRD, SEM. This
had seen that the plant growth is normal in
catalyst would be helpful to understand the
degraded samples. Hence, the process described in
advantages combination of the properties of
the paper may be used to treat the industrial dyes
homogenous catalyst and the development of new
solutions.
catalytic systems. Further the same Catalyst can be
used for a number of cycles which will reduce the
cost of operation.

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