Volume 7, Issue 11, November – 2022 International Journal of Innovative Science and Research Technology

ISSN No:-2456-2165

Green Synthesis of Calcium Oxide Nanoparticles

using Murraya Koenigii Leaf (Curry Leaves) Extract
for Photo-Degradation of Methyl Red and Methyl
Blue
Muhammad Ismail1, Chen Xiaoguang1, 2, *
1. Shanghai Frontier Science Research Center for Modern Textiles, College of Environmental Science and Engineering,
Donghua University, Shanghai, 201620, China
2. State Environmental Protection Engineering Center for Pollution Treatment and Control in Textile Industry, Donghua
University, Shanghai, 201620, China

Abstract:- Dyes are the main input as a coloring agent for earth. Therefore, its proper treatment is necessary before
textile and some other industries. When these discharging it to environment (Zhou et al., 2021b).
wastewaters enter into nearby marine environment, it can
harm marine species and pollute the whole freshwater Nanotechnology is a new, advanced and promising for
ecosystem. So, treatment of these industrial effluents is treatment of pollutions. Nanoscience is today on the path of
necessary before discharging it to the environment. generating new, advanced and sustainable materials.
Currently, we have synthesis a non-toxic and biogenic Traditionally, Nanoparticles and nanomaterials have been
CaO nanoparticle from the leaves of Murraya koenigii made using chemical and physical process. However, these
leaves. Then the nanoparticles were characterized using nanoparticles were toxic, expensive and unsustainable for
UV, FTIR, XRD, SEM and TEM. The UV data shows application in the field of Environment and several others.
absorbance at 345 nm. While the obtained band gap was Currently, scientists are exploring biological approach for
about 2.5 eV. Further, characterization tests confirmed synthesis of nanoparticles. (Jyoti and Singh, 2016)
the formation of CaO nanoparticles. CaO nanoparticles
was applied for treatment of methyl red and methyl blue Bio-nanoparticles are those nanoparticles composed
dyes solutions under UV light and without UV light in from biological sources such as plants, bacteria, Fungai and
order to check its degradation capability. Methyl red yeast. An extensive work has been done on synthesis of green
degradation was slow as compared to methyl blue. The nanoparticles from various biological sources (Jyoti and
results obtained shows that, under UV light the Singh, 2016) (Saravanan et al., 2017) (Sriramulu and
synthesized nanoparticles fully degrade methyl blue in 20 Sumathi, 2018) (Nadaf and Kanase, 2019). While its
minutes. Whereas, 70% methyl red was degraded in 60 treatments capabilities of dyes in aqueous media was also
minutes under UV light. While, without UV light the studied. Most commonly, metals oxides and plants extracts
degradation was about 10% for methyl blue and 5% for are mixed with each other as a precursor and reducing agent
methyl red respectively. for synthesize of various metals-based nanoparticles.
However, some researches show that, these metals-based
I. INTRODUCTION nanoparticles can put adverse effects on living cell and can
damage DNA, cell membrane and electron transport chain
Since 1856, after the discovery of first synthetic dye, (Griffitt et al., 2008) (Rana et al., 2020).
about 10000 new dyes has been produced until now. While,
approximately 70%-75% of these dyes are azo dye. Which Green Calcium oxide is considered as non-toxic, cheap,
are considered very hazardous for human health. Methyl red efficient, sustainable and suitable for application in the
and methyl blue is also an azo dye and contain aromatic and treatment of wastewater. (Jaiswal et al., 2021) synthesized
–N = N– groups in their molecules. It is very toxic for CaO nanoparticles from eggs shell and applied it for
humans, plants and animals. It can cause a series of human photocatalysis of methyl blue. The results indicated that 98%
health problems including cancer, birth defects, allergies and of methyl blue was degraded in 180 minutes. However, plant
endocrine disruption (Zhou et al., 2021a). extract based CaO nanoparticle is not fully explored for
degradation of methyl red.
These dyes are mainly used by textile industries as a
coloring agent. Every year more than 800000 tons of dyes are In this research, we have synthesized a green calcium
produced and utilized for coloring purposes. However, during nanoparticle from the leaves extract of Murraya Koenigii
dye-processing major portion of dyes are lost in the form of (curry) plant and eualvate its photodegradation capabilities of
wastewater. These dyes-containing wastewater are released Methyl red and methyl blue dye.
to fresh water bodies. Where these wastewaters mix-up with
clean water and contaminate the little available fresh water
and put hazardous effects on humans, flora and fauna of the

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Volume 7, Issue 11, November – 2022 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
II. MATERIALS AND METHODS the degradation ability of green CaO nanoparticle. 50mg dye
was dissolving into 100 ml distilled water. While 10mg CaO
A. Synthesis of CaO nanoparticle nanoparticles was added to the dye solution along with 5ml
Firstly, for preparation of leaves extract, we take 50 of 0.05 mole NaBH4. The solution was stirred using magnetic
grams of dried Murraya Koenigii plant leaves, wash it with stirrer under 100-watt bulb and samples were taken after
distilled water and cut it into more small pieces. While boiled every 5 minutes. Finally, all samples were tested.
it in 100 ml distilled water for about 1 hour. After boiling, the
solution was filtered using filter paper and get the extract of III. RESULTS AND DISCUSSIONS
Murraya Koenigii plant leaves.
A. Characterization of nanoparticles
Secondly, 2 grams of Calcium Chloride was dissolved The synthesized nanoparticles were characterized in
in 20 ml distilled water. The solution of calcium chloride was order to know the physical and chemical characteristics of the
added to 30ml plant extract and was stirred using a magnetic prepared nanoparticles.
stirrer for one hour. While 4 grams NaOH was dissolved in
40 ml distilled water and was added drop wise to the solution  UV–visible absorption
during stirring. During reaction, when we added reducing agent the
color of the reaction was changed from green to yellow and
Finally, the stirred solution was filtered using filter after calcination the color of the particles changed from
paper and the obtained precipitate was dried in an oven for 3 yellow to gray clearly indicating that reducing agent was
hours at 100 Co. Then the dried precipitate was calcinated for involved in reaction and particles were properly calcinated.
3 hours at 400 Co (Bano and Pillai, 2020). Further analysis was done using UV-visible absorption
spectrometer in order to confirm the formation of CaO
B. Characterization nanoparticle. A small amount of CaO nanoparticles was
Characterization was done using various instruments dissolved in distilled water and the sample was sonicated for
and characterization technique to examine the 2 minutes and then UV was performed. The UV spectra
physiochemical properties of the prepared CaO nanoparticle. absorbance was peaked at 345 nm. The sharp peak visibly
These techniques include UV-Visible spectroscopy, Fourier representing the characteristic of a nanoparticle. The band
transform infrared spectroscopy (FRIR), X-ray diffraction gap of the synthesized nanoparticle was also calculated using
(XRD), scanning electron microscopy (SEM), and Tauc plot method. The obtained band gap was about 2.5 eV.
transmission electron microscopy (TEM). The smaller band gap material performs better in a
photocatalytic activity. Because, the excitation of electron
C. Photocatalytic degradation setup depends upon the band gap. The smaller the band gap, the
An experiment on the photocatalytic degradation of easily will be the excitation of electron from valence band to
methyl blue and methyl red was carried out in order to know the conduction band.

Fig 1 : UV-VIS graph and Band gap

Fourier Transform Infrared (FTIR) Spectroscopy

Fourier Transform Infrared (FTIR) Spectroscopy of CaO nanoparticle was performed in the range of 4000 cm -1 to 600 cm-1 in
order to know about different functional groups present on the surface of the nanoparticles. The FTIR spectra Shows that the sharp
peaks were found at 1394.54 cm-1, 871.82 cm-1 and 711.73 cm-1 respectively. These peaks indicate the presence of C–O, C–C, Ca–
O linkage etc in the nanoparticle. The Sharp peak at 1394.54 cm-1 and at 871.82 cm-1 suggests the presence of C-O and C-C bond

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Volume 7, Issue 11, November – 2022 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
which can be appointed to the carbonation of CaO nanoparticles. While a sharp peak at 711.73 cm-1 indicates the presence of Ca–O
bonding which can be attributed to the presence of calcium oxide.

Fig 2: Fourier Transform infrared spectroscopy graph.

 X-ray Diffraction (XRD)

X-ray Diffraction (XRD) Analysis were performed to identify the crystallinity and nanosize of the prepared CaO nanoparticle
in the spectrum range of 10o to 60o. The X-ray diffraction patterns shows sharps and definite X-ray diffraction peaks. Which clarify
that particles size of the prepared CaO nanoparticles were in the nanoscale range. The observed diffraction peaks located at 23.0,
29.4, 31.4, 35.9, 39.4, 43.1, 45.5, 47.5, 48.5, 56.3, and 57.4° are found in good agreement with standard JCPDS data NO.77-2,376.
The Crystallinity of the prepared nanoparticles were calculated using the Debye-Scherrer formula (𝐃 = Κλ/β cos 𝜃). where D is
the average particle size, k is the Scherrer constant (0.94 for spherical particles), λ is the wavelength (1.54A), and ß is the FWHM
(full width at half-maximum). The crystallite size of the most intense peak located at 29.3 o is about 31.65 nm and the crystallite
size of the lowest peak located at 56.3o is about 0.34 nm. While the average crystallite size is 3.89 nm.

Fig 3: XRD graph

 Scanning Electron Microscopy (SEM)
Scanning Electron Microscopy (SEM) was performed to assess the morphology and particle size of the CaO nanoparticle. The
SEM micrographs indicates that the particles are in irregular shape. Additionally, its distributions are nonuniform and looks like a
cluster because of agglomerations of particles. While the size of the particles is ranging from 6.3 nm to 18.3 nm and the average
particle size is about 9.9 nm.

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Volume 7, Issue 11, November – 2022 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165

Fig 4: Scanning Electron Microscopy

 Energy-Dispersive X-ray (EDX)

Energy-Dispersive X-ray Analysis (EDX) was performed in order to identify the elemental composition of CaO. The EDX
clearly reveal the formation of CaO nanoparticles. The total Percentage of Ca was about 24.54% while the percentage of oxygen
was 50.14 %. While the presence of C was due to plant extract and Na and Cl due to the chemicals used in the reaction.

Fig 5: Energy-Dispersive X-ray

B. Analysis of Photodegradation Properties of Nanoparticles

The CaO nanoparticles were applied for degradation of azo dyes under UV light source and without UV light source to assess
the photodegradation property of nanoparticles.

 Degradation of dyes with UV light

In order to test the dyes degradation capability of calcium oxide nanoparticles, the photocatalytic activity was carried out on
methyl blue and methyl red. Methyl blue and methyl red solution was prepared by dissolving 50 mg dye in 100 ml distilled water
and the initial absorption peak was recorded for both dyes using UV- Visible spectrometer. While only 10mg CaO nanoparticle was
added along with 5ml of 0.05 mole NaBH4. Both solutions were stirred under 100-watt bulb and samples were taken after every 5
minutes and investigated using UV- Visible spectrometer. Methyl blue was fully degraded in 20 minutes. The degradation
percentage of methyl blue was the same in every sample. Methyl red was initially degraded very fast and slowed down with time.
While after 60 minutes further degradation was almost constant.

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Volume 7, Issue 11, November – 2022 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165

Fig 6: Methyl blue photodegradation and effects of time

Fig 7: Methyl red photodegradation and effects of time

 Degradation of dyes without UV light

An experiment on the degradation of dyes without UV light was carried in order to know about the absorption capacity of the
synthesized nanoparticles. Dyes solutions of Methyl red and methyl blue were prepared by dissolving 50 mg dye in 100 ml distilled
water and the initial absorption peak was recorded for both dyes using UV- Visible spectrometer. While only 10mg CaO nanoparticle
was added along with 5ml of 0.05 mole NaBH4. Both solutions were kept in dark for about 2 hours and samples were taken from
both solution after every 30 minutes. The results show that, the absorption capacity of CaO with UV is very low. Methyl red was
degraded up to 5% in 120 minutes and after 120 minutes the same peak was observed showing no more degradation. Similarly,
about 10% methyl blue was degraded in 180 minutes. While after 180 minutes the degradation was stopped as shown in the following
figures.

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Volume 7, Issue 11, November – 2022 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165

Fig 8: Methyl blue and methyl red degradation in dark

IV. CONCLUSION oxide for photocatalytic application in methylene blue

dye degradation under natural sunlight irradiation.
Nanoparticles and nanomaterials have very great Inorganic and Nano-Metal Chemistry, 51, 995-1004.
potential. Biobased Calcium oxide nanoparticle are cheap and [4]. JYOTI, K. & SINGH, A. 2016. Green synthesis of
non-toxic to humans and all other species. nanostructured silver particles and their catalytic
(1) We synthesized a biobased CaO nanoparticle in this application in dye degradation. Journal of Genetic
study. The prepared nanoparticles were characterized for Engineering and Biotechnology, 14, 311-317.
physicals and chemicals characteristics. The UV-VIS [5]. NADAF, N. Y. & KANASE, S. S. 2019. Biosynthesis
spectroscopy data reveals the formation of good and of gold nanoparticles by Bacillus marisflavi and its
stable nanoparticles. The FTIR and TEM data further potential in catalytic dye degradation. Arabian Journal
clarify the presence of calcium and oxygen bond and of Chemistry, 12, 4806-4814.
calcium oxygen contents respectively. While, XRD and [6]. RANA, A., YADAV, K. & JAGADEVAN, S. 2020. A
SEM shows that the synthesized nanoparticles are in nano comprehensive review on green synthesis of nature-
size. inspired metal nanoparticles: Mechanism, application
(2) It has the potential to degrade dyes and majority of other and toxicity. Journal of Cleaner Production, 272,
pollutants. The synthesized CaO nanoparticles fully 122880.
degrade methyl blue in 20 minutes under UV light. While, [7]. SARAVANAN, C., RAJESH, R., KAVIARASAN, T.,
only 70% methyl red was degraded in 60 minutes under MUTHUKUMAR, K., KAVITAKE, D. & SHETTY, P.
UV light. Whereas, without UV light the degradation was H. 2017. Synthesis of silver nanoparticles using
about 10% for methyl blue and 5% for methyl red bacterial exopolysaccharide and its application for
respectively. degradation of azo-dyes. Biotechnology Reports, 15, 33-
40.
ACKNOWLEDGEMENTS [8]. SRIRAMULU, M. & SUMATHI, S. 2018. Biosynthesis
of palladium nanoparticles using Saccharomyces
The project was funded by Shanghai Frontier Science cerevisiae extract and its photocatalytic degradation
Research Center for Modern Textiles，Donghua University. behaviour. Advances in Natural Sciences: Nanoscience
and Nanotechnology, 9, 025018.
REFERENCES [9]. ZHOU, W., CHEN, X., ISMAIL, M., WEI, L. & HU, B.
2021a. Simulating the synergy of electron donors and
[1]. BANO, S. & PILLAI, S. 2020. Green synthesis of different redox mediators on the anaerobic
calcium oxide nanoparticles at different calcination decolorization of azo dyes: Can AQDS-chitosan
temperatures. World Journal of Science, Technology globules replace the traditional redox mediators?
and Sustainable Development, 17, 283-295. Chemosphere, 275, 130025.
[2]. GRIFFITT, R. J., LUO, J., GAO, J., BONZONGO, J. C. [10]. ZHOU, W., CHEN, X., WANG, Y., TUERSUN, N.,
& BARBER, D. S. 2008. Effects of particle composition ISMAIL, M., CHENG, C., LI, Z., SONG, Q., WANG,
and species on toxicity of metallic nanomaterials in Y. & MA, C. 2021b. Anaerobic co-digestion of textile
aquatic organisms. Environmental Toxicology and dyeing sludge: Digestion efficiency and heavy metal
Chemistry: An International Journal, 27, 1972-1978. stability. Science of The Total Environment, 801,
[3]. JAISWAL, K. K., DUTTA, S., POHRMEN, C. B., 149722.
VERMA, R., KUMAR, A. & RAMASWAMY, A. P.
2021. Bio-waste chicken eggshell-derived calcium

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