Sustainable Chemistry and Pharmacy 22 (2021) 100453

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Sustainable Chemistry and Pharmacy

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Photocatalysts synthesized via plant mediated extracts for degradation of

organic compounds: A review of formation mechanisms and application in
wastewater treatment
Angel Joseph , Arya Vijayanandan *
Department of Civil Engineering, Indian Institute of Technology, New Delhi, India

A R T I C L E I N F O A B S T R A C T

Keywords: Photocatalysis is a promising technology to remove several persistent and recalcitrant pollutants in water and
Green photocatalyst wastewater. Most of the conventional chemical and physical synthesis routes of photocatalysts result in the
Green synthesis release of toxic pollutants to the environment and hence green synthesis is a better alternative. Green synthesis of
Nanoparticles
photocatalyst using plants, fungi, bacteria, yeast, and other biological sources is widely explored in recent years.
Photocatalysis
Photodegradation
The presence of various biomolecules used in green synthesis replaces conventional reducing and stabilizing
Water and wastewater treatment agents such as hydrazine, sodium borohydride, ascorbic acids, and other polymer substitutes. This review focuses
on the synthesis of photocatalysts using plant extracts through different synthesis routes and explores the efficacy
of photocatalyst synthesized via plant extract mediated synthesis routes in the photodegradation of organic
compounds present in water. The pathway as well as the factors affecting the formation of photocatalysts, the
role of plant extract in the photocatalytic properties are explored in detail. The action of plant-mediated pho-
tocatalyst on the pollutant and the underlying predominant degradation mechanism are also discussed. Besides,
this study gives an insight into the recyclability of the photocatalyst synthesized via plant extract mediated
synthesis routes and addresses future perspectives and the challenges of green photocatalysts.

1. Introduction cadmium sulfide (CdS) (Xiong et al., 2013), cadmium selenide (CdSe)
(Amiri et al., 2014), iron oxide (FeO) (Khedr et al., 2009), zinc oxide
Photocatalysis has emerged as a promising treatment technology for (ZnO) (Lee et al., 2016) and, tungsten oxide (WO3) (Mohagheghian
the degradation and complete mineralization of toxic pollutants such as et al., 2015) are some of the photocatalysts which are extensively used in
pharmaceuticals (Mirzaei et al., 2016), pesticides (Fiorenza et al., 2020), the laboratory scale studies for the degradation of organic pollutants.
surfactants (Castillo et al., 2001), microplastics (Tofa et al., 2019), and Application of nanoparticles (NPs) such as silver (Ag) (Jiao et al., 2015;
other persistent organic pollutants present in water bodies (Yerkinova Yola et al., 2013), gold (Au) (Wang et al., 2008), TiO2 (Shahrezaei et al.,
et al., 2018). Compared to other conventional treatment technologies, 2012), Copper Oxide (CuO) (Rafique et al., 2020), copper (Cu) (Hai
photocatalytic processes are considered to be less expensive (Bumpus et al., 2013), cerium (Ce) (Sasikala et al., 2016; Xue et al., 2011), nickel
et al., 1999) and are free of polycyclic product formation (Muhd Julkapli ferrite (NiFe2O4) (Xu et al., 2007), iron (Fe) (Solano et al., 2019), iron
et al., 2014). Photocatalytic processes are not widely adopted as an in- oxide (FeO) (Xu et al., 2012), iron (III) oxide (Fe3O4) (Mousavi and
dustrial treatment option due to challenges faced in the development of Habibi-Yangjeh, 2018), molybdenum trioxide (MoO3) (Xi et al., 2019),
improved catalyst materials, catalyst recovery (Djuri!si”c et al., 2020), nickel oxide (NiO) (Hayat et al., 2011), tin dioxide (SnO2) (Srivastava
toxicity, safe disposal of synthesized catalyst (Zakria et al., 2021), and Mukhopadhyay, 2014), selenium (Se) (Alagesan and Venugopal,
immobilization of the catalyst and in build-out of reactor configurations 2019), and, ZnO (Jadhav and Biswas, 2018; Zhang et al., 2018) were
(Loeb et al., 2019). The efficiency of the photocatalytic process mainly considered to be one of the main breakthroughs in the advancement of
depends on its ability to produce reactive oxygen species (ROS) such as photocatalytic processes, as NPs ensure more surface area thereby
hydroxyl radicals, superoxide ions, and peroxyl radicals (Prihod’ko and increasing the selectivity of the catalyst (Kamat and Meisel, 2002). Due
Soboleva, 2013). Titanium dioxide (TiO2) (Kanakaraju et al., 2014), to unique particle properties and high surface area, NPs are used widely

* Corresponding author.
E-mail address: aryav@[Link] (A. Vijayanandan).

[Link]
Received 1 December 2020; Received in revised form 11 May 2021; Accepted 13 May 2021
Available online 11 June 2021
2352-5541/© 2021 Elsevier B.V. All rights reserved.
A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

in various areas such as biomedical, optical, energy, and electronics and cost effective (Nasrollahzadeh et al., 2019). In this context, the
(Kharisov et al., 2019). synthesis of novel and green photocatalyst with high degradation po-
Basically, the synthesis of NPs includes physical, chemical, and tential is the need of the hour. Nonetheless, green catalysis, which relies
biological methods. One of the main drawbacks associated with NPs is on two key concepts of atom efficiency and E factor, makes the treat-
the difficulty in recovery after the treatment. Hence, there is a chance of ment processes more sustainable (Sheldon et al., 2007).
these nano-sized photocatalysts escaping into the environment and Recently, photocatalysts synthesized through biological routes are of
becoming another toxicant (Lee and Park, 2013). In most of the chemical great interest as it contributes to clean technology. Green synthesis of
processes, different reducing and stabilizing agents such as hydrazine, NPs has many advantages as it is environment-friendly and relatively
sodium borohydride, ascorbic acids, polymers are highly exploited (Md cost-effective (Kharissova et al., 2013). In green synthesis approaches,
Ishak et al., 2019). natural substitutes like plants (Goutam et al., 2020), fungi (Gupta and
Conventional synthesis processes such as physical and chemical ap- Chundawat, 2019; Li et al., 2019), and bacteria (Pugazhendhi et al.,
proaches require higher energy utilization and are comparatively 2018; Srivastava and Mukhopadhyay, 2014) are used in the synthesis of
expensive (Ijaz et al., 2020). In most of the chemical synthesis processes, photocatalyst (Ravichandran et al., 2019). This type of green photo-
highly toxic solvents are required and the generation of toxic catalyst reduces the need for excessive chemicals. Among these natural
by-products is unavoidable (Pantidos, 2014). The main difference in substitutes, plants have been greatly explored for the production of
plant extract mediated synthesis route lies in the replacement of metal NPs such as TiO2 (Nadeem et al., 2018), ZnO (Ong et al., 2018),
chemical reducing agents with biomolecules of plant extract which is CuO (Das et al., 2018; Haseena et al., 2019) magnesium oxide (MgO)
exemplified in Fig. 1. The plant extracts are generally prepared by a (Jeevanandam et al., 2017; Suresh et al., 2018a), platinum (Pt) (Song
simple extraction process (boiling leaves in deionized water for a et al., 2010), and Ag (Kuppusamy et al., 2016; Latha et al., 2019;
particular period and specified temperature) (Hamidi et al., 2019; Kar- Taghavizadeh Yazdi et al., 2019). Compared to other biological nano-
thik et al., 2017; Ravichandran et al., 2019). Hence these approaches are particle synthesis routes (bacteria, yeast, and fungi), plant extract
considered to be feasible for the commercial production of NPs on a mediated nanoparticle synthesis routes are considered to be a more
larger scale. However, the challenges include difficulty in controlling advantageous method as in the case of microorganisms, cell mainte-
the stability and aggregation of synthesized nanocomposites/NPs (Das nance time is limited, the risk of contamination is more, requires high
et al., 2017). These underlying challenges are common in nanoparticle aseptic conditions and long incubation periods (Baker et al., 2013;
synthesis and however, more attention should be given to the plant Narayanan et al., 2011). Different parts of the plant including leaves,
extract mediated synthesis of photocatalysts approaches as these hold a fruits, seeds, flowers, and other parts are reported in the utilization for
high degree of futuristic scope (Bhattarai et al., 2018). Cost-effectiveness the synthesis of metal NPs with different sizes and shapes (Prasad et al.,
is another important factor that needs to be analyzed to understand 2017). Plants contain active biomolecules such as sugars, terpenoids,
industrial feasibility. In case of chemical synthesis, the main cost of the polyphenols, phenolic acids, alkanoids and proteins, which cause the
process depends upon the reducing agents and from the metal salt bioreduction of metallic ions. The selection of plant parts (leaves, root,
(Vasyliev et al., 2020). However, in plant-mediated photocatalyst syn- fruit, stem, or seed) depends on the presence of these biomolecules and
thesis process, the overall cost mainly relies only on the metal salt. their concentration (Jain and Mehata, 2017). Recently, several studies
Hence this plant mediated route results in recyclable waste materials have focused on the development of photocatalysts produced via
and safer disposal of the used NPs makes the approach more sustainable plant-extract- mediated synthesis processes (PPS) as plant extracts have

Fig. 1. Comparison of chemical and plant extract-mediated photocatalysts synthesis approach.

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

been identified with its potential to form stable NPs (Kumar et al., 2020; (c) Termination phase: This phase defines the shape of NPs and
Kuppusamy et al., 2016; Md Ishak et al., 2019; Mittal et al., 2013). In the marks the end stage of NPs synthesis. Due to the action of sec-
past decade, many studies have been reported the pollutant degradation ondary metabolites, the stabilization of NPs takes place and NPs
potential of PPS (Adinaveen et al., 2019a; Arularasu et al., 2018; Begum attain stable morphology. (Si and Mandal, 2007). The hydroxyl
and Ahmaruzzaman, 2018; Karthik et al., 2017; Sethy et al., 2020). groups present in the Eichhornia Crassipes were reported to be the
Ample attention should be given to green synthesis approaches that dominant factor behind the stabilization of TiO2 NPs which also
explore sustainable methods for water and wastewater treatment. aided in the inhibition of subsequent agglomeration of particles
In this context, the main focus of this article is to review the available (D. Lu et al., 2019). As the period of the growth phase extends,
literature on PPS and its prospective applications in wastewater treat- NPs possess different shapes and sometimes may result in irreg-
ment. Besides, PPS synthesis approaches, mechanisms involved in the ularity in shapes as well. During the termination phase, the in-
formation of NPs using plant extracts, factors affecting PPS formation, teractions of plant biomolecules enable NPs to acquire stable
pollutant degradation mechanisms, and reusability possibilities of PPS morphology (Ghodake et al., 2010).
are presented in detail and research gaps are identified. Even though
several studies have been conducted in the field of green synthesis of Different morphological variations (nanorods, triangles, nanowires,
NPs, the studies focusing on the applicability of PPS in the field of hexagons, pentagons, cubes, ellipsoids, and spheres) in NPs are resulted
photocatalysis with a focus on water and wastewater treatment are still due to the variations in interactions between metal ions and bio-
limited and this review aims to give an insight into these aspects. molecules (Haverkamp and Marshall, 2009). The size and morphology
of NPs mainly vary depending upon the interaction of metal ions and
2. Mechanism of formation of PPS biomolecules of plants (Shankar et al., 2004). Previous studies have
investigated the morphological characteristics of PPS using Field Emis-
PPS are synthesized using plant extracts in which the biomolecules sion Scanning Electron Microscope (FE-SEM), Transmission Electron
present in plants act as stabilizing and reducing agents. (Raveendran Microscopy (TEM) and Energy Dispersive X-Ray analysis (EDX). Kahsay
et al., 2003). Various metabolites present in plants including terpenoids, et al. (2019) reported the formation of hexagonal and triangular ZnO
polyphenols, sugars, alkaloids, phenolic acids, and proteins aid in the nanostructures having size ranging from 7 to 49 nm (Fig. 2 (i)) using
biological reduction of precursor metal ions and also ensure subsequent plant extract of Dolichos lablab L. while the formation of rod-shaped
stability (Shankar et al., 2003). The polyphenols such as flavonoids ZnO nanostructures was reported by Davis et al., 2019 following a
comprising anthocyanins, isoflavonoids, flavonols, chalcones, flavones, normal chemical synthesis route (Fig. 2(ii)). Variation from rod-like
and flavanones assist in nanoparticle formation (Vijayaraghavan and shape to the triangular shape of ZnO nanostructures shows that the
Ashokkumar, 2017). During the synthesis process, the plant secondary plant extracts have a significant role in determining the morphology of
metabolites react with the metal salt added and cause the reduction of synthesized nanoparticles and similar observations were reported in
metal ions to its NPs form. Additionally, the release of reactive hydrogen other studies (Sheny et al., 2011; Vijayaraghavan and Ashokkumar,
atoms due to the flavonoid transformations (from enol-form to 2017). It is also reported that the hexagonal and spherical-shaped ZnO
keto-form) also causes the reduction of metal ions (Shankar et al., 2003). nanoparticles with higher specific surface area exhibited enhanced the
Also, these biomolecules prevent the agglomeration of NPs and act as a photocatalytic activity (Demissie et al., 2020). The presence of plant
stabilizing agent. The main advantage of PPS is that the biomolecules of extracts attributed to the formation of hexagonal wurtzite structured
plant extract can provide the dual role function of both reducing and ZnO thereby enhancing the phase purity and crystallinity of the syn-
capping agent. The process of syntheses of PPS initially starts with the thesized nanoparticles. The presence of C in the peaks of EDX analysis
mixing of a suitable plant extract with the precursor salt. The primary confirms that organic molecules of plant extract were predominant and
role of reducing agents is to transfer electrons to the precursor metal ions acted as the capping agent for ZnO formation.
to form atoms and further these atoms combine to form particles. While SEM and TEM images of CuO/TiO2 nanocomposite synthesized via
the capping agent aids in the stabilization of the NPs. Stabilization is the hydrolysis method using Eichhornia crassipes represented that these
process that controls the growth of particles, inhibits particle aggrega- nanocomposites exhibited smaller crystalline structure, higher pore
tion, and controls the overall size of the particle (Ahmed et al., 2016; volume, smaller size, and higher specific surface area compared to pure
Lade and Shanware, 2020). Several studies have elucidated the mech- CuO/TiO2 nanocomposite (D. Lu et al., 2019). Aggregation was not
anism of PPS formation. Three mechanisms are reported to take place apparent in NiO nanoparticles synthesized using Nephelium lappaceum L.
during NPs synthesis using plant extracts. peel extract and PPS exhibited uniform morphology and better photo-
catalytic properties due to higher surface area (Adinaveen et al., 2019).
(a) Activation phase: During this phase, the reduction of metal ions Another study reported that due to the presence of phenolic compounds,
will take place and the subsequent nucleation of reduced metal enhancement in the surface area and morphological characteristics of
ions will be initiated. The biomolecules mainly take part in this TiO2 NPs (synthesized by utilizing Jatropha curcas L. plant extracts) was
reduction process, thereby metal ions from their higher oxidation achieved (Goutam et al., 2018). TEM images of TiO2 NPs, produced
states are converted to their lower oxidation states mainly to using V. Thapsus plant extract showed dispersed particles without any
zero-valent form (Singh et al., 2018). For example, the u-OH agglomeration which indicates the capping efficiency of phytochemicals
group present in fructose (biomolecule present in the extract) was present in the plant extract (Esfahani et al., 2020).
responsible for the reduction of the ionic state of Ag ions to its However, some studies reported that controlling the morphology of
zero-valent state (Zaheer, 2018). Phenolic compounds present in PPS is challenging due to the aggregation of NPs. The aggregation of
the germanium leaves were observed to bind and reduce the Ag ZnO NPs has been noticed in the case of plant extract mediated synthesis
salt into NPs form (Shankar et al., 2003). Further, these reduced route while normal ZnO nanoparticle exhibits distinct spherical shapes
metal atoms begin the new phase of the particle formation with the least aggregation (Stan et al., 2015). Similarly, agglomeration
through the nucleation of these atoms and progressively move to of CuO NPs prepared from Artabotrys hexapetalus and Bambusa vulgaris
the next stage. plant extract was also observed. This agglomeration is due to the pres-
(b) Growth phase: This phase mainly results in the spontaneous ag- ence of plant biomolecules on the surface of the NPs. These surface
gregation of the small adjacent NPs, which coalesce to form biomolecules attract the adjacent other biomolecules and initiate
particles of a larger size. In this stage, due to non-selective ag- agglomeration (Haseena et al., 2019). In the case of ferrite NPs, in
gregation, particles are reported to show different morphologies addition to the biomolecule attraction, agglomeration due to magnetic
(Iravani, 2011). dipole interaction was also reported (Somanathan et al., 2019).

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

Fig. 2. (i) (a–c) FE-SEM and (d) EDX of hexagonal and triangular shaped ZnO nanostructures synthesized from leaf extract of Dolichos lablab L. (Reproduced from
Kahsay et al. (2019) with permission of the Royal Society of Chemistry) (ii) SEM images of rod-shaped ZnO nanostructures synthesized from the chemical route
(Reproduced from Davis et al. (2019) with permission of the Royal Society of Chemistry).

Fig. 3. Pathway of PPS formation.

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

Fig. 3 represents the reaction mechanism behind the metal NPs for- and protein in apple extract act as the main cause of the reduction of
mation using plant extracts. In general, the plant part (leaves, seed, metallic Ag ions to Ag NPs (Parthibavarman et al., 2019). The presence
stem, flowers, or fruits) undergoes drying and other pretreatment pro- of -OH, -C-O-, -NH2, -C-O- and -C↑O in flavonoids and terpenoids en-
cesses followed by the preparation of plant extract (which mainly con- hances linkages on the NPs surfaces which support Ag NPs fabrication
stitutes biomolecule part). Further, precursor metal salt reacts with this using Azadirachta indica leaf extract and reported as effective PPS for the
biomolecule to form complexes which then hydrolyze to form PPS. catalytic degradation of dyes (Singh et al., 2019). Enhancement in the
Subsequently, the calcination process helps the synthesized PPS to attain thermodynamic stability of the particle can be ensured by the action of
crystallinity. these biomolecules (Alagesan and Venugopal, 2019). Different peak
Matinise et al. (2017) investigated the properties of ZnO NPs syn- variations of the FTIR spectrum confirms the presence of different
thesized using Moringa Oleifera and concluded the study by proposing functional groups such as OH group, -C-O- bonds of carboxylic groups,
the mechanism of synthesis in which solvated Zn2→ ions are reduced to and alcohols and aromatic phenols present in the biomolecules of
their lower state by the action of three phytochemicals such as flavo- C. sinensis leaves extract and aid in the formation of copper NPs (Ahmed
noid, phenolic acid, and other vitamin compounds and the process et al., 2019). C-N aliphatic amines, amino and carboxylic groups, carbon
further proceeds to electrostatic attraction of free radical and cation and hydroxyl group proteins, amide II grouped proteins, C-O of amide
present in the precursor salt added. Osuntokun et al., 2019 described a conjugates of protein, hydroxyl groups of phenol, alcohols, and C-H
plausible mechanism for the formation of ZnO NPs using broccoli extract alkane groups attributes to the formation of cogpper NPs by using
and exemplified the potential of synthesized ZnO NPs as PPS for the Artabotrys hexapetalus and Bambussa vulgaris plant extract (Haseena
degradation of methylene blue (MB) and phenol red dyes. Quercetin is et al., 2019; Shim et al., 2019). In the zirconium NPs synthesis using
one of the main biomolecules present in the broccoli extract which acts Ficus benghalensis leaf extract, the polyphenols present in leaf extract
as the main reducing agent in the synthesis of ZnO NPs. Basically, two actuates the complex formation with -OH groups. FTIR analysis sub-
steps were involved in ZnO formation, firstly, zinc hydroxide formation stantiated the presence of C-H, C↑O, O-H bonds validating that inter-
stage from zinc chloride salt and secondly conversion of this interme- mediate forms of phenolic groups, proteins, carboxyl groups, amines,
diate product formed into ZnO NPs by calcination process (Ezealisiji and carbohydrates are the principal factors governing the NPs formation
et al., 2019). The formation of the hydroxide complex is due to the (Shinde et al., 2018).
bonding of the OH group present quercetin with metal chloride. Sub-
sequently, the calcination process caused the reduction of metallic ions 3. Synthesis routes of PPS
and resulted in the formation of ZnO NPs (Suresh et al., 2018b). Kashay
et al., 2019 also proposed the mechanism of ZnO formation using Doli- NPs can be synthesized in two ways: one approach is top to bottom
chos lablab L as the reducing and stabilizing agent. Flavonoids and (from the bulk material, size is reduced) and the other one is bottom to
phenolic compounds are found to be the most effective phytochemicals top (from the atomic level to the nanosize level). In the case of top to
responsible for the formation of Ag NPs using Parkia speciosa leaves bottom approach, nanoscale particles are obtained from grinding or
extract (Ravichandran et al., 2019). The presence of the enol group in milling the bulk materials (physical methods) whereas, in the bottom to
these phytochemical releases electrons which breaks the O-H bond and top approach, NPs are formed by the clustering of atoms or molecules
also causes the reduction of Ag ion to its zero-valent state. Further, the (includes chemical and biological approaches). PPS synthesis comes
Fourier-transform infrared (FTIR) analysis confirms the involvement of under the bottom-up approach of synthesis (Peralta-Videa et al., 2016).
these compounds in the reduction part and also acts as the capping agent In most of the chemical approaches, NPs are synthesized by the inter-
(Alagesan and Venugopal, 2019). action of three components, namely, precursor, reducing agent, and
Identification of reducing agents present in the selected plant species capping, or stabilizing agent. Table 2 gives an overview of different
is an important aspect to be considered as the nanoparticle formation types of PPS synthesized from different plant varieties. Basically, in PPS
depends upon the biomolecules present in the plant species as well its synthesis, biomolecules present in the plant extract act as a substitute for
reducing capacity. The reducing power of the plant species is deter- the toxic reducing and capping agents such as sodium borohydride and
mined using Ferric-Reducing Antioxidant Power (FRAP) method (El polyvinyl alcohol (Küünal et al., 2018). The nature and properties of NPs
Jemli et al., 2016). Some of the commonly used plant extracts were may vary depending upon the synthesis approach chosen. Even in the
arranged in the order of their power as a reducing agent and provided in final stage of synthesis, the separation technique (usually centrifuga-
Table 1. Mangifera indica (Olabinri et al., 2009) is found to possess tion) and the method chosen for purification have a major role in
comparatively more reducing power than the other species considered. determining the nature of NPs synthesized (Patra and Baek, 2014)
Parkia speciosa and Azadirachta indica can be preferably chosen for the (Baker et al., 2013). The synthesis route adopted for the biological
synthesis of PPS as the presence of reducing agents in these species was synthesis of PPS is chemically assisted but the main difference lies in the
also reported. Therefore the selection of such plant species containing replacement of reducing and capping agents by biomolecules of plant
strong biomolecules (reducing agent) is a crucial step in the overall extract. Different methods are used in the synthesis of PPS and certain
synthesis process (Das et al., 2017). important synthesis processes are discussed below.
The presence of phenolic and flavonoid compounds in V. thapsus
extract for the synthesis of TiO2 NPs was quantified using Folin - Cio-
calteu and aluminum chloride methods (Esfahani et al., 2020). And 3.1. Hydrothermal processes
suggested that these are the main factors responsible for the NPs for-
mation by acting as strong non-toxic reductants (Elemike et al., 2016). In the hydrothermal process, a reducing agent and a strong oxidizer
From the FTIR spectrum study, it has been concluded that ascorbic acid are introduced together in an aqueous medium under suitable pH con-
ditions. The process continues with the reaction of these reagents under
high pressure and at a specified temperature and duration (Genuino
Table 1 et al., 2012). Hydrothermal processes utilize a pressurized atmosphere
Reducing power of some of the commonly utilized plant species.
for the synthesis of NPs and usually, an autoclave is used for this purpose
Plant Species Reducing Power Reference (Carp et al., 2004). The hydrothermal route was used for the synthesis of
Mangifera indica 12.20–15.20 mM Fe2→/g Olabinri et al. (2009) iron oxide NPs synthesis using bamboo leaf extract (Fatimah et al.,
Parkia speciosa 11.7 mM Fe2→/g Siow and Gan (2013) 2019). Since this method requires additional systems for the generation
Azadirachta indica 6.80–9.20 mM Fe2→/g Olabinri et al. (2009) of pressurized atmosphere, this method is not highly recommended for
Moringa oleifera 0.99 ↓ 0.06 mM Fe2→/g Yong-Bing et al. (2019)
metal NPs synthesis.

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Table 2
Various types of PPS synthesized by adopting different synthesis routes.
Plant PPS Plant part Biomolecule Precursor salt Synthesis route References

Parkiaspeciosa Ag Leaf Flavonoids and phenolic Silver nitrate Colloidal Ravichandran et al.
compounds (2019)
Azadirachta Indica Ag Leaf Not mentioned (NM) Silver nitrate Colloidal Singh et al. (2019)
Extract of apple and grape Ag Fruit Carboxylic acids, proteins Silver nitrate Colloidal Parthibavarman et al.
(2019)
Tribulus Terrestris L. Ag Shoot NM Silver nitrate Colloidal Hamidi et al. (2019)
Camelia Japonica Ag Leaf Biomolecule containing -OH Silver nitrate Colloidal Karthik et al. (2017)
group
Palm date fruit Ag Fruit Fructose; pyranoid and furanoid Silver nitrate Colloidal Zaheer (2018)
Barleria longiflora L. Ag Leaf Phenolic agents and proteins Silver nitrate Colloidal Cittrarasu et al.
(2019)
Solidagoaltissima Ag Leaf Terpenoids, glycosides, Silver nitrate Colloidal Kumar et al. (2016)
acetylenes, phenols, and
components containing Cl↔
Averrhoa bilimbi and Au/TiO2 Fruit&Leaf NM Tetrachloroauric acid; Hydrolysis &Colloidal Yulizar et al. (2019)
Pandanus amaryllifolius Titanium (IV) isopropoxide
Madhuca longifolia CuO Flower& NM Copper (II) nitrate Colloidal Das et al. (2018)
seeds
Camelia Sinensis Cu Leaf OH-group, polyphenols, Copper(I) chloride Colloidal Ahmed et al. (2019)
Carboxylic groups
Artabotryshexapetalus and CuO Leaf Amino and carboxylic groups Copper (II) nitrate Colloidal Haseena et al. (2019)
Bambusa Vulgaris
Eichhornia crassipes CuO/ Leaf Hydroxyl groups Copper nitrate; Titanium Co-precipitation; Lu et al. (2019)
TiO2 chloride Hydrolysis
Calotropis Gigantean Ce/ Leaf Flavonoids; polyphenols Ferric nitrate, Nickel Microwave-assisted Somanathan et al.
NiFe2O4 nitrate, and ceric nitrate (2019)
Bamboo Leaf Ash FeO Leaf NM Ferric chloride Hydrothermal Fatimah et al. (2019)
Kappaphycusalvarezii Fe3O4 Leaf NM Iron (III) chloride Hot plate combustion (M. V. Arularasu
tetrahydrate; et al., 2018)
Iron (III) chloride
heptahydrate
Hibiscus Sabdariffa Fe Flower Phenolic compounds, flavonoids, Ferric chloride Colloidal Alshehri et al. (2017)
glycosides, and anthocyanins
Amaranthusdubis Fe Leaf Peptide bonds, amine, and a Ferric chloride Co-precipitation (M. Harshiny et al.,
carboxylic group 2015)
Abutilon Indicum MoO3 Leaf Vitamin E, mono linolein, palmitic Molybdate Colloidal Abinaya et al. (2019a)
acid, phytol, 9,12
Octadecadienoyl chloride
Nepheliumlappaceum L. NiO Fruit Ellagic acid Nickel nitrate Colloidal followed by Adinaveen et al.
calcination (2019b)
Aeglemarmelos NiO Leaf Carbonyl group; Hydroxyl group Nickel nitrate Hot plate combustion Angel Ezhilarasi et al.
(2018a)
Parkiaspeciosa Hassk SnO2 Seed NM Tin chloride Microwave-assisted Begum and
Ahmaruzzaman
(2018)
Withaniasomnifera Se Leaf Alcohols and phenols; carboxylic Selenious acid Colloidal Alagesan and
acids Venugopal (2019)
Verbascumthapsus TiO2 Leaf Polyphenols; carboxyl group Titanium oxide bulk powder Colloidal method Esfahani et al. (2020)
followed by
precipitation
JatrophacurcasL. TiO2 Leaf Polyphenolic tannins hydroxyl Titanium chloride Co-precipitation Goutam et al. (2018)
group
Justicia gendarussa TiO2 Leaf Hydroxyl alcohol group (O–H), Titanium tetra isopropoxide Sol-gel Senthilkumar and
Rajendran (2018)
Dolichos Lablab L. ZnO Leaf Alcohol or phenol, carboxylic, and Zinc acetate dihydrate Colloidal Kahsay et al. (2019)
ester groups
Allium sativum, Allium cepa, ZnO Leaf Free amino and carboxylic groups, Zinc nitrate hexahydrate Sol-gel Stan et al. (2015)
Petroselinumcrispum polyphenols
Cassia fistula ZnO Leaf Polyphenols and flavonoids Zinc nitrate hexahydrate Combustion Suresh et al. (2015)
Terminalia chebula ZnO Leaf Phenolic hydroxyl group, phenolic Zinc nitrate hexahydrate Co-Precipitation Rana et al. (2016)
acids, tannins, carboxylic acid,
and esters.
Azadirachta indica ZnO Leaf Flavanones, terpenoids, and Zinc acetate dihydrate Co-precipitation Bhuyan et al. (2015)
aldehyde groups
Citrus aurantifolia ZnO Fruit Carboxylic acid groups Zinc acetate Sol-gel Davar et al. (2015)
Moringa Oleifera ZnO Leaf Protein, hydroxyl, and carboxyl Zinc acetate dihydrate Co-precipitation Pal et al. (2018)
groups
Aloe vera ZnO Leaf NM Zinc acetate di-hydrate Co-precipitation Sharma et al. (2020)
Suaeda Japonica Makino ZnO Stem & Proteins, polyphenols, Zinc nitrate hexahydrate Co-precipitation Shim et al. (2019)
Leaf polysaccharides, carboxylic acids,
and hydroxyl group
Stevia Rebaudiana ZnO Leaf Phenols, flavonoids, and diterpene Zinc nitrate hexahydrate Co-precipitation Hoon Seo et al. (2019)
glycosides
Physalis alkekengi L. ZnO Shoot Zinc nitrate Co-precipitation Cong et al. (2014)
(continued on next page)

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

Table 2 (continued )
Plant PPS Plant part Biomolecule Precursor salt Synthesis route References

Polyphenols, hydroxyl, and

ketone
Codonopsis lanceoloata Cl-ZnO Root Aromatic aldehydes, amine, and Zinc nitrate hexahydrate Co-precipitation (Lu et al., 2019)
the carboxyl group
Ferulagoangulata ZnO and Leaf Polyphenols Zinc acetate dihydrate, Sol-gel Shayegan Mehr et al.
CuO Copper (II) acetate (2018)
monohydrate
Ficus Benghalensis ZrO2 Leaf Polyphenols and hydroxyl groups Zirconyl chloride Microwave-assisted Shinde et al. (2018)
octahydrate

3.2. Microwave-assisted methods metal ions or any organometal complexes (Ghodake et al., 2010; Mac-
Wan et al., 2011). For example, in the synthesis of nickel oxide NPs,
Microwave-assisted processes belong to rapid synthesis processes hydroxyl groups present in ellagic acid in rambutan react with nickel
that eliminate highly temperature-dependent calcination processes ions and result in the formation of metal - ellagate complexes. The
(Corradi et al., 2005). Microwave heating methods exclude the calci- resulting nickel-ellagate complex further undergoes hydrolysis and
nation process which is time-consuming and hence speeds up the entire precipitates metal oxides or hydroxides (Barnaby et al., 2011). Finally,
reaction (Ekar et al., 2017). This method was used for the synthesis of these complexes are subjected to the calcination process and result in
SnO2 and ZrO2 using extracts of Parkiaspeciosa Hassk and Ficus Bengha- nickel oxide NPs (Yuvakkumar et al., 2015). This method has also been
lensis respectively, (Begum and Ahmaruzzaman, 2018; Shinde et al., adopted for the synthesis of ZnO (Davar et al., 2015) and TiO2 (Sen-
2018). thilkumar and Rajendran, 2018) using Citrus aurantifolia and Justicia
gendarussa respectively.
3.3. Hydrolysis method
3.4. Co- precipitation methods
Hydrolysis synthesis of NPs is reported to be the most versatile
method as it has many advantages such as allowing impregnation (for In this method, soluble salts of required metal are co-precipitated in
doping), homogeneity of the product, and maintaining purity in chem- the common medium, usually hydroxides. Fig. 4 represents the stages
ical and morphological properties (Mackenzie and Bescher, 2007). involved in the synthesis of TiO2 PPS using [Link]
Basically, in this method, metal ions, as a result of hydrolysis produce a (Goutam et al., 2018). Co-precipitation involves the simultaneous for-
gel, which coagulates the particles so formed. Here the precursor can be mation of different phases such as nucleation, growth, and

Fig. 4. Stages of PPS formation by co-precipitation method.

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

agglomeration processes (Rajaeiyan and Bagheri-Mohagheghi, 2013). incorporated for the synthesis of PPS such as Ag, Cu, Fe, MoO3 and Se
This process has several advantages such as low temperature and energy respectively by following this method.
requirement, better control over the particle morphological character- Previous studies have reported the variations in the morphological
istics, and exclusion of organic solvent in the synthesis (Rane et al., characteristics of synthesized nanoparticles depending upon the syn-
2018). ZnO PPS is mainly synthesized using this method and this route thesis route adopted (Ravichandran et al., 2019; Fatimah et al., 2019;
has been reported to be one of the facile methods (Bhuyan et al., 2015; Sharma et al., 2020). Davar et al. (2015) reported that semi-spherical
Pal et al., 2018; Rana et al., 2016; Shim et al., 2019; Suresh et al., 2015). structures of ZnO resulted from sol-gel process. Pal et al. (2018) re-
ported the formation of spherical ZnO nanoparticles synthesized via
3.5. Hot plate combustion method co-precipitation route using Moringa Oleifera plant extract. Hexagonal
and triangular ZnO nanostructures were reported by Kahsay et al.
One of the rapid synthesis processes is the solution combustion (2019) through the colloidal synthesis process using Dolichos lablab L
process where the reactions mainly take place between an oxidizer such leaf extract (Fig. 5(a)) while hexagonal and spherical shaped ZnO
as metal nitrates and a fuel such as hydrazides, glycines, or urea. Based nanoparticles were identified by Demissie et al. (2020) using leaf ex-
on the precursors utilized, the combustion process may take place either tracts of Lappia adoensis synthesized by co-precipitation method (Fig. 5
by volume or by layer to layer propagation of modes, thereby resulting (b)). In both the studies, the precursor salt used was the same, hence the
in crystalline structure enhancing further impurity doping (Aruna and differences in the plant species and the synthesis route adopted have
Mukasyan, 2008). Synthesis of PPS such as NiO (Angel Ezhilarasi et al., resulted in the morphological changes of the synthesized nanoparticles.
2018a) and Fe3O4 (M. V. Arularasu et al., 2018) using Aeglemarmelos and Table 2 represents various PPS synthesized from plant species by
Kappaphycusalvarezii has been accomplished using this method. adopting respective synthesis routes. Depending upon the concentration
of biomolecules present, different parts (leaves, seed, stem, etc.) of the
plant can be used for the preparation of plant extract. Also, the dominant
3.6. Colloidal method biomolecule that aids in the NPs formation may vary with the plant
species selected.
This method is considered to be quite the easiest and cheaper one
compared to other synthesis routes and has been adopted for the syn-
4. Factors affecting PPS formation
thesis of most of the PPS. The process of synthesis is initiated by the
mixing up of plant metal salt with plant extract solution under
In the synthesis of PPS using plant extracts, the metal precursor so-
controlled temperature and pressure to form insoluble precipitates.
lution is mixed with plant extract and the rate of NPs formation is
Subsequent centrifugation of the colloidal precipitation results in the
controlled by different factors such as nature and concentration of
formation of metal NPs which are further dried to attain crystallinity
phytochemical used, the concentration of metal salt, pH, temperature,
(Hamidi et al., 2019). Colloidal routes of synthesis are categorized under
electrochemical potential and reaction time. These factors control the
liquid-phase synthesis in which the reactants taking part can be both
formation of NPs as well as their stability (Dwivedi and Gopal, 2010).
organic as well as inorganic and the biomolecules present in the plant
extract prevents aggregation of NPs by electrostatic precipitation (Papp
et al., 2012). Plant extracts such as Azadirachta Indica (Singh et al., 4.1. Concentration of plant extract
2019), Camelia SinensisG (Ahmed et al., 2019), Hibiscus Sabdariffa
(Alshehri et al., 2017), Abutilon Indicum (Abinaya et al., 2019a), and The concentration of plant extract has a significant influence on the
Withaniasomnifera (Alagesan and Venugopal, 2019) are reported to be shape and size of NPs. Optimization of phytochemical concentration is

Fig. 5. TEM images of ZnO nanoparticles synthesized from plant extracts (a) Hexagonal-triangular shaped ZnO nanostructures produced via the colloidal route
(Reproduced from Kahsay et al. (2019) with permission of The Royal Society of Chemistry) (b) Hexagonal-spherical shaped ZnO nanostructure via co-precipitation
method (Reproduced from Demissie et al., 2020) with permission of the publisher).

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

considered to be an essential step in the synthesis of NPs (Sheny et al., another study, they pointed out that in the synthesis of NPs, the con-
2011; Vijayaraghavan and Ashokkumar, 2017). Variations in the con- centration of plant extract and reaction temperature are related to each
centration of Aloe vera extract have changed the shape of synthesized other and reported that at lower reaction temperatures, more quantity of
gold NPs from triangular plates to spherical form (Shah et al., 2015). biomass extract is required for the synthesis (Kredy, 2018).
Furthermore, the selection of suitable plant parts having rich phyto-
chemicals and subsequent extraction processes have significant influ- 4.3. pH
ence over the quality of NPs formed (Narayanan and Sakthivel, 2010).
The proteins or peptides present in the plant extract control PPS for- Recent studies suggested that variation in pH could influence the
mation and biomolecules such as tryptophan and amino acids are re- charge transformations inside the plant metabolites and affect its ca-
ported as superior reducing agents (Narayanan and Sakthivel, 2010). pacity to chelate the metallic ions thereby resulting in the morphological
Moreover, polypeptides with mixtures of tryptophan molecules were changes of NPs (Shamaila et al., 2016). pH has a critical role in altering
found to be more efficient in the reduction process than with single electrical charges of the biomolecule, which affects its stabilization as
residues of tryptophan and due to entropic effects, peptides with diverse well as capping ability (Jain and Mehata, 2017). Hence pH optimization
amino acids are not sometimes recommended for NPs synthesis (Courrol should be necessarily carried out during the synthesis process. Peralta
et al., 2019). It is also suggested in many studies that the chances of et al. indicated that the pH of the solution is the primary factor to control
quick dissociation of peptide - metal ion bond may be encountered with the variation of particle size which affected the reduction of poly-
peptides, having amino acid chains that are poorly bound to tetra- dispersity of the gold NPs (Peralta-Videa et al., 2016; Shamaila et al.,
chloroauric acids (Suchomel et al., 2018). Hence alterations in the 2016). Larger-sized particles are obtained in an acidic medium while in
amino acid chains by any means may also affect the size and other basic media, resultant particles are comparatively smaller (Vadlapudi
characteristics of the NPs formed (Vijayaraghavan and Ashokkumar, and Kaladhar, 2014). Therefore, the basic condition is more recom-
2017). The morphology of NPs can be varied depending upon the plant mended in the synthesis process, which increases the surface to volume
extract. MgO NPs synthesized using cauliflower extract were reported to ratio of particles, consequently, higher stabilizing and capping proper-
show higher photodegradation of organic dyes than those prepared ties. Moreover, acidic conditions are not recommended for the synthesis
using pomegranate peels because of the size of NPs produced by cauli- of PPS because at lower pH NPs may aggregate to form larger-sized
flower extract was comparatively smaller than that of pomegranate particles. Therefore, alkaline conditions are preferred for NPs synthe-
peels (Winthachai, S.; Vaithanomsat, P.; Punsuvon, 2015). Hence during sis as it enhances homogeneous nucleation and thereby increases the
the synthesis, a plant extract that can produce NPs of smaller size is rate of metallic ion reduction (Zhan et al., 2011).
preferred because as the size decreases, the surface to volume ratio in-
creases which in turn results in better photocatalytic activity of the 4.4. Solvent used
synthesized PPS.
It has been reported that the antioxidant and catalytic properties of It has been highlighted in Montes et al. that, even the solvent used for
the NPs vary depending upon the amount of leaf mass used. Since the the preparation of extract determines the shape of the final NPs formed.
biomolecules present in the plant act as the main reducing agent which Triangular-shaped nanoplates were formed when water extracts of
mainly relies on the leaf mass, an increase in leaf mass increases the Medicago sativa are utilized while the shape has been notably changed to
concentration of these phytochemicals. If the selected plant extract decahedra and icosahedra with alcohol extract (Montes et al., 2011).
contains more phytochemicals, lesser the time required for the reduction
of metal ions, and if the phytochemicals are fewer, a long period is 4.5. Electrochemical potential
required, thereby increasing the stirring time (Balavandy et al., 2014).
Stirring time is considered as the time required for the NPs formation The electrochemical potential is also considered to be another
starting from the addition of reactant and defines the overall interaction important factor in determining the quality of PPS. Metal ions with
time of precursor salt and reducing components (biomolecules). higher ionizing potential could be reduced more effectively by phyto-
chemicals and hence Ag → ions having greater electrochemical potential
4.2. Temperature could be reduced quickly when compared to Au → ions (Haverkamp and
Marshall, 2009).
Some studies suggested that temperature change also affects the
formation of PPS because as the temperature increases beyond an op- 4.6. Concentration of metal salt
timum level, it causes the degradation of active amino acids and other
effective phytochemicals (Liu et al., 2020). A temperature range of The concentration of precursor salt determines the shape of NPs
50 ↗ C–100 ↗ C was reported for the preparation of iron NPs from Amar- formed and different morphological changes can be caused to the NPs as
anthus dubius leaf extract (Muthukumar Harshiny et al., 2015). An in- the concentration of metal salt varies. Also, if the concentration of salt is
crease in temperature improves NPs properties by the enhancement in too high, the reduction of metallic ions will not be effective. Hence there
the crystallinity as well as the nucleation of NPs (Cruz et al., 2010). is a need for optimizing this parameter too in the synthesis process
When compared to physical and chemical methods of synthesis, bio- (Gopinath et al., 2013).
logical synthesis requires less temperature, and literature reports that
the nature of the NPs formed is temperature-dependent (Rai et al., 4.7. Environmental conditions and other factors
2006). Certain NPs were also reported to be synthesized at particular
temperature ranges and change in the temperature may result in the Studies indicated the effect of the surrounding environment on the
alteration of shape and other characteristics of NPs (Bankar et al., 2010). properties of synthesized NPs. Ambient pressure condition is more
In the synthesis of Ag NPs using Cassia fistula plant extract, changes to preferable for the faster reduction of metal ions by the plant phyto-
the structural form of the NPs were observed with the temperature chemicals (Abhilash and Pandey, 2012; Tran et al., 2013). The NPs may
variation (Suresh et al., 2015). At ambient temperature, nanoribbons of also lose potential properties when stored for long or when the shelf life
Ag were noticed while at temperatures above 60 ↗ C, the formation of is over (Baer, 2011). Crystalline structures of zinc sulfide NPs were
spherical NPs was observed. The study concluded that at found to be altered notably when the surrounding environment changed
high-temperature nucleation rate increased. Nevertheless, the range of from wet conditions to dry (Kuchibhatla et al., 2012). Proximity effects
temperature may vary significantly depending upon the type of metal of other NPs such as particle charging or magnetic properties were also
ions as well as the method of synthesis adopted (Lin et al., 2010). In reported to alter the characteristics of NPs (Baer et al., 2008). PPS may

9
A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

exhibit different morphologies concerning the change in reaction time turbidity and reduces UV penetration, and results in decreased photo-
and stirring time. Stirring time is considered to be a function of several degradation processes. Prior research suggested that the optimization of
factors including the pH of the surrounding media, temperature, light the concentration of PPS is an important parameter to achieve maximum
intensity, reduction potential, and concentration of phytochemicals degradation potential (Sharma et al., 2020). Attempts to study the ki-
(Balavandy et al., 2014; Lade and Shanware, 2020). netics of photodegradation using PPS were also reported and most of the
kinetic study concluded with pseudo-first-order kinetics (Fatimah et al.,
5. Pollutant degradation mechanism of photocatalysts 2019). The chances of recombination of electron and hole pairs can be
reduced by stabilizing the NPs. In this aspect, PPS having plant bio-
PPS has been employed successfully for the degradation of organic molecules as the stabilizing agent reported being excellent in the sepa-
pollutants present in the wastewater. Most of the recent studies have ration of holes and electrons which causes effective photodegradation of
assessed the potential of PPS by conducting batch studies for the pho- hexavalent chromium (Abinaya et al., 2019b). Capping agents such as
todegradation of model pollutant dyes (Senthilkumar and Rajendran, saponins and tannins present in the C. lanceolata extract were found to
2018; Sharma et al., 2020; Zaheer, 2018). The degradation mechanism be the main factor behind the restriction in the recombination of elec-
of MB blue using cerium incorporated nickel ferrite (Ce0.2Ni0.8Fe2O4), a trons and holes that causes furtherance in reactive species formation and
green photocatalyst prepared using calotropis gigantean plant extract has improved photodegradation efficiency of ZnO NPs (J. Lu et al., 2019).
been reported by somanathan et al. (Somanathan et al., 2019). Similarly, Enhancement in the migration efficiency of electrons and holes has also
the suitability of PPS in the oxidation of textile dyes has been explored been achieved, when normal metal oxide form is replaced with iron
and proved to be an alternative to the conventional photocatalysts oxide NPs synthesized using K. alvarezii plant (M.V. Arularasu et al.,
(Arularasu et al., 2018). Many recent studies have elucidated mecha- 2018). Due to the supplement of Aegle marmelos leaf extract in the
nisms behind the degradation of organic dyes using PPS (Nagajyothi synthesis of NiO NPs, intrinsic and surface defects have been naturally
et al., 2019). When a suitable light source having energy sufficient produced without the addition of any impurities that make the synthe-
enough to overcome the bandgap energy (Eg) is incident on the catalyst sized NiO NPs efficacious in the photocatalytic activities (Angel Ezhi-
surface, the electrons (e-) on the valence band of the photocatalyst get larasi et al., 2018b). Stabilization of iron NPs by anthocyanin (a type of
excited to the conduction band, and at the same time holes (h→) are flavonoid biomolecule) present in Hibiscus sabdariffa plant extract assist
generated in the valence band. These electrons and holes act as the main in the immobilization of organic pollutants on the surface of the catalyst,
reducing and oxidizing agents, respectively, in photocatalytic reactions. which further advances the photocatalytic degradation of pollutants. It
Whenever the excited electrons in the conduction band drop back to the is reported that plant extract (panax species) can cause inherent
valence band, recombination occurs. The excited electrons react with morphological variations in the ZnO NPs structure which additionally
molecular oxygen to form superoxides and the hydroxyl radicals are provide more active sites for the reactive species interaction with
formed due to the reaction of generated holes with water molecules organic pollutants under U.V irradiation (Kaliraj et al., 2019). Photo-
(Arularasu et al., 2018). The light source and its fluence rate (exposure luminescence studies inferred that rapid recombination of electron and
rate) is an important factor that determines the effectiveness of photo- hole has been observed for bismuth oxychloride (BiOCl) photocatalyst
catalytic processes. Depending upon the capacity of the batch reactors synthesized without plant extract, whereas plant extract (Azadirachta
employed, the efficiency of the photodegradation process varies as the indica) incorporated BiOCl shows significant improvement in photo-
fluence rate with the capacity of the reactor. Hence optimization of current response, accelerate surface charge transfer, and inhibited
fluence rate is crucial, as the rate of production of ROS primarily de- recombination to some extent (Garg et al., 2018). Varieties of plants
pends on light (Bolton and Linden, 2003). Such reactive species gener- have been explored to date for the synthesis of different PPS with
ated during the photocatalytic process are capable of degrading organic remarkable photodegradation efficiencies (Stan et al., 2015).
pollutants present in water and wastewater and the degradation effi- Recent studies have revealed that PPS has been successfully applied
ciency directly depends upon these reactive species generated. The se- for the treatment of real wastewater contaminated with textile dyes and
ries of reactions that are taking place in the photocatalytic system of PPS other organic pollutants (Nagajyothi et al., 2019). PPS have been
are represented below (Shinde et al., 2018). deployed for the degradation of organic pollutants and Table 3 brings
out a comparison between different PPS and its degradation potential
PPS (oxide form) → hts e- CB → h→ VB (1) towards the targeted pollutants. Most of the researchers have evaluated
h →
VB → H2 O s H→ → OH ∙ (2) the efficacy of PPS by conducting degradation experiments (Abinaya
et al., 2019a; Cittrarasu et al., 2019; Das et al., 2018; Lu et al., 2019;
h→VB → OH - s OH∙ (3) Zaheer, 2018) in batch photoreactors where PPS is suspended in the
- ∙ system. Photoreactor configuration is considered to be a significant
e CB → O2 s O2 (4)
parameter for the improvement in the treatment efficiency and studies
O2 ∙ →
→ H s H 2O (5) have also focused on the enhancement of photodegradation with the
∙
variations of the light source (Ahmed et al., 2019; Das et al., 2018; Lu
Organic pollutants or dyes → OH → O∙2 s End products (6) et al., 2019). Goutam et al., (2018) evaluated the performance of TiO2
The applicability of PPS (TiO2 NPs using Jatropha curcas L.) in PPS synthesized from Jatropha curcas L. for the degradation of tannery
treating tannery wastewater has been demonstrated in a recent study wastewater operated at the continuous mode in a parabolic trough
and considered as one of the green approaches for the treatment of reactor. Obviously, in the treatment of real wastewater, there might be
tannery wastewater. This green synthesis is additionally attributed to the inhibitory effect of background compounds such as natural organic
the increase in the surface area of TiO2 NPs that enhances the adsorption matter (NOM). As these compounds can interfere the photodegradation
of hexavalent chromium (Goutam et al., 2018). The utilization of plant as well as act as a hindrance to light illumination and ROS production,
extract in the synthesis of photocatalyst reduces the optical band gap of such effects should also be taken into account while defining the efficacy
synthesized NPs which increases the excitation potential of electrons of PPS in treating real wastewater (Brame et al., 2015). Only limited
from the valence band (Stan et al., 2015). The specific surface area of studies have been extended the scope of PPS assessment in a continuous
PPS is reported to be higher than that of conventional NPs that account reactor and monitored a steady rate of photodegradation of real
for the increased catalyst and reactant interaction. Even though photo- wastewater treatment efficiency. Hence a notable gap has been identi-
catalytic degradation increases with the surface area of the catalyst, it fied and future studies have to give more attention to this aspect, to
should be well noted that a high concentration of PPS may increase increase the visibility of PPS in this domain.
Table 3 summarizes the application of PPS in the photodegradation

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

Table 3
PPS and their application in wastewater treatment.
Plant Species PPS Bandgap Light Sources Reactor Type Targeted Pollutants Removal References
(eV) efficiency

Parkiaspeciosa Ag Not Solar exposure Batch reactor MB 84% in 180 min Ravichandran et al.
mentioned (2019)
(NM)
Azadirachta Indica Ag NM Sunlight Batch reactor 4-nitrophenol and 100% within 120 Singh et al. (2019)
congo red dye min
Extract of apple and grape Ag 2.97; 2.83 Halogen lamp; 352 nm Batch reactor Phenol and congo- 95% and 98% Parthibavarman
red (CR) within 100 min et al. (2019)
Tribulus Terrestris L. Ag NM UV light; 434 nm Batch reactor MB NM Hamidi et al. (2019)
Camelia Japonica Ag NM Visible light irradiation Batch reactor Nitrobenzene and ω97% within 60 Karthik et al. (2017)
(tungsten lamp (500 W); Eosin – Y dye min
400–450 nm
Palm date fruit Ag NM Sunlight irradiation Batch reactor 4 –nitrophenol 95% within 8 min Zaheer (2018)
Barleria longiflora L. Ag NM Halogen lamp; 443 nm Batch reactor MB 93% within 45 Cittrarasu et al.
min (2019)
Solidagoaltissima Ag NM Irradiation of light Batch reactor RhB (Rhodamine B) Reduction in Kumar et al. (2016)
generated from the solar absorption peak
simulator
Averrhoa bilimbi and Au/TiO2 2.87 Sodium light Irradiation; Batch reactor MB 88 and 40.6% Yulizar et al. (2019)
Pandanus amaryllifolius 547 nm within 60 min
Madhuca longifolia CuO 2.31; 3.90 Visible light irradiation; Batch reactor MB 77% and 46% Das et al. (2018)
450 nm within 150 min
Camelia Sinensis Cu NM Sunlight irradiation Batch reactor Bromophenol dye 83.7% within Ahmed et al. (2019)
2160 min
Artabotryshexapetalus and CuO 2.5; 2.32 Halogen lamp; 554 nm Batch reactor RhB 91 and 96% within Haseena et al.
Bambusa Vulgaris 150 min (2019)
Eichhornia crassipes CuO/ NM A mercury lamp (8 W) Batch reactor Phenol 100% within 80 Lu et al. (2019)
TiO2 UV light and a Xeon and 120 min for
lamp for visible light; UV and visible
340 nm light
Calotropis Gigantean Ce/ NM A halogen lamp (150 W) Batch reactor MB 99.9% within 150 Somanathan et al.
NiFe2O4 was used for the visible min (2019)
light irradiation; ω420
nm
Bamboo Leaf Ash FeO 2.27 U V light; 296 nm Batch reactor RhB 57% within 60 Fatimah et al.
min (2019)
Kappaphycusalvarezii Fe3O4 2.8 High-pressure mercury Multi-lamp Hazardous textile 75% within 180 (Arularasu et al.,
lamp (300 W; photoreactor; Batch dye waste min 2018)
wavelength peak at 420 reactor
nm cutoff fleeter)
Hibiscus Sabdariffa Fe NM UV irradiation; 365 nm Batch reactor Congo red dye 96.1% within 70 Alshehri et al.
min (2017)
Amaranthusdubis Fe NM UV light of 20 W; 260 Batch reactor MO 81% within 120 (Harshiny et al.,
nm min 2015)
Abutilon Indicum MoO3 2.57 Irradiated under visible Batch reactor Hexavalent 99% within 30 Abinaya et al.
light; 483 nm chromium min (2019a)
Nepheliumlappaceum L. NiO 3.8 Medium pressure A Heber multi-lamp RhB 92.3% within 180 Adinaveen et al.
mercury vapor lamps; photoreactor; Batch min (2019b)
UV irradiation; 319 nm reactor
Aeglemarmelos NiO 3.58 UV light irradiation Batch photoreactor 4-chlorophenol 87% within 180 Angel Ezhilarasi
using a low-pressure min et al. (2018a)
mercury lamp; 365 nm
Parkiaspeciosa Hassk SnO2 4.3 UV254 irradiation; 254 Batch reactor Acid Yellow23 dye 98% within 24 Begum and
nm min Ahmaruzzaman
(2018)
Withaniasomnifera Se 2.75 Solar irradiation Batch reactor MB NM Alagesan and
Venugopal (2019)
Verbascumthapsus TiO2 3.48 250 W Mercury Lamp Cylindrical reactor Chromium 79.6% within 120 Esfahani et al.
further UV lamp; 365 nm Batch reactor min (2020)
JatrophacurcasL. TiO2 3.68 Solar Continuous Reactor Tannery 76.48% within Goutam et al.
wastewater 300 min (2018)
Justicia gendarussa TiO2 3.1 UV irradiation; 336 nm Batch reactor MB NM Senthilkumar and
Rajendran (2018)
Dolichos Lablab L. ZnO 3.4 Visible and near UV Batch reactor MB, RhB, and MB (80%), RhB Kahsay et al. (2019)
irradiation; 354 nm orange II dye (95%), and OII
(66%) within 210
min
Allium sativum, Allium ZnO 3.19; 3.21; UV lamp (30 W); 365 nm Batch reactor MB Reduction in Stan et al. (2015)
cepa, 3.12 absorption peak
Petroselinumcrispum
Cassia fistula ZnO 3.33 UV and sunlight; 370 nm Batch reactor MB 94% within 120 Suresh et al. (2015)
min
Terminalia chebula ZnO 3.22 30 W U V irradiation; Batch reactor RhB 70% within 300 Rana et al. (2016)
325 nm min
(continued on next page)

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A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

Table 3 (continued )
Plant Species PPS Bandgap Light Sources Reactor Type Targeted Pollutants Removal References
(eV) efficiency

Azadirachta indica ZnO 3.87 G30T8 UV lamp; Batch reactor MB 82.1% within 180 Bhuyan et al. (2015)
300–400 nm min
Citrus aurantifolia ZnO 3.21 400 W Osram UV lamp; Batch process Methyl orange Reduction in Davar et al. (2015)
325 nm (MO), MB, and absorption peak
methyl red (MR)
Moringa Oleifera ZnO NM Sunlight Batch reactor Titan yellow 96% within 60 Pal et al. (2018)
min
Aloe vera ZnO 3.4 UV light; 369 nm Batch reactor MO 95% within 160 Sharma et al. (2020)
min
Suaeda Japonica Makino ZnO NM UV light illumination Batch reactor MB 54% within 60 Shim et al. (2019)
(~346 nm) min
Stevia Rebaudiana ZnO NM UV light; 254 nm Batch reactor MB 76% within 30min Hoon Seo et al.
(2019)
Physalis alkekengi L. ZnO 4.18 UV light irradiation (30 Cylindrical Photo Bisphenol A 74.3% within 90 Cong et al. (2014)
W metal halide lamp) reactor (100 mL); min
Batch reactor
Codonopsis lanceoloata Cl-ZnO 3.3 UV light irradiation; Batch reactor MB 90.3% within 40 (J. Lu et al., 2019)
356 nm min
Ferulagoangulata ZnO and NM Visible light irradiation Batch reactor RhB 93% and 83% Shayegan Mehr
CuO using a fluorescent lamp; within 150 min et al. (2018)
ω400 nm
FicusBenghalensis ZrO2 4.9 UV light (365 nm) and a Batch reactor MB and MO 91 and 69% within Shinde et al. (2018)
High-pressure mercury 240 min
lamp (Philips HPL-N,
250 W)

of organic pollutants present in wastewater. Most of the studies focused Recently, many studies are focusing on the immobilization of the PPS on
on batch experiments with synthesized PPS and reported higher reduced graphene (Nasrollahzadeh et al., 2016) which enhances the
degradation efficiency. The bandgap corresponding to the synthesized reusability potential, and hence nanocomposite PPS are yet to be
NPs and light source used for the photodegradation were also indicated. explored more in this field.

6. Recyclability of PPS 7. Conclusions

The reusability of catalysts is an important factor to be considered for The present study focused on the review of synthesis routes, factors
practical applications, especially in continuous water and wastewater affecting and the mechanism of formation, and the photocatalytic ac-
treatment. The reusability of PPS determines the overall stability, tivity of PPS. From the review, it can be concluded that:
robustness as well as efficiency of the catalyst. Recyclability also defines
the economic aspects of the catalyst and the catalysts which are reused ↘ The main advantage of PPS is its dual role as reducing and stabilizing
or regenerated for the maximum number of times without losing their agents. Plant extracts play a significant role in PPS formation. Plant
catalytic properties are considered to be highly economically stable. extracts can control the charge carriers and thereby enhance pho-
Usually, the PPS reusability is examined by conducting different cyclic tocatalytic activity in addition to replacing other toxic and expensive
experiments and identifying the cycle corresponding to the decrease in chemicals used for the synthesis of nano photocatalyst.
degradation efficiency. Somanathan et al. reported that after the fifth ↘ Factors such as concentration of plant extract, temperature, pH,
cycle, degradation efficiency Ce0.2Ni0.8Fe2O4 nanoflakes (synthesized synthesis route adopted, concentration of metal salt, and electro-
using Calotropis gigantean extract) was reduced due to the blocking of the chemical potential affect the morphology and functional groups
active sites by the contaminant by-products, and further, the catalyst present in the catalyst. Hence, further studies are required to eluci-
was removed using an external magnet and then reused (Somanathan date the effect of secondary metabolites present in the plant extract
et al., 2019). that may control the morphological characteristics of the synthesized
Recyclability of green synthesized TiO2 has been reported in which PPS.
for every new cycle of experiment, TiO2 NPs were washed, boiled, ↘ Controlling the morphological characteristics is the main challenge
centrifuged, and oven-dried (100 ↗ C for 2 h). The regenerated TiO2 NPs in commercial production of PPS as the biomolecules present in plant
exhibited good repeatability with a percentage reduction of only 1.5% in extract undergo multiple redox reactions and may ultimately lead to
efficiency even after the use of five times (Esfahani et al., 2020). X-Ray the aggregation of the particles.
Diffraction and TEM analysis indicated that the crystalline structure, as ↘ Photocatalysis using PPS is a promising clean technology with po-
well as morphological characteristics of PPS, remains the same even tential applications in water and wastewater treatment. Most of the
after it has been repeatedly used for five cyclic experiments (Begum and studies related to PPS was conducted at laboratory scale because of
Ahmaruzzaman, 2018). Previous research found that molybdenum the lower catalyst production rate and limitations in its reusability
trioxide synthesized using Abutilon Indicum shows higher regenerative and immobilization. Considering this, future research should focus
capacity as its photodegradation potency remains constant up to three on scaling up the technology and on the treatment of real
cycles of use which is validated by conducting UV- Visible absorbance wastewater.
spectroscopy study (Abinaya et al., 2019b). The regeneration process of
PPS basically involves washing, centrifugation, and subsequent drying CRediT authorship contribution statement
which are considered to be uncomplicated compared to other photo-
catalyst regeneration methods. Most of the researchers concluded that Angel Joseph: Conceptualization, Data curation, Writing – original
PPS can be reused most effective up to five or six cycles without any draft. Arya Vijayanandan: Supervision, Writing – review & editing.
considerable reduction in photocatalytic activities (D. Lu et al., 2019).

12
A. Joseph and A. Vijayanandan Sustainable Chemistry and Pharmacy 22 (2021) 100453

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