Journal of Environmental Management 238 (2019) 25–40

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Journal of Environmental Management

journal homepage: www.elsevier.com/locate/jenvman

Review

Polymeric graphitic carbon nitride (g-C3N4)-based semiconducting T

nanostructured materials: Synthesis methods, properties and photocatalytic
applications
Kakarla Raghava Reddya,1, CH. Venkata Reddyb,1, Mallikarjuna N. Nadagoudac,
Nagaraj P. Shettid, Shim Jaesoolb,∗∗, Tejraj M. Aminabhavie,∗
a
School of Chemical and Biomolecular Engineering, The University of Sydney, Sydney, NSW 2006, Australia
b
School of Mechanical Engineering, Yeungnam University, Gyeongsan, 712-749, South Korea
c
Department of Mechanical and Materials Engineering, Wright State University, Dayton, OH 45324, United States
d
Department of Chemistry, K. L. E. Institute of Technology, Gokul, Hubballi, 580030, Affiliated to Visvesvaraya Technological University, Karnataka, India
e
Sonia College of Pharmacy, Dharwad, 580 002, Karnataka, India

ARTICLE INFO ABSTRACT

Keywords: In recent years, various facile and low-cost methods have been developed for the synthesis of advanced na-
Carbon nitride (C3N4) nostructured photocatalytic materials. These catalysts are required to mitigate the energy crisis, environmental
Heterogeneous hybrid nanostructures deterioration, including water and air pollution. Among the various semiconductors explored, recently novel
Photocatalysis classes of polymeric graphitic carbon nitride (g-C3N4)-based heterogeneous photocatalysts have established
Bandgap engineering
much greater importance because of their unique physiochemical properties, large surface area, low price, and
Hydrogen production
long service life, ease of synthesis, product scalability, controllable band gap properties, low toxicity, and high
CO2 reduction
Chemical transformation photocatalytic activity. The present comprehensive review focuses on recent achievements in a number of facile
Treatment of air and water pollution chemical synthesis methods for semiconducting polymeric carbon nitrides and their heterogeneous nanohybrids
with various dopants, nanostructured metals, metal oxides, and nanocarbons, as well as the parameters influ-
encing their physiochemical properties and photocatalytic efficiency, which are discussed with reference to
various catalytic applications such as air (NOx) purification, wastewater treatment, hydrogen generation, CO2
reduction, and chemical transformation. The mechanisms for the superior photocatalytic activity of polymeric g-
C3N4-based heterogeneous photocatalysts are also discussed. Finally, the challenges, prospects, and future di-
rections for photocatalytic polymeric g-C3N4-based semiconducting materials are described.

1. Introduction Therefore, novel technologies are important to overcome these severe

Human activities over the past century have resulted in increased
amount of carbon dioxide (CO2) in the atmosphere. According to the
International Panel on Climate Change (IPCC), it is predicted that CO2
levels in the atmosphere may increase to 590 ppm level by 2100, and
the worldwide average temperature might increase by 1.9 °C. These
changes may have calamitous effects (Zhang et al., 2018a; Corma and
Garcia, 2013), resulting in the development of green energy and
eco–friendly technologies because of the over-use of fossil fuels and
unrestrained harmful emission of CO2 from the burning of fossil fuels.
Adding to this, rapid urbanization and industrialization have resulted in
acute energy requirements due to environmental contamination.
problems. The use of solar power with the support of semiconducting
photocatalysts is one of such a technique (Ji et al., 2018) and semi-
conductor photocatalysts have shown enormous promise for improve-
ment in energy associated methods, green protection and carbon-based
production (Reddy et al., 2011, 2016; Dharupaneedi et al., 2019; He
et al., 2018a). The majority of available conventional photocatalysts are
expensive metals, metal oxides, or enzymes (Reddy et al., 2018; Kamat,
2012), but because of their lower catalytic activity, cost, and the risk of
serious environmental pollution, their practical applications are lim-
ited. Consequently, carbon-based photocatalysts have been progres-
sively used to substitute conventional photocatalytic materials or as
support matrices to increase the photocatalytic activity (Sabahi et al.,

∗
Corresponding author.
∗∗
Corresponding author.
E-mail addresses: jshim@ynu.ac.kr (S. Jaesool), aminabhavit@gmail.com (T.M. Aminabhavi).
1
Authors for an equal contribution.

https://doi.org/10.1016/j.jenvman.2019.02.075
Received 4 January 2019; Received in revised form 12 February 2019; Accepted 16 February 2019
Available online 04 March 2019
0301-4797/ © 2019 Elsevier Ltd. All rights reserved.
K.R. Reddy, et al.
2018; Reddy et al., 2014, 2015; Anjum et al., 2018a, 2018b). Because of
its enormous specific surface area, excellent thermal conductivity, and
electron transport characteristics (Novoselov et al., 2004; Gopinath
et al., 1016), graphene is considered as one of the excellent materials
for developing new catalysts (Ong et al., 2015; Feng et al., 2018), but its
catalytic activity is weak. Therefore, it is necessary to find ways to in-
crease the activity for its catalytic applications, for example, hy-
bridization of graphene with other carbonaceous materials.
The development of inexpensive photocatalysts with a high activity
is vital for practical applications of photocatalytic reduction of CO2
(Maeda et al., 2013). Compared to metal oxide photocatalysts, non-
metallic semiconducting materials exhibit similar efficiencies because
of their low material costs and a similar range of light absorption.
Polymeric graphitic carbon nitride (g-C3N4) is a metal-free and in-
tensively studied visible-light-driven photocatalytic material and was
extensively studied for synthetic photosynthesis and environmental
remediation, such as wastewater treatment and air purification. The g-
C3N4 is a polymeric layered catalytic material having a similar structure
to that of graphene.
Graphene is composed of pure carbon (C), but g-C3N4 contains C
and nitrogen (N). Fig. 1 displays the polymerized chemical structure of
g-C3N4 (Zhang et al., 2012a). The benefits of g-C3N4 for CO2 photo-
catalytic reduction over other materials include (i) its low cost and (ii)
good CO2 activation properties arising from its nitrogen–rich structure
(Huang et al., 2013); (iii) for photocatalytic CO2 reduction, its band
structure is suitable for the formation of several value-added mixtures,
(iv) it can transfer electron to the surface chemical adsorption sites due
to its 2D layered structure; (v) g-C3N4 structure can be tuned by varying
the precursors and polymerization conditions; thus, a slight band off set
can be achieved (Cao et al., 2015). Moreover, by simply adding ad-
ditives of preferred monomer molecules to precursors, comonomers can
be prepared (Zhang et al., 2012b), and these can significantly modify
the light absorption capability and electron transfer abilities of g-C3N4
in H2 production, the degradation of organic compounds (e.g. dyes),
and oxidation of nitrogen oxides (NO) that can be enhanced by metal
doping (Li et al., 2016a; Guo et al., 2016; Kumar et al., 2019).
The semiconducting properties of g-C3N4 are considerably different
from those of graphene sheets. The band-gap of bulk g-C3N4 is ca.
2.7 eV, and is a mediocre band gap semiconducting material. Due to its
yellow color, g-C3N4 an optical absorption peak at about 460 nm. It is a
remarkable material for harvesting solar energy and because of its ex-
traordinary thermal and chemical stability, it is an interesting material
for photocatalytic reactions (Li et al., 2018). Moreover, g-C3N4, also
known as “melon”, is a stable allotrope among the various carbon ni-
tride-based materials. Thus, of all the non-metal semiconducting ma-
terials, g-C3N4 is a very favorable photocatalyst because of its low cost,
Fig. 1. Schematic representation of the proposed structure of polymerized
graphitic C3N4 (blue: carbon atom; gray: nitrogen atom) Reproduced from Ref
(Zhang et al., 2012a). with permission from Wiley.
26
Journal of Environmental Management 238 (2019) 25–40
ease of synthesis, comparatively better stability, suitable electronic
structure, and outstanding photocatalytic performance. Furthermore, g-
C3N4 is collected from two earth ample components (carbon and ni-
trogen) and hence, it is material inexpensive and economical for large-
scale applications in photocatalytic solar water splitting and energy
conversion (Zhou et al., 2016). Due to its rich hydrogen absorption
locations, and tunable band structure, graphitic carbon nitride has been
effectively used in photocatalytic hydrogen evolution reaction, but its
electrical resistance controlled its electrocatalytic activity (Zhong et al.,
2018). Until now g-C3N4 has been mostly used in powder form, which
obstructs its repeated use for some applications. Hence, the controlled
accessible association of 2D building blocks into macroscopic 3D
structural designs are extremely important for numerous applications
(He et al., 2018b).
In search of artificial photosynthesis using CO2 by-product of energy
fuels, the discovery of cost–effective and efficient photocatalytic sys-
tems based on g-C3N4 merits consideration. However, photocatalytic
CO2 conversion studies based on g-C3N4 materials are somewhat rare
compared to those of inorganic metal oxides, and therefore, studies on
the reduction of CO2using g-C3N4 based-materials as photocatalytic
materials are significantly less (Shown et al., 2018; Raziq et al., 2018;
Huang et al., 2015; Tonda et al., 2018).
Fig. 2 shows a schematic representation of the photocatalytic con-
version of CO2 to various possible products. Photocatalytic CO2 re-
duction principally involves one or more of the following five path-
ways:(i) CO2 adsorption and reduction, (ii) creation of electrons and
holes in the conduction band (CB) and the valence band (VB) of the
semiconducting material, (iii) photogenerated charge carrier separation
and transmission to the surface of the catalyst, (iv) adsorption of surface
species and reaction with electrons/holes, and (iv) products desorption
and reactant re-adsorption. However, conversion capacity for the gen-
eration of hydro-carbon gasses via CO2 reduction with H2O has not
been well studied because the reaction requires a high energy input
(ΔGfo = −394.39 kJmol-1) due to the high stability of the reactants
(Jiang et al., 2018).
The present comprehensive review deals with recent developments
in the various synthesis methodologies of various g-C3N4-based na-
nostructured hybrid photocatalysts, their physicochemical properties,
band-gap characteristics, influencing parameters to enhance catalytic
efficiency, catalytic mechanism and different photocatalytic applica-
tions, such as photocatalytic degradation of toxic environmental pol-
lutants, H2 generation, air purification, CO2 reduction, and chemical
transformations. In order to understand the characteristic features of g-
C3N4-based nanohybrids for the different photocatalytic applications
comprehensively, the physiochemical properties, and property-appli-
cation relationships of g-C3N4 are discussed in greater details. The fu-
ture perspectives towards its large scale photocatalytic applications are
Fig. 2. Schematic representation of five key pathways in the photocatalytic
conversion of CO2 to different products.
K.R. Reddy, et al.
also discussed.
2. Synthesis methodologies for polymeric g-C3N4 photocatalysts
Various meso- and microporous structured materials (e.g., cera-
mics), activated porous carbons, fly ash, carbon materials (e.g. gra-
phene, reduced graphene oxide (rGO), carbon nanotubes (CNTs)),
zeolites and polymers have been used as supporting modifiers for the
dispersion of catalysts because of their large specific surface areas,
porous structures, and excellent stability to chemicals and temperature
(He et al., 2018c; Zhu et al., 2017; Ma et al., 2017a; Wang et al., 2017a;
Zhao et al., 2017a; Rostami, 2017; Hamdy, 2017; Hipolito et al., 2017;
Su et al., 2017). Among them, polymeric photocatalysts, such as poly-
meric carbon nitrides and polymer-functionalized semiconducting ma-
terials have received much greater attention because they are in-
expensive, easy to fabricate on a large scale that is resistant to
corrosion, stable at high temperatures and the aggressive environment
(Wang et al., 2017b; Zhou et al., 2017a; Ji et al., 2107; Shaikh et al.,
2017; Zhou et al., 2018; Zhang et al., 2018b). Because some of these
functionalized hybrid photocatalysts have ultra-porous structures, they
can adsorb not only the pollutants in the air, but also heavy metal ions
(e.g. Hg, Cd, As) in contaminated wastewater.
The g-C3N4 catalysts are generally synthesized from thermal poly-
merization of small organic compounds, such as cyanimide, melamine,
urea, or Dicyanamide (as shown in Scheme 1). Polymerization produces
g-C3N4 with a low surface area and low photocatalytic performance for
hydrogen production because of the high rate of charge recombination.
Therefore, various approaches have been employed to modify the sur-
faces to enhance photocatalytic efficiency for hydrogen generation as
well as to increase the surface area of the catalyst.
The photoactivity of the polymeric carbon nitride has been reported
with respect to both rate criteria (moles of hydrogen produced per hour
and the determined quantum-efficiency). In general, polymeric carbon
nitride semiconducting catalysts are composed of two chemical units in
the backbone, such as triazine or tri-s-triazine rings (heptazine).
Heptazine-based polymeric nitride catalysts are prepared from the
straight high-temperature polymerization of their precursors. Apart
from having four structural models, polymeric C3N4 also contains a
condensed poly(tri-s-triazine imide) structure, as evident from the high-
resolution electronic microscopic images.
2.1. Polymeric g-C3N4–based hybrid photocatalysts for wastewater
treatment
Ibad et al. (2017), described the fabrication of porous polymeric
graphitic carbon nitrides by a combination of soft-template sol-
vothermal process and a post-thermal method starting from low tem-
peratures at a low heating rate, as shown in Fig. 3. In this process,
melamine and an amphiphilic block copolymer were dissolved in an
aqueous H2SO4 solution to form a white precipitate that was allowed to
Scheme 1. Schematic synthesis representation of g-C3N4 using different che-
micals.
27
Journal of Environmental Management 238 (2019) 25–40
Fig. 3. Reaction route for the fabrication of g-C3N4with mesoporous structures.
Reproduced from Ref (Ibad et al., 2017). with permission from Elsevier.
polymerize and condense under argon gas flow at 380 °C and then at
600 °C in a quartz tube. A soft yellow solid mesoporous polymeric
carbon nitride photocatalyst was obtained after pyrolysis for 3 h at
different temperatures in the muffle furnace. Further, it was in-
vestigated for its ability to photodegrade the anti-inflammatory drug
ibuprofen (IBP) in solution under visible white light produced by a 16-
W cold white light emitting diode (LED) lamp. It was found that pho-
todegradation of ibuprofen proceeds via three steps: (i) hydroxylation
of ibuprofen molecules, (ii) aromatic ring opening by insertion of
oxygen molecules, and (iii) oxidative decarboxylation of obtained in-
termediates such as carbonic acids.
Xue et al. (2015), investigated the preparation of an Au-modified
polymeric graphitic carbon nitride/graphene layered ternary plasmonic
composite photocatalyst (Au/g-C3N4@GR) by the ultrasonic photo-de-
position method. In this method, porous polymeric carbon nitride was
initially prepared by straight high-temperature thermal polymerization
of inexpensive urea in a muffle furnace at 550 °C for 3 h. During the
heating reaction, gas bubbles created acted as soft-templates to gen-
erate pores with a size of 24 nm in the yellow-colored graphitic carbon
nitride. Then, it was modified with graphene through electrostatic in-
teractions by the sonochemical method in the presence of ammonia
solution. In this ternary structured catalyst, porous g-C3N4 was coated
onto the surface of 3D graphene nanosheets, as explained for the for-
mation of a layered photocatalyst containing small gold nanoparticles
(Au NPs) with a diameter of 10–15 nm, which were homogeneously
distributed on the surface of the layered g-C3N4/GR structure via
photodeposition method. Then, the solution was photo-irradiated for
2 h with a 250-W mercury arc lamp (λ = 365 nm), and finally the
ternary photocatalyst was tested for the photo-degradation of model
pollutants, an organic dye (methylene blue (MB)) and antibiotic ma-
terial (ciprofloxacin (CIP)) under visible-light illumination produced by
a 500-W xenon lamp (Philips) with a porous cut-off screen at 420 nm.
The concentrations of MB and CIP pollutants were measured by the
intensities of the absorption peaks of 663 nm (λMB) and 272 nm (λCIP).
It was found that photodegradation kinetic of MB and CIP over this
ternary catalyst were 4.3 and 3 times greater, respectively than that of
the porous polymeric g-C3N4 semiconductor, and even 7.4 and 6.1
times greater, respectively related to pristine g-C3N4 photocatalyst. This
is because of the surface modification with gold and electron-acceptor
character of 3D graphene sheet, which enhances the absorption of
visible light, creation of active reactive sites on their surface, separation
of photoinitiated charge carriers, and synergistic effect between them,
contributing to the improvement of photocatalytic activity of the
ternary catalyst (Fig. 4).
A novel photocatalytic material, a photonic-crystal-supported cata-
lyst was synthesized on a large scale by encapsulating mesoporous g-
C3N4 nanorods (5 mg) on the surface of strong, narrow reflective nano-
silica/trimethylopropane ethoxylate triacrylate (ETPTA) film
(dia = 9 cm) fabricated by spin coating method (Pang et al., 2015).
Functionalizing the polymeric carbon nitride with the crystalline pho-
tonic crystals resulted in a photonic-crystal-based photocatalyst with a
tunable bandgap and yielded a reusable material with a long photo-
catalytic life as well as easier separation compared to dispersed
K.R. Reddy, et al.
Fig. 4. Schematic representation of the photocatalytic mechanism of a ternary
structured polymeric g-C3N4/Au@GR photocatalyst in the presence of visible-
light. Reproduced from Ref (Xue et al., 2015). with permission from RSC.
photocatalysts. This catalyst was used for both the degradation of or-
ganic pollutants and photocatalytic water splitting. The introduction of
photonic crystals as the supporting material enhanced the photo-
catalytic efficiency, and the addition of photonic material resulted in
stronger reflections, giving better catalytic performance for the photo-
degradation of rhodamine B (RhB); for example, the intensity of re-
flections increased from 13%,48%–93% and rate constants increased
from 0.0368,0.0424, to 0.0481 min−1, respectively all of which were
much higher than the rate constant (0.0274 min−1) of mesostructured
polymeric carbon nitride nanorods immobilized on the surface of pure
ETPTA films without a silica colloid because the simulated solar light
irradiates and passes through mesoporous structured polymeric gra-
phitic nitride. Thus, there is no reflected light other than that being
absorbed by the photocatalytic material. The well-dispersed mesos-
tructured rod-like polymeric carbon nitride photocatalyst degraded the
rhodamine dye up to 97.9% upon irradiation with the visible light.
Li et al. (2016b) synthesized new photocatalyst by exfoliating mo-
lecularly grafted polymeric carbon nitride to ultrathin nanosheets, fol-
lowed by self-assembly on the surface of NaYF4:Yb, Tm up-conversion
phosphor (UCP) micro-rods. In this method, the catalyst was prepared
in two steps as shown in Fig. 5: (i) copolymerization of graphitic carbon
nitride precursor with a monomer molecules of 2-aminobenzonitrile,
followed by an exfoliation to achieve 2D structures to reduce the
bandgap (bathochromic change to visible-light region) and (ii) the
coupling of doped carbon nitride nanosheets with the electron ac-
cepting UCPs, which convert the near IR (NIR) light to visible light via
anti-stokes photoluminescence, leading to efficient visible-NIR photo-
catalysts. This new catalyst allowed complete utilization of visible-NIR
light source to show much greater catalytic performance than the
previously reported carbon nitrides or CP-based photocatalytic mate-
rials. The authors further studied this catalyst for photocatalytic de-
gradation of rhodamine B dye at 554 nm and found that dye degrada-
tion rate at 980 nm light was about 1.5 times higher than that by the Er
(III)-doped polymeric carbon nitride under red light irradiation. Fur-
thermore, photodegradation experiments were performed under full
range (visible-NIR light from a xenon lamp with the cut-off wavelength
of 400 nm) illumination and the hybrid catalysts have exhibited higher
28
Journal of Environmental Management 238 (2019) 25–40
Fig. 5. Fabrication of UCP/polymeric carbon nitride hybrid photocatalyst and
catalytic mechanism upon solar light. Reproduced from Ref (Li et al., 2016b).
with permission from RSC.
catalytic performance than the UCP/TiO2 hybrid catalysts. This may be
due to the holes (h+) present in the catalyst, which would oxidize the
dye molecules directly, and the electrons (e−) are trapped by the ad-
sorbed oxygen molecules to generate superoxide radicals.
Kumar et al. (2014) prepared the novel and stable hybrid photo-
catalyst by wrapping nitrogen-doped SrTiO3 nanoparticles into the
layers of polymeric carbon nitride nanosheets using a simple and re-
peatable polymer citrate and high-temperature exfoliation process at
500 °C for 2 h, The NeSrTiO3/g-C3N4 hybrid catalyst had an absorption
edge at higher wavelength compared to that of pristine carbon nitride
polymer, as well pure N-doped SrTiO3 catalysts. Under visible-light il-
lumination, these hybrid catalysts exhibited enhanced electrochemical
response of photocurrent, photocatalytic performance, photo-stability,
and recyclability of 0.05 g of catalyst for photodegradation of rhoda-
mine B organic dye and 4-chlorophenol under-visible light irradiation
with a solar simulator (300- W Xe lamp, wavelength range of
400–700 nm, and light intensity of 115 mWcm−2). Degradation oc-
curred because at the boundary of polymeric carbon nitride and
NeSrTiO3heterojunctions, high migration, and the separation of charge
carriers was possible (Fig. 6). The authors also conducted photo-stabi-
lity and recyclability tests on the hybrid catalyst for five successive
experimental cycles to find that 90% of the photocatalytic efficiency
was retained, demonstrating the potential of catalyst for environmental
remediation, particularly in pollutant degradation under the sunlight as
well as effective photocatalytic water spitting for the evolution of hy-
drogen.
A novel photocatalyst was developed by coating uniform carbon
spheres onto the surface of layeredpolymeric metal-free carbon nitride
via two steps:(i) thermal polycondensation of melamine to carbon ni-
tride by heating the melamine in a loosely covered crucible at 500 °C at
the heating rate of 15°Cmin-1, and (ii) hydrothermal carbonization of D-
glucose with carbon nitride in an oven at 135–180 °C for 3 h (Sun et al.,
2014). The coating of carbon spheres onto carbon nitride polymer
surface remarkably enhanced photo-oxidation ability (4.79 times
higher than that of pure carbon nitride) for photodegradation of phenol
under artificial sunlight irradiation using 575-W metal halide lamp with
the visible light intensity (λ > 420 nm) of 129 mWcm−2. The authors
also tested the catalyst stability by conducting the photocatalytic
measurements for three runs and the activity remained constant, de-
monstrating that this hybrid photocatalyst is stable for the photo-
degradation of chemical pollutants under solar light irradiation.
Zhao et al. (2016a) synthesized of three copper (II) coordination
polymers by hydrothermal reaction and utilized them as high-perfor-
mance photocatalysts for the photodegradation of methyl orange (MO)
dye under UV-light. The degradation of MO reached 91.75% in
140 min. From the catalytic recycling tests, the authors noted that the
photocatalysts could be recovered from the reactive catalytic system
K.R. Reddy, et al.
Fig. 6. Schematic representation of the photocatalytic mechanism of polymeric
carbon nitride/nitrogen-doped SrTiO3nanohybrid catalyst for the photo-
degradation of (synthetic dyes) under visible-light illumination. Reproduced
from Ref (Kumar et al., 2014). with permission from RSC. Want et al. (Wang
et al., 2014), prepared visible-light driven polymeric g-C3N4/SiO2 photocatalyst
by heating a mixture of melamine and silica (surface area, 289 m2g-1) at 520 °C
for 4 h in a muffle furnace. The hybrid catalyst showed enhanced surface area
and reduced aggregation of carbon nitride, leading to improvements in catalytic
efficiency for the photodegradation of rhodamine B in the presence of visible
light with a Xe lamp (excitation at λ of 365 nm) as the light source. It was found
that 14.3 wt% SiO2/g-C3N4 hybrid catalysts could completely degrade the dye
in 80 min. The photodegradation rate of hybrid catalyst was 0.051/min, which
is 2.3 times higher than that of the nascent g-C3N4.
and may be reused for five catalytic cycles. On the other hand, the 2D
graphitic carbon nitride photocatalyst was prepared by the self-as-
sembly method (Xia et al., 2017), and these results that provide a very
high specific surface area along with porosity as well as more catalytic
active sites, resulting in increased photocatalytic efficiency of this
photocatalyst for the reduction of CO2. Furthermore, this catalyst has
shown excellent stability for CO2 reduction and thus, has the potential
for other photocatalytic applications, such as the treatment of waste-
water and hydrogen evolution.
2.2. Polymeric g-C3N4–based nanohybrid photocatalysts in air pollution
treatment
The quality of indoor air has received a much greater attention in
recent years because the indoor environment plays a key role in
maintaining the human health and hygiene. Some air pollutants such as
nitrogen oxides (NO2, NO), sulfur oxides (SO2, SO3), exhaust gases,
traffic pollutants, carbon monoxides (CO), and other volatile organic
compounds that come from combustion, cooking, smoking, and con-
struction materials can cause serious health hazards including sore
throat, headache, drowsiness, mental illness. Therefore, it is necessary
to develop technologies to remove indoor and outdoor air pollutants
completely. Traditional methods to reduce indoor air pollution involve
the use of air purifiers, which increase air exchange or regulation of the
pollutant source. These methods have drawbacks because the source
control is challenging and increased air exchange may distribute more
pollutants. Thus, normal air purifiers contain sorption materials to
adsorb chemical gases or odors, but this may only transfer the pollu-
tants to another location instead of completely removing or degrading
them. Consequently, additional equipment and further steps are re-
quired. As a result, heterostructured photocatalytic oxidation (PCO)
method has been proposed as an alternative air purification method,
and PCO has been extensively studied that was efficient for the
29
Journal of Environmental Management 238 (2019) 25–40
purification of indoor and outdoor air.
Semiconducting metal oxide photocatalysts such as polymeric gra-
phitic carbon nitrides, TiO2, WO3, ZrO2, and ZnO are frequently used in
PCO process. Among them graphitic-carbon-nitrides-based semi-
conducting photocatalysts have been extensively studied. The g-C3N4
contains tris-triazine units associated with the planar amino groups in
each layer, as well as the weak van-der-Waals forces between the layers.
This material has attracted significant attention. Furthermore, the
fabrication of polymeric semiconducting g-C3N4 based hybrids is well
established to yield the visible-light-driven catalysts because of the
improved visible light absorption and effective transfer of photo-in-
duced charges (Sun et al., 2015). Ho et al. (2015) developed a novel
photocatalyst by replacing single nitrogen atom with a carbon atom in
the triazine ring of the polymeric graphitic carbon nitride through co-
polymerization of melamine (MA) with 2,4,6-triaminopyrimidine (TAP)
in a covered crucible at 550 °C for 4 h, leading to the encapsulation of
C4N2 ring from the TAP into the network structure of g-C3N4 catalyst.
In the above process, g-C3N4 nanosheets roll-up into tubular struc-
tures, leading to a reduction in bandgap energy (Eg = hc/λ) from 2.7 to
2.4 eV through the shifting of valence band of g-C3N4, as well as im-
proving photocatalytic efficiency to remove 600 ppb NO gas with 0.1 g
of the photocatalyst under 30-W visible LED irradiation (Fig. 7). Such as
improvement in the catalytic efficiency is due enhanced migration of
the charge-carriers and their separation as well as decrease inπ-defi-
ciencies and creation of inconsistent electron density in the π-electron
conjugated units of the polymeric carbon nitride backbone due to the
encapsulation of TAP. It was found that the amount of NO gas was
reduced rapidly from 605 to 362 ppb over the pure polymeric carbon
nitride upon visible LED irradiation. However, the concentration of NO
gas was further decreased to 245 ppb when 1% TAP was introduced in
the catalytic reaction system, indicating that NO was removed up to
59.4% when 1% TAP was incorporated into polymeric carbon nitride.
Dong et al. (2014) described the synthesis of mesoporous polymeric
g-C3N4 by thermal polycondensation polymerization using high surface
area silica and nanosilica particles hard-templates. The resulting porous
carbon nitride polymers have surface areas of 105–112 m2g-1 and me-
sopores of 9.3 nm dia with a narrow size distribution. Such mesoporous
catalysts have been studied for the removal of NO gas in air under
visible light illumination, and the results have shown that these have
the catalytic performance superior to that of the bulk carbon nitride and
non-metals (carbon and nitrogen)-doped TiO2. Such a superior perfor-
mance is due to the synergistic properties arising from the porosity,
large surface area, enhancement in light absorption, redox potential,
and reduction in charge carrier recombination. Authors also found that
there was no loss of catalyst performance even after six cycles of NO gas
removal under the visible light irradiation. Thus, this catalyst provided
enhanced catalytic efficiency for the removal of environmental pollu-
tants.
Another new visible-light-active photocatalyst with a nanos-
tructured polymeric carbon nitride structure was developed by direct
Fig. 7. Schematics showing the conversion of polymeric carbon nitride na-
nosheets into 1D tubular structure and its catalytic mechanism for the removal
of NO gas. Reproduced from Ref (Ho et al., 2015). with permission from ACS.
K.R. Reddy, et al.
pyrolysis of urea in a covered alumina crucible at 550 °C for different
pyrolysis time (Don et al., 2013). With increasing pyrolysis time, the
crystalline nature of carbon nitride increased, while the size and
thickness of layers decreased. In addition, pore volume and the surface
area were notably improved, but the bandgap values have shifted. The
as-synthesized yellow-colored polymeric semiconducting photocatalyst
was tested for photocatalytic removal of NO gas from air and rhoda-
mine B under visible light irradiation with a 150-W tungsten halogen
lamp (λ > 420 nm). The pyrolysis time was increased from 0 to
240 min, and NO gas removal increased from 26% for carbon nitride
(pyrolysis time is zero) to 32.1% for carbon nitride prepared at pyr-
olysis time of 240 min, after irradiating the catalyst for 45 min. The
latter photocatalyst degraded 100% of rhodamine dye after 300 min
irradiation. Other researchers have reported similar results that the
carbon nitride polymers and other inorganic photocatalysts have sui-
table bandgaps of 2.68–2.78 eV, indicating that excitation by visible-
light irradiation and removal of NO gas in air is due to catalytic reaction
between NO and photo-initiated radicals, where the final product is
HNO3 after the oxidation of intermediate NO2 gas (Dong et al., 2011b,
2014).
Recently, novel visible-light-active polymeric carbon nitride pho-
tocatalysts were developed and used for the removal of NO using pre-
cursors-rich in C and N, such as dicyandiamine, urea, melamine and
thiourea at the pyrolysis temperature maintained between 450 and
600 °C for 4 h at the heating rate of 15 °C/min (Lu et al., 2017). Poly-
meric g-C3N4 prepared from dicyandiamide and melamine showed
higher yield, while photocatalytic properties of graphitic carbon nitride
fabricated from dicyandiamide alone was greatly enhanced for re-
moving NO. Higher catalytic activity to remove NO gas under the
visible-light illumination is due to different band-gap values of gra-
phitic nitride and melem, which drives photo-initiated electron-hole
separation due to bandgap offset.
The effect of pyrolysis temperature on NO removal efficiency of
polymeric graphitic nitride was also investigated and carbon nitride
catalyst prepared at 500 °C showed the most stable NO removal effi-
ciency, reaching up to 28% after 30-min of irradiation by converting
NO gas into NO3. The carbon nitride CB and VB potentials of (T450) are
−0.71 and 2.05 eV, while the conduction band and valence band po-
tentials of carbon nitride prepared at 600 °C are −0.65 and 1.85 eV,
respectively. Because of the difference in conduction band potential,
photo-initiated electron transfer has occurred from the carbon nitride
(T450) to melem, and holes were transferred from melem to graphitic
carbon nitride. Therefore, it appears that the number of holes and
electrons play a key role towards the efficiency of catalyst for removing
NO. Six successive experimental runs for the photodegradation of NO
gas over carbon nitride (T500) were performed using visible light, which
showed that NO removal ratio was maintained at an increasing trend
even after six cycles, reaching the maximum of 28%, which remained
the same as the value for 1st cycle (Fig. 8). This demonstrates the ex-
cellent photochemical stability of the catalyst systems for air purifica-
tion.
Lu et al. (2018) evaluated the NO gas removal rate using polymeric
g-C3N4 under different light sources such as metal halide lamp, LED
lamp, and high-pressure sodium lamp. The temperature was adjusted
from 450 to 600 °C to obtain high efficiency and photocatalytic per-
formance. Under the irradiation of a metal halide lamp, the g-C3N4
synthesized at 500 °C exhibited greater NO removal ratio (29.3%)
compared to other light sources. This enhancement was due to the
conduction band potential difference between g-C3N4 and melem, re-
sulting in the heterojunction formation between melem and g-C3N4,
which has significantly decreased the combination ratio of photoexcited
electrons and holes and hence, increase of photocatalytic properties of
g-C3N4. Furthermore, compared with other lamps, the metal halide
lamp light intensity was the most appropriate light source to drive the
g-C3N4 reaction.
In order to attain photocatalytic air purification using surface
30
Journal of Environmental Management 238 (2019) 25–40
Fig. 8. Photocatalytic reusability tests for the removal of NO gas (concentration
of 100 ppb) using polymeric carbon nitride prepared at 500 °C. Reproduced
from Ref (Lu et al., 2017). with permission from Elsevier.
Plasmon resonance (SPR) an effect, Dong et al. (2015) reported semi
metal−organic Bi spheres−gC3N4 nanohybrid prepared by in-situ
growth of Bi nanoparticles onto the surface of g-C3N4 nanosheets.
Owing to SPR effect provided by Bi particles, the synthesized Bi−g-
C3N4 nanohybrid showed an outstanding and highly stable visible-light
photocatalytic activity for NO removal compared to that of pristine g-
C3N4 catalyst. The SPR properties of Bi noticeably improved the visible-
light absorption capacity and photo-exited charge separation.
2.3. Polymeric g-C3N4–hybrid photocatalysts for hydrogen evolution
Hydrogen is one of best source of energy due to its excellent energy
density (141 MJKg−1) that is three times higher than gasoline.
Photocatalytic water splitting for hydrogen production is becoming
increasingly attractive as the demand for solar energy production in-
creases (Turner, 2004). For hydrogen production, various photo-
catalytic materials have been widely used such as ceramic powders,
semiconducting materials, noble metals (Pt and Pd), metal-free carbon
nitride, and polymeric graphitic carbon nitride (Sadanandam et al.,
2017; Dozzi et al., 2017; Herranz et al., 2018; Zhang et al., 2017).
Carbon nitride consists of carbon, nitrogen and oxygen and exhibits
excellent catalytic efficiency for hydrogen evolution from the aqueous
system. Among the various photocatalysts, the polymeric semi-
conductor g-C3N4 has an eco-friendly chemical composition and ease of
fabrication making it a promising catalyst for hydrogen production.
However, its photocatalytic efficiency is narrowed by the lack of re-
sponse in the longer wavelength region, and the high recombination of
electron-hole pairs.
The structure of g-C3N4 consists of 2D layers that are inter-con-
nected via H-bonds and the layers are linked via van der Waals forces,
thus forming a 3D structure. Wu et al. (2018) reported the preparation
of polymeric carbon nitride by polymerizing melem molecules along
with the loss of ammonia gas (Fig. 9). This structure showed excellent
electronic properties with a low bandgap (2.7 eV), which enables the
capture of some solar irradiation and evolution of hydrogen and oxygen
from water through photocatalytic splitting. The authors fabricated a g-
CN network structure with its layers encapsulated with melem oligo-
mers for photocatalytic hydrogen production with high rate from trie-
thanolamine aqueous solution under visible-light illumination (300-W
xenon lamp with a cutoff wavelength of light of 420–800 nm). Ther-
mally condensed urea was used to produce g-CN 3D sheets that an-
nealed in argon to form structure-distorted CN (Fig. 10). The N-CNs has
active amino sites on their surface, and exhibit hydrogen evolution
K.R. Reddy, et al.
Fig. 9. Schematic structures of polymeric graphitic carbon nitride (g-CN),
melon strain, melem molecules, and heptazine. Reproduced from Ref (Wu et al.,
2018). with permission from Wiley.
Fig. 10. Schematics of the synthesis of nitrogen-doped carbon nitride (NeCN).
Reproduced from Ref (Wu et al., 2018). with permission from Wiley.
activity much higher (ten times) than that of CN upon exposure to
visible light, having quantum yields of 17% and 15% at 420 and
450 nm, respectively. It was observed that at 3 wt% loading of platinum
particles when deposited onto the catalyst surface during in-situ pho-
tocatalytic reaction, the CN and NeCN catalysts showed quantum
yields of 3.7% and 17%, respectively.
Metal-free, core-shell carbon spheres/polymeric graphitic carbon
nitride photocatalysts have been fabricated by using an electrostatic
self-assembly method (Ma et al., 2017b). In this process, tri-s-triazaine
was used during polymerization to prepare polymeric C3N4. Tri-s-tria-
zaine is stable up to 873 K in air and is not soluble in aqueous solution
or organic solvents. Such characteristics allow the formation of na-
nostructured g-C3N4 through solution chemistry. On the other hand,
melon units have many active sites and serve as ammonium-ion species
(Fig. 11). The protonated g-C3N4 would repolymerize after the removal
of strong oxidizing agents, and grow along the surface of carbon layers.
In the next step, nitric acid was used as a medium for solution pro-
cessing of g-C3N4 because of the strong oxidizing nature of nitrate ions.
The protons can intercalate easily into the 3D layer structures of g-
C3N4. This formed a 2D g-C3N4 shell in-situ on the carbon spheres,
yielding carbon@g-C3N4 core-shell nanostructures by the chemical
method as shown in Fig. 12. This photocatalytic material was metal-
Fig. 11. Schematic representation of the structures of carbon nanomaterials,
tri-s-triazine, and g-C3N4. Reproduced from Ref (Ma et al., 2017b). with per-
mission from ACS.
31
Journal of Environmental Management 238 (2019) 25–40
Fig. 12. Field emission scanning electron microscopy (FE-SEM) images of (a)
carbon spheres, (b) a mixture of C3N4 gel and carbon spheres, (c) carbon/g-
C3N4 core-shell hybrids, (d) transmission electron microscopy (TEM), (e)
magnified TEM images of carbon/g-C3N4 core-shell catalysts, and (f) close-up
images of g-C3N4shell of 3-nm thickness on carbon particles. Reproduced from
Ref (Ma et al., 2017b). with permission from ACS.
free, highly effective, and highly stable visible light active for hydrogen
production up to 129 molh-1 in visible light (λ = 420 nm). Core-shell
carbon@g-C3N4 catalysts showed eight-times higher hydrogen pro-
duction rate compared to that of nascent g-C3N4 catalysts. However, the
greater photocatalytic activity was attributed to its efficient light ab-
sorption and establishment of the well-designed core-shell structure
that remarkably improved the light absorption as well as separation of
the photo-initiated electron-hole pairs via electrostatic field in the in-
terlayer of carbon spheres and g-C3N4.
Kalousek et al. (2017) described the preparation of a novel photo-
catalyst, such as g-C3N4/Ni-complex, and tested it for hydrogen evo-
lution in the presence of tri-ethanolamine as a sacrificial agent. They
found that the catalyst prepared with 0.4 wt% of nickel-mercapto
ethanol complex displayed maximum photocatalytic efficiency with a
hydrogen production rate of 2.59 molh-1 after 3 h, which remained the
same for the next 5 h. This is due to the electrons photogenerated by
bandgap excitation, which are moved to the Ni complex. The complex
was reduced from Ni (II) ions to Ni (I), which were oxidized by pro-
tonation and H atom on nickel atom was then reduced to hydrogen.
A novel porous polymeric g-C3N4/TiO2 donor-acceptor heterojunc-
tion catalyst was fabricated through the combination of template
technique and co-calcination process. This catalyst showed much
higher catalytic activity, high surface area and absorption of light than
the pure TiO2 nanoparticles and g-C3N4 (Shen et al., 2017). In this
method, porous melem was initially synthesized by using CaCo3 as a
green template, which could be easily removed with dilute acidic HCl.
The heterojuction catalyst was then obtained by the self-assembly and
subsequent co-calcination (Fig. 13).
Ke et al. (2017) described the construction of sulfur-doped poly-
meric carbon nitride (SeC3N4) by introducing sulfur into C3N4 to
weaken the planar hydrogen bonds. They studied this new catalytic
material for the photocatalytic reduction of uranyl ions (UO22+) in an
aqueous system under the visible light irradiation, at the maximum rate
of 0.16 min−1, which was nearly 3 times higher than that of pure g-
C3N4. The S-doping of the SeC3N4 catalyst modified its electronic
structure, reflected by the elevated conduction and valance band levels,
and narrower band-gap as well as enhanced transport capability of
photogenerated electrons.
Another novel mesoporous polymeric organic framework was pre-
pared by the reaction of phloroglucinol and terephthaldehyde under
pyrolysis conditions, and used as an effective photocatalyst for the re-
duction of hexavalent chromium ions (Cr6+) from an aqueous solution
under the UV light with an 18 W lamp. The catalytic efficiency of this
K.R. Reddy, et al.
Fig. 13. Fabrication of porous polymeric carbon nitride/TiO2 hybrid catalyst.
Reproduced from Ref (Shen et al., 2017). with permission from Elsevier.
material was 200% higher than that of the Degussa's P25 TiO2 photo-
catalyst (Kostas et al., 2017). The catalyst was also successfully recycled
for the reduction of chromium ions at least ten times. The morphology-
dependent photocatalytic hydrogen generation performance of g-C3N4
photocatalysts was also demonstrated for the 2D structure (Lin and
Wang, 2013).
Zheng et al. (2014) reported that polymeric g-C3N4can imprinted
with the morphological structures of twisted hexagonal nanorods by
using a nanocasting process in the presence of a chiral porous SiO2 as
the sacrificial hard-template. As shown in Fig. 14, the chiral meso-
porous silica (CMS) was acidified with diluted HCl to stimulate the
reaction between CMS and cyanamide (CY) through acid-base interac-
tions under sonication which allowed the CY molecules to enter into the
channels of CMS. Then, the CMS/Cy reaction mixture was thermally
polymerized under an inert atmosphere to generate CMS/g-C3N4. In the
final step, the hard silica -template was completely removed by etching
with an NH4HF2 solution and washing with an excess amount of deio-
nized water and ethanol, resulting in the formation of helical nanorod
photocatalysts with a surface area of ca. 56 m2/g. The new material
possessed two types of pores in the nanorods: (i) small mesopores with
size of 3.8 nm, and (ii) large mesopores with a size of 10.7 nm dia. This
twisted helical nanostructured chiral photocatalysts showed excellent
photocatalytic activity and optical characteristics because the separa-
tion of charge carriers and mass transfer in polymeric carbon nitride
was promoted, allowing it to serve as highly stable photocatalytic
material for hydrogen generation as well as for the reduction of CO2.
Further, it was observed that helical structured carbon nitride
Fig. 14. Schematic diagram for the fabrication of helical nanorod-structured
polymeric graphitic carbon nitride. Reproduced from Ref (Zheng et al., 2014).
with permission from Wiley.
32
Journal of Environmental Management 238 (2019) 25–40
Fig. 15. The photocatalytic hydrogen evolution performance of helical na-
norod-structured polymeric g-C3N4 photocatalyst containing 3 wt% of Pt par-
ticles under visible light illumination with the wavelength of λ > 420 nm.
Reproduced from Ref (Zheng et al., 2014). with permission from Wiley.
photocatalysts with 3 wt% Pt as the co-catalyst showed an initial hy-
drogen production rate of 74 μmolh−1 with inherent catalytic stability
over four successive experimental runs, which is seven times greater
than that of pure carbon nitride (10 μmolh−1) as shown in Fig. 15. This
further proved the stability of morphology, texture, properties, and
photocatalytic efficiency of helical nanorod carbon nitride photo-
catalysts (see Table 1).
The photocatalytic activity of polymeric g-C3N4 was studied in
aqueous system with and without platinum particles as a co-catalyst,
which showed a better activity than the pure carbon nitride (Wang
et al., 2009). Later, various strategies were established to improve the
photocatalytic hydrogen generation of polymeric carbon nitride by
modifying the surface with non-metals (B, F, O, S, P and self-doping);
this enhanced the solar light absorption, and yielded novel morpholo-
gical structures such as porous, core-shell, helical, and hollow particle,
with the active sites (Zhang et al., 2014a). The existence of sacrificial
electron donors in the polymeric nitride catalyst, resulted in an increase
of quantum efficiency of hydrogen generation upon exposure to the
visible light, and the catalytic rate was superior to that of inorganic
semiconducting catalysts. It was noticed that using the light elements
(C, N, and S) to modify the polymeric nitride, stable catalysts were
resulted in the photocatalytic performance for H2 generation. Interest-
ingly, nitrogen generation during water oxidation process did not on
the polymeric g-C3N4 catalyst. Similarly, the polymeric g-C3N4 photo-
catalyst was modified with various co-catalysts (e.g. Fe, Ni, Au, Ag, Co,
and ZnO) for hydrogen evolution, and the results are summarized in
Table 2.
2.4. Polymeric g-C3N4–based hybrid photocatalysts for CO2 reduction
Polymeric g-C3N4-based nanohybrids photocatalytic materials have
shown the potential for photocatalytic CO2 reduction into solar fuels.
However, photocatalytic CO2 reduction efficiency of pristine g-C3N4 is
currently poor because of its weak absorption of visible light and rapid
charge recombination rate. By combining g-C3N4 with a second semi-
conductor, photosensitizers or a co-catalyst to form a composite pho-
tocatalytic CO2 reduction rate can be enhanced. Various approaches
have been advanced to change the electronic band structure such as
adding a narrow bandgap semiconductor, doping with metal ions,
dispersion of nobel metal particles, and surface sensitization with syn-
thetic dyes or inorganic metal complexes (Murugesan et al., 2017). For
 K.R. Reddy, et al.

Table 1
The list of recent photocatalysts based on various polymeric hybrid semiconductors.
Polymeric photocatalysts Modifier Immobilization method Pollutant removal Light source Ref.

g-C3N4 Ag/AgO In situ process Voilet-7 12 fluorescent lamps Vidyasagar et al. (2018)
C3N4 Phthaloyanine Impregnation MB 500 W Xe lamp Zhang et al. (2016a)
Porous polymeric g-C3N4 – Hydrothermal Ibuprofen 16W LED Ibad et al. (2017)
Polymeric carbon nitride Ag Heating via horizontal furnace MO 350-W Xe lamp Wu et al. (2017)
Polymeric carbon nitride Phosphate Thermal condensation MB UV light Lakshminarasimhan et al. (2017)
Polymeric g-C3N4 Sulfur Thermal polymerization Reduction of Cr (VI), RhB degradation Visible light Zheng et al. (2017)
Polymeric g-C3N4 RGO In-situ pyrolysis 17-β-estradiol, Ciprofloxacin, CO2 reduction Solar light Kumar et al. (2017a)
Polymeric g-C3N4 Magnetic BaFe12O19 Calcination RhB Visible light Wang et al. (2017c)
2D Graphitic carbon nitride Amino functionalization Self-assembly CO2 reduction 300 W Xe lamp Xia et al. (2017)
Polymeric g-C3N4 Quantum dots One-step Rose bengal 450W Xelamp Fabregat et al. (2017)
Triazine N-oxide-based porous polymer – 1,3-cycloaddition MO 400 W LED lamp at 420 nm Li et al. (2017)
Supramolecule- based g-C3N4 Carbon dopant Polycondensation Phenol 1000 W xenon lamp at 400 nm Zheng et al. (2016)
Polymeric g-C3N4 MS2 Direct heating of melamine Viral disinfection Visible light Li et al. (2016c)
Polymeric g-C3N4 – High temperature polycondensation at Tetracycline, Ciprofloxacin, Salicylic acid, UV–Visible light (35 W) Urestia et al. (2016)
500 °C Ibuprofen

33
Polymeric g-C3N4 Ru (II)-complex High temperature pyrolysis CO2 reduction Visible light Kuriki et al. (2016)
Graphitic carbon TiO2 Polymerization and calcination MO, RhB, MB, 4-CP UVlight (Hg lamp) Zhang et al. (2016b)
Polymeric g-C3N4 Co-Pi, Co3O4, Thermal polymerization Oxygen evolution 300 W Xe Zhang et al. (2016c)
Polymeric g-C3N4 Co0.5Zn0.5Fe2O4 Hydrothermal method Chloromycetin 300 W Xe Ma et al. (2016)
Polymeric g-C3N4 Barbituric acid Condensation CO2 reduction 300 W Xe Qin et al. (2015)
Mesoporous g-C3N4 – Polycondensation MO, H2 generation 300 W Xe Shi et al. (2015a)
Polymeric g-C3N4 Polyoxometalate Hydrothermal method MB, and phenol UV-light (metal halide, He et al. (2015a)
575 W)
Polymeric nanotube – Slow heating process MB 300 W Xe Li et al. (2015a)
Polymeric g-C3N4 BiFeO3 Hydrothermal RhB 300 W Xe Fan et al. (2015a)
Polymeric g-C3N4 Fe2O3 Slow heating RhB 500 W Xe Ye et al. (2013)
Poly(1-naphthylamine) organic – Polymerization Coomassie Blue RG-250 Sun light Riaz and Ashraf (2012)
semiconductor
Polyimide N-oxide organic photocatalyst – Direct heating MO Visible light Yang et al. (2012)
Polymeric g-C3N4 Activated with H2O2 Thermal polycondensation RhB 500 W halogen lamp Cui et al. (2012)
(λ < 400)
Polymeric g-C3N4 Ag Heating MO H2/10.1 μmol/h 500 W Xe Ge et al. (2011a)
Polymeric g-C3N4 – Heating of urea in air RhB 500 W Xe (λ < 400) Dong et al. (2011a)
Polymeric g-C3N4 Bi2WO6 Calcination MO 500 W Xe Ge et al. (2011b)
Polymeric g-C3N4 – Amidation reaction MO Visible light (λ > 400) Guo et al. (2010)
Journal of Environmental Management 238 (2019) 25–40
K.R. Reddy, et al. Journal of Environmental Management 238 (2019) 25–40

Table 2
Summary of hydrogen generation performance of various polymeric- semiconducting based photocatalysts. Note: The values reported in the fourth column are based
on specific experimental conditions described in the specific studies and direct comparison between these values should not be done.
Polymeric carbon nitride based Reaction solution Light source H2 production μmol. h−1 g−1
cat Ref.
catalysts

Polymeric g-C3N4 TEOA + H2O 300 W Xe 50 Wang et al. (2017d)

Urea-modified Pt/C3N4 CH3OH + H2O Solar 56.2 Lau et al. (2017)
Boron-doped g-C3N4 TEOA + H2O 300 W Xe with 420 nm 9.1 Gu et al. (2016)
g-C3N4/Bi4Ti3O12/Bi2Ti2O7 TEOA + H2O 300 W Xe 638 Zhao et al. (2016b)
Quasi-2D g-C3N4 TEOA + H2O Xe lamp with > 300 nm 898.2 Ma et al. (2015)
g-C3N4/conjugated copolymer TEOA + H2O 300 W Xe 436 Fan et al. (2015b)
Nitrogen self-doped 2D g-C3N4 TEOA + H2O Visible light with > 400 nm 44.28 Fang et al. (2015)
PolymericPt g-C3N4/NaNbO3 wires H2O 300 W Xe lamp, 420 nm Reduction of CO2 to CH4, with 6.4 μmol. Shi et al. (2014)
h−1 g−1
Polymeric g-C3N4 C2H5OH + H2O 2 kW Xe lamp, > 420 nm H2O2 with 30 μmol Shiraishi et al. (2014)
Iodine-doped g-C3N4/3 wt% Pt TEOA + H2O Solar (500–550 nm) 38 Zhang et al. (2014b)
Polymeric g-C3N4/NiS2/1 wt% Pt TEOA + H2O 300 W Xe with > 420 nm 1.14 Yin et al. (2014)
Polymeric g-C3N4/thiophene/3 wt% Pt TEOA + H2O 300 W Xe with > 420 nm 131 Zhang et al. (2014c)
Sulfur-doped polymeric g-C3N4/1 wt% CH3OH + H2O 300 W Xe lamp 12.16 Ge et al. (2013)
Pt
Polymeric g-C3N4/CdS/1 wt% Pt CH3OH + H2O 300 W Xe lamp 17.27 Ge et al. (2012)
Polymeric g-C3N4/Co3O4 H2O Visible light O2 with 90 μmol Zhang et al. (2012c)
Hallow polymeric g-C3N4 TEOA (0.2 wt% Pt cocatalyst)+H2O 300 W Xe lamp 81.58 Liu et al. (2018a)
(λ > 420 nm)
Phosphorus-doped polymeric g-C3N4 TEOA + H2O 300 W Xe lamp 303.97 Liu et al. (2018b)
Polymeric g-C3N4/Ag fiber TEOA(1% Pt)+H2O 300 W Xe lamp 625 Wang et al. (2017e)
(λ > 420 nm)
Polymeric g-C3N4/Co2P (2 wt%) TEOA + K2HPO4+H2O 300 W Xe lamp 27.81 Shen et al. (2018)
(λ > 420 nm)

instance, Ag compounds can considerably increase the photoactivity of

Fig. 16. CO2 photoreduction mechanism and band structure alignment.
Reproduced from Ref (Putri et al., 2016). with permission from RSC.
Fig. 17. Schematic representation of composite fabrication. Reproduced from
Ref (Xu et al., 2018). with permission from Elsevier.
g-C3N4 in the presence of light. The plasmonic effect of Ag nano-
particles can significantly boost visible light absorption of the catalyst,
improve the incident light absorption, and stimulate the separation of
electrons and the hole.
The Ag3PO4@g-C3N4 hybrid catalysts have been synthesized via in-
situ deposition route to achieve enhanced photocatalytic reduction of
CO2 (He et al., 2015b). The results have shown that the existence of
Ag3PO4 on to the surface of g-C3N4 significantly enhanced the light
absorption capacity. More significantly, because of the formation of a
heterojunction structure between Ag3PO4 and g-C3N4, the separation of
charge carriers through Z-scheme mechanism improved the CO2 re-
duction activity of Ag3PO4@g-C3N4hybrid photocatalyst. Under the si-
mulated sunlight illumination, the optimized Ag3PO4@g-C3N4 hetero-
structured catalyst exhibited a greater CO2 conversion rate
(57.5 μmolh−1gcat−1), which was 6.1 and 10.4 times greater than those
of the pure g-C3N4 and P25 catalysts, respectively.
In order to exploit the advantages of g-C3N4 and the classic TiO2,
composites of TiO2 and g-C3N4have been proposed to form (g-C3N4-
TiO2). Linking TiO2 to a g-C3N4 catalyst composite appears to be a
potential way to create a heterojunction structure, which improved the
photoactivity, charge transfer capability, and increase the diversity of
photocatalyst system. In this direction, a series of hybrid photocatalysts
of g-C3N4 and nitrogen (N)-doped titanate (g-C3N4@NeTiO2) was
prepared using direct pyrolysis of urea and Ti(OH)4 for the photo-
reduction of CO2 to CO (Zhou et al., 2014). While developing these
hybrid catalysts, the weight ratio of urea to Ti(OH)4 had a key effect on
the performance. Therefore, the composites of g-C3N4 and N-doped
TiO2 have been prepared with high mass ratios of urea to Ti(OH)4,
where as in the N-doped TiO2 only low ratios were used. Thus, prepared
N-doped TiO2 photocatalysts have shown to evolve CO and CH4, where
as the g-C3N4@NeTiO2 hybrid catalysts yielded CO. Under 12 h light
irradiation, the optimized photocatalyst produced four times more CO
(14.73 mol) than that of P25 catalyst. When comparative studies were
conducted with the pristine g-C3N4 and pristine P25 catalysts, the as-
synthesized g-C3N4-NeTiO2 photocatalysts show improved photo-
catalytic activity for catalytic reduction of CO2 in the presence of water
vapor at room temperature.

34
K.R. Reddy, et al. Journal of Environmental Management 238 (2019) 25–40

Fig. 18. (a) Schematic representation of the synthesis process of ACNNG-x hybrid catalysts, and (b, c) SEM images suggested a photocatalytic mechanism for
photodegradation and CO2 reduction by the composites. Reproduced from Ref (Li et al., 2015b). with permission from Wiley.

Table 3
Summary of CO2 reduction performance of various polymeric semi-conducting materials based photocatalysts. Note: The values in the fourth column are based on
specific experimental conditions described in the specific studies and direct comparison between these values should not be done.
Polymeric based photocatalyst Modifier Light source Main products Ref

g-C3N4 B4C 300W Xenon short arc lamp (0.84 μmolg−1 CH4 Zhang et al. (2016d)
h−1)
g-C3N4 boron doped AM 1.5 G solar -simulated light CO and C2H5OH Sagara et al. (2016)
g-C3N4 Bi2WO6 300 W xenon arc lamp CO (5.19 mmolg−1h−1) Li et al. (2015c)
g-C3N4 BiOI Visible light > 400 nm CO (4.86 μmolg−1h−1) CH4 (0.18 μmolg−1h−1) Wang et al. (2016)
g-C3N4 CdIn2S4 300W Xenon lamp CH3OH (42.7 μmolg−1h−1) Liu et al. (2017)
g-C3N4SnO2/BeP Co-doped(> 420 nm) 300 W Xe lamp CH4 (49 μmol) Raziq et al. (2017)
g-C3N4 CO4 300 W Xe lamp CO (107 μmolg−1h−1) Zhao et al. (2017b)
C3N4 Co-porphyrin 300 W Xe lamp CO (17 μmolg−1h−1) Zhou et al. (2017b)
g-C3N4 UiO-66300 W Xe lamp CO (9.9 μmol gCN−1 h−1) Shi et al. (2015b)
g-C3N4 CH4 Carbon nanodots Xe lamp (> 400 nm) CO (58.8 μmol gCN−1 h−1) (29.23 μmol gCN−1 Ong et al. (2017)
h−1)
g-C3N4 CdS 250 W lamp CH3OH 1352.07 μmolh−1gcat−1 Yang et al. (2016)
g-C3N4 CeO2 300 W Xenon-arc lamp CO (0.590 μmol) CH4 (0.694 μmol) Li et al. (2016d)
Npg-C3N4 Ir-T Visible light CH3OH (9934 μmol g cat −1) Kumar et al.
(2017b)

Ohno et al. (2014) synthesized an extremely active visible-light
photocatalyst consisting of WO3, and g-C3N4 for CO2 reduction by three
different methods (mixture using an agate mortar, infuse and terrestrial
mill). The WO3/g-C3N4 hybrid catalysts prepared using a planetary ball
mill exhibited superior photocatalytic properties. Furthermore, gold
nanoparticles were added to WO3/g-C3N4 composite by photo-deposi-
tion. The Au metal encapsulated composite catalyst resulted in in-
creased production of CH3OH because the encapsulated Au metallic
particles played a significant role in multi-electron reduction of CO2.
The Au NPs-encapsulated hybrid catalyst showed the photocatalytic
activity 1.7 times greater than that of the photocatalyst synthesized
without using Au NPs. The extraordinary oxidation capacity of WO3
and the improved reduction ability of g-C3N4was achieved because of
the Z-scheme catalytic reaction in the hybrid photocatalyst and im-
proved the photocatalytic reduction of CO2.
As per findings, several silver-based modifiers such as AgBr, AgCl,
Ag, Ag3PO4, Ag3SO4 (Putri et al., 2016) were found to be capable of
forming a new class of visible-light-driven photocatalysts owing to their
photosensitive properties. During photocatalytic process, some of the
silver salts were instantaneously reduced to metallic Ag0, which boosts
the photocatalytic performance because of the synergistic properties
arising from the surface Plasmon resonance effect. The initial formation
of Ag0 particles generates an Ag/AgX heterojunction that increases the
electron–hole separation, resulting in extremely stable photocatalysts.

35
K.R. Reddy, et al.
Fig. 19. Synthesis of AgPd@g-C3N4.
Fig. 20. Visible light mediated upgrading of biomass and N-aminoformylation
of nitroarenes. Reproduced from Ref (Verma et al., 2016b). with permission
from Wiley and RSC.
Fig. 21. Synthesis of photoactive oxo-vanadium VO(acac)2 catalyst.
Reproduced from Ref (Verma et al., 2016e). with permission from ACS.
To study the properties of carbon nitrate and AgX, Putriet al (Putri
et al., 2016). reported silver chloride (AgCl)/g-C3N4 hybrid prepared
using a deposition–precipitation method for the reduction of CO2 to
CH4. The as-prepared AgCl/g-C3N4 composites showed improved light-
harvesting capabilities and enhanced electron and hole separation
abilities. The optimized AgCl/carbon nitride photocatalyst showed 2.5
times enhancement upon visible light irradiation compared to pure
carbon nitride. This enhancement may be due to the formation of Ag0
during photocatalytic reaction, which exhibits SPR effect in the visible
region, thereby improving the light absorption capacity and further
encouraging the photogenerated charge transfer.
On the basis of band levels of AgCl and carbon nitride, the possible
36
Journal of Environmental Management 238 (2019) 25–40
mechanism of charge transfer in Ag/AgCl/carbon nitrate composite is
shown in Fig. 16. Upon light irradiation, the prepared hybrid photo-
catalyst excites electron-hole pairs, when a photon energy equivalently
to or higher than their bandgap energy of catalyst material. Electrons
are excited from the VB to the CB of each particular material, leaving
the same amount of holes. Then, the successive CO2 transformation
procedure is a consecutive combination of H2O oxidation and CO2 re-
duction. Electrons preferably flow from carbon nitride to the attached
AgCl because the conduction band potential of carbon nitrides is more
negative than that of AgCl. Meanwhile, because of the SPR effect of Ag,
the Plasmon-induced electrons also transfer to AgCl, moving to the AgCl
surface. On the other side, photoinduced holes moved in the opposite
direction and are collected in CN because the valence band potential of
AgCl is more positive than that of carbon nitride. For CO2 photo-
reduction, these spatially divided electrons and holes are huge re-
sources. Because the redox potentials for H+/H2O and CO2/CH4lie
within the valence band of carbon nitride and the conduction band of
AgCl, the AgCl/carbon nitride composites can react with surface-ad-
sorbed H2O and CO2 to form CH4.
For the binary composites, there is a disadvantage; for instance, it is
difficult to transfer the separated charges so that they can contribute to
redox reactions. To overcome this problem, ternary composites can be
prepared by introducing an additional co-catalyst that can deliver the
efficient redox reaction sites, prevent possible charge recombination,
and reduce the reaction activation energy. Furthermore, this kind of
super-hybrid photocatalytic ternary structured catalysts can remarkably
overcome the disadvantages associated with the single components and
achieve high charge separation rates as well as excellent redox ability
and durability. Xu et al. (2018) synthesized a Ag2CrO4/g-C3N4/gra-
phene oxide ternary nanocomposite for enhanced photocatalyst CO2
reduction into methanol (CH3OH) and methane (CH4). In the synthe-
sized ternary nanocomposite, silver chromate (Ag2CrO4) nanoparticles
acted as a photosensitizer and graphene oxide (GO) as the co-catalyst.
The composites were fabricated by self-assembly precipitation tech-
nique as shown in Fig. 17.
The prepared ternary photocatalyst Ag2CrO4/g-C3N4/GO composite
exhibited an improved CO2-conversion activity of 1.03 μmol g−1 with a
turnover frequency (TOF) value of 0.30 h−1 under sunlight exposure,
which is 2.3 times greater than that of bare g-C3N4. The light absorption
capacity of g-C3N4 was enhanced by Ag2CrO4 nanospheres, because the
Ag2CrO4 nanoparticles acted as a photosensitizer and the GO na-
nosheets as the electron acceptors, which encouraged the charge se-
paration. In addition, there are many active sites available for photo-
catalytic activity. Additionally, because of the charge relocation
between Ag2CrO4 and g-C3N4, which followed the straight Z-scheme
catalytic mechanism that encouraged charge separation and increased
the redox capability of the photocatalytic system.
Li et al. (2015b). fabricated AgBr nanospheres-coated onto the outer
surface of g-C3N4-modified nitrogen-doped graphene (NG) ternary
structured catalysts (ACNNG-x) with a different weight ratio of CNNG
in (AgBr + CNNG) for the photodegradation of organic dyes and re-
duction of CO2under visible light. Fig. 18 (a) shows a schematic re-
presentation of the preparation process of ACNNG-x nanocomposite.
Fig. 18 (b) shows SEM image of the optimized ternary nanocomposite.
The optimized ternary composite sample showed that CO2 reduction
achieved the rates of 105.89 μmol g−1 for methanol, and
256.45 μmol g−1 for ethanol, respectively. The suggested photo-
catalytic mechanism for photodegradation of organic dye pollutants
and photoreduction of CO2 of the optimized ternary composite is shown
in Fig. 18 (c).
From the analysis of data, ternary nanocomposite exhibited out-
standing CO2 reduction under visible light illumination, probably
arising from the heterojunction system, which can effectively increase
the photogenerated charge carrier separation efficiency, decrease the
recombination rate of electron–holes pairs, and separate more charge
carriers to form more reactive species (see Table 3).
K.R. Reddy, et al. Journal of Environmental Management 238 (2019) 25–40

(b)
(a)

(c)

Fig. 22. Application of VO@g-C3N4 in C-H activation under visible light irradiation. Reproduced from Ref (Verma et al., 2016c, 2016e). with permission from ACS.

Fig. 23. Synthesis of magnetic graphitic carbon nitride (Fe@g-C3N4).

Fig. 25. Synthesis of photoactive palladium nanoparticles immobilized gra-

phitic carbon nitride, Pd@g-C3N4 catalyst (Verma et al., 2018), Reproduceble
from Elsevier.

2.5. Polymeric g-C3N4–based nanohybrid photocatalysts in chemical

transformation

Energy consumption and demand continue to grow in both the

Fig. 24. Fe@g-C3N4 catalyzed hydrogenation of alkenes and alkynes.
Reproduced from Ref (Baig et al., 2016). with permission from ACS.
United States and the world. Thus, one can predict that petroleum
consumption may surpass its production due to finite quantities of
petroleum (Turner, 2015). The importance of limiting fossil fuel re-
sources to reduce climate change and greenhouse gas emission cannot
be ignored (Reddy et al., 1016). Biomass and chemical feedstocks de-
veloped from renewable resources are a sustainable method of reducing

37
K.R. Reddy, et al.
Fig. 26. Pd@g-C3N4 catalyzed oxidative esterification of alcohols (Verma et al.,
2018), Reproduceble from Elsevier.
Fig. 27. Synthesis of bimetallic photoactive CuAg@g-C3N4 catalyst.
Reproduceble from ACS (Verma et al., 2017).
Fig. 28. Hydroxylation of benzene via CeH activation using bimetallic CuAg@
g-C3N4. Reproduceble from ACS (Verma et al., 2017).
our dependence on crude oil, while at the same time, recycling carbon
dioxide through photosynthesis. Though these biofuels hold many dis-
tinct advantages for the environment when applied as a petroleum al-
ternative, they also present a major challenge, since one must chemi-
cally modify bio-derived fuels to make them compatible with the
existing technology (Phongamwong et al., 2017). To solve this chal-
lenge, Nadagouda et al. designed a novel method for photoactive g-
C3N4- based catalysts (Verma et al., 2016a; Verma et al., 2016b; Nasir
Baig et al., 2016; Verma et al., 2016c; Verma et al., 2016d; Verma et al.,
2016e; Baig et al., 2016; Verma et al., 2018). They further utilized this
38
Journal of Environmental Management 238 (2019) 25–40
material in designing AgPd@g-C3N4heterogeneous catalyst [Fig. 19],
which has the ability to absorb visible light energy to cross the energy
barrier in the reaction (Verma et al., 2016a, 2016b; Nasir Baig et al.,
2016). After dispersing g-C3N4 in water, adding AgNO3 and Pd(NO3)2 to
the solution, and later treated it with sodium borohydride to reduce
silver and palladium salts to Ag (0) and Pd(0) nanoparticles over g-C3N4
that led to a brown-black AgPd@g-C3N4 powder catalyst (Verma et al.,
2016a). The authors demonstrated its application in the upgrading of
biomass via hydro deoxygenation of vanillin (Verma et al., 2016a),
cyclative hydrogenation of levulinic acid (Verma et al., 2016b) and N-
amino formylation of nitroarenes (Nasir Baig et al., 2016) under visible
light using {{}}{{}}domestic 40 W bulb [Fig. 20].
In previous reports for the upgrading of 4-hydroxy-3-methox-
ybenzaldehyde (vanillin), a common component available in lignin, the
use of hydrogen at elevated pressure resulted in the formation of 4-
hydroxymethyl-2-methoxyphenol as a by-product and no side product
was observed (Verma et al., 2016a). The key step in the synthesis of γ-
valerolactone (GVL) is the cyclative hydrogenation of levulinic acid
(LA) (Verma et al., 2016b). However, only immobilization of palladium
over g-C3N4 in different proportions, failed to accomplish such trans-
formation using formic acid as a source of hydrogen under photo-che-
mical conditions, but synergic effect between silver and palladium na-
noparticles played a major role in the reaction (Verma et al., 2016b).
Furthermore, visible light energy activation did not require high
temperature and hydrogen pressure that is normally used in upgrading
the biomass (Verma et al., 2016b; Nasir Baig et al., 2016) and this
method utilized formic acid as a source of hydrogen under photo-che-
mical conditions and increased the degree of dissociation of formic acid
into hydrogen and carbon dioxide under visible light irradiation (Verma
et al., 2016a, 2016b; Nasir Baig et al., 2016). The authors developed
sustainable protocols in organic synthesis and synthesized oxo-vana-
dium-supported g-C3N4 photocatalyst Verma et al., 2016c; Verma et al.,
2016d; Verma et al., 2016e; Fig. 21] and demonstrated these in oxi-
dation reactions [Fig. 22] such as selective oxidation of series of alco-
hols (Verma et al., 2016c), oxidative esterification of alcohols (Verma
et al., 2016d) and oxidation of hydrocarbon via Ce activation (Verma
et al., 2016e). Further, calcination of urea was used to synthesize g-
C3N4, by adding a methanolic solution of VO(acac)2. The mixture was
centrifuged and dried to produce a VO@g-C3N4 catalyst that was ef-
fective for clean environment and energy via visible light absorption
{{}} (Verma et al., 2016c).
In continuation, Nadagouda et al. also synthesized magnetic Fe@g-
C3N4 as a photocatalyst [Fig. 23] for use in hydrogenation of alkenes
and alkynes using aqueous hydrazine as a source of hydrogen (Baig
et al., 2016). The catalyst eliminated high-pressure hydrogen and per-
mitted the reaction at room temperature. Due to non-covalent inter-
actions between nano-ferrites and photoactive g-C3N4 surface, Fe@g-
C3N4 showed high stability. Hydrogenation of a library of alkenes and
alkynes was achieved in excellent yields at ambient reaction condition
using the visible light as a source of energy (Baig et al., 2016; Fig. 24).
Further, a highly efficient and a simple method was also used for the
synthesis of esters from the corresponding alcohols via CeH activation
using g-C3N4 supported palladium nanoparticles viz., Pd@g-C3N4 as a
photocatalyst at room temperature (Verma et al., 2018; Fig. 25). Here,
aerial oxygen was used as a co-oxidant, which was adsorbed by Pd@g-
C3N4 leading to CeH activation and consequently, oxidative ester-
ification of aromatic alcohols (Verma et al., 2018; Fig. 26).
The bimetallic photoactive CuAg@g-C3N4 catalyst developed
[Fig. 27] by the immobilization of copper and silver nanoparticles over
the surface of g-C3N4 was demonstrated for the synthesis of phenol
using hydrogen peroxide as an oxidant via CeH activation of benzene
(Verma et al., 2017). The nitrogenous framework in g-C3N4 absorbs the
visible light and distributes in the reaction media leading the facilita-
tion of the CeH bond of benzene. Additionally, synergistic interaction
of copper and silver nanoparticles enhanced the dissociation of H2O2 to
OH radical due to the formation of phenol in less than 30 min [Fig. 28].
K.R. Reddy, et al.
3. Challenges, prospects and future trends
This review emphasizes recent developments used in synthetic
strategies for the preparation of polymeric graphitic carbon nitride (g-
C3N4)-based heterogeneous photocatalysts along with their outstanding
physicochemical properties, morphological structures, and unique
photocatalytic applications in air (NOx) purification, wastewater
treatment, hydrogen production, CO2 reduction and chemical trans-
formation. These new photocatalytic materials possess intriguing phy-
sical, chemical, structural, morphological, electronic, catalytic, and
narrow bandgap characteristics. Their properties and photocatalytic
efficiencies can be tuned by controlling the size, morphological struc-
tures, bandgap, chemical functionalities, and heterostructures with the
dopants, nanoscale metal oxides, and carbon materials.
The functionalization process which is a synergistic combination
between graphitic-C3N4 and other dopants or metal oxides or nano-
carbons, has a significant effect on the physicochemical properties,
bandgap as well as photocatalytic performance of their hybrid photo-
catalysts. Along with a wide range of remarkable key properties, these
catalysts show the potential for a series of novel photocatalytic appli-
cations in the areas of energy production and environmental remedia-
tion. Their photocatalytic efficiency for these applications is superior to
other conventional inorganic metal oxides (e.g. TiO2or ZnO)-based
photocatalytic materials.
Despite the recent significant developments, research efforts in the
area of polymeric semiconductor (g-C3N4)-based hierarchically struc-
tured photocatalysts are still in its infancy, and numerous challenges
yet remain to be solved. For instance, those related to physicochemical
characteristics such as thickness, shape, bandgap, edge engineering,
doping effects, and chemical modification. Therefore, it is important to
develop highly efficient and advanced synthetic routes for precise
control to achieve advanced photocatalysts for their cost-effective,
large-scale applications in numerous fields. In summary, an in-depth
understanding of the properties, as well as the photocatalytic me-
chanism, still requires a deeper understanding of the various phe-
nomena involved as well as the photophysical principles.
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