Magnetic field-assisted photochemical oxidation of benzyl alcohol to corresponding aldehydes by introducing TiO2(P25)-ZnO/Fe3+ as a novel nanophotocatalyst

Article abstract of DOI:10.1002/jccs.202100300

For the first time, the surface modification of nanophotocatalyst TiO₂(P25)-ZnO was reported by the introduction of Fe³⁺ for modulation of the photocatalytic activity. The nanophotocatalyst TiO₂(P25)-ZnO/Fe³⁺ wa

Full text of DOI:10.1002/jccs.202100300

Received: 11 July 2021
Revised: 6 August 2021
Accepted: 9 August 2021
DOI: 10.1002/jccs.202100300
A R T I C L E
Magnetic field-assisted photochemical oxidation of benzyl
alcohol to corresponding aldehydes by introducing
TiO2(P25)-ZnO/Fe3+ as a novel nanophotocatalyst
Saied Fallahnezhad | Ali Amoozadeh
Department of Organic Chemistry,
Abstract
Faculty of Chemistry, Semnan University,
Semnan, Iran
For the first time, the surface modification of nanophotocatalyst TiO2(P25)-
ZnO was reported by the introduction of Fe3+ for modulation of the photo-
catalytic activity. The nanophotocatalyst TiO2(P25)-ZnO/Fe3+ was synthesized
and its crystal structure, morphology, and photocatalytic activity were well
determined by, diffuse reflectance spectroscopy, energy dispersive X-ray, X-ray
diffraction, and scanning electron microscope analyses. The photocatalyst was
applied for the selective oxidation of different aryl alcohols to the respective
aldehyde beneath visible light (blue LED lamp, λ > 420 nm) in the presence of
nitrate ion as oxidant. Also, for the first time, the effect of presence of an exter-
nal magnetic field (5,000 G) contemporary with photoreaction was studied
simultaneously by applying an external magnet field of 5,000 G and valuable
results were obtained so that the time of photoreaction declined considerably
up to 65%. This study has many advantages like the use of a magnetic field as a
green technology, being clean, and zero energy. Also, the photoreaction did
stop at the stage of aldehyde to provide a considerable selectivity.
Correspondence
Ali Amoozadeh, Department of Organic
Chemistry, Faculty of Chemistry, Semnan
University, 35131-19111, Semnan, Iran.
Email: aamozadeh@semnan.ac.ir
Funding information
Semnan University, Grant/Award
Number: Ali amoozadeh
K E Y W O R D S
magnetic field, photocatalyst, surface modification
1 | INTRODUCTION
and brookite. The anatase phase has superior photo-
catalytic attributes owing to the low recombination speed
The goal of TiO2-based photocatalysts is to reduce
organic contaminants.[1–9] When a photon of enough
high-energy encounters the surface of Titania, an elec-
tron (eꢀ) can be banished from the valence band (VB) to
the conduction band (CB). At the same time, this makes
a hole (h+), which is the loss of an electron, in the
VB. The holes can operate as forceful oxidizing agents,
while the ejected electrons have powerful reducing abil-
ity. Because these two active kinds have a sufficiently
long lifetime in semiconductor materials (such as TiO2),
their oxidizing and reducing power can operate on other
species. TiO2 has three crystalline phases: rutile, anatase,
of electron–hole couples resulting from the devious
bandgap. The band gaps of the rutile and anatase phase
are 3.03 and 3.20 eV, severally, and blended rutile and
anatase samples have greater work operation and elec-
tron affinities.[10] Newly, the CB of anatase has been
placed 0.2 eV under that of rutile.[10] As considered in
ref. [10], in the blended rutile and anatase samples,
which have great photocatalytic activities, the electrons'
motion from the rutile to the anatase phase, whenever
the holes travel in the inverse orientation. Commercial
Degussa TiO2(P25) has a 3:1 combination proportion of
anatase and rutile phases and a medium crystallite size of
J Chin Chem Soc. 2021;1–8.
http://www.jccs.wiley-vch.de
© 2021 The Chemical Society Located in Taipei & Wiley-VCH GmbH
1

2
FALLAHNEZHAD AND AMOOZADEH
21 nm.[11] Although the manners for the adaptation of
P25 are complicated and need high-temperature condi-
tions.[12] Also, the accurate mechanism and reason for
the reclaimed photocatalytic attributes on correction are
yet unfamiliar. However, the restriction of TiO2 is its
broad bandgap, which limited area from 3.0 to 3.2 eV,
and can be only activated by ultraviolet (UV) light
(λ < 380 nm). UV light comprises about 4% of the solar
energy attaining at the Earth's surface.[13] Because of the
low entering flux, the photocatalytic activity of TiO2
upon a broad span of wavelengths must be enhanced,
and this has been the subject of many research studies.
Zinc oxide is an inorganic compound with the formula
ZnO. It is a white powder that is insoluble in water.
ZnO is present in the Earth's crust as the mineral
zincite, which crystallizes in three several structures:
wurtzite, zincblende, and rock salt. ZnO has a powerful
normal leaning to crystallize in the wurtzite structure
and so, approximately all photocatalytic surveys are cen-
tralized on this structure. Pertaining on the optical
absorption confidants, the refractive index of ZnO (2.0)
is smaller than that of TiO2 (2.5–2.7), so ZnO with
difficulty diffuses light, thereupon manufacturing it
colorless and improves the transparency.
Extensive research attempts have been managed
toward raising the photocatalytic activity of TiO2. The
development of the TiO2-based photocatalysts has
accordingly appeared as a research subject of significance
and immediacy.[14] Expansion of new visible light-
sensitive TiO2 photocatalyst has been recently extensive
through dye sensitization,[15,16] transition metal,[17] non-
metal doping[18,19] and surface modification.[20,21] One
method to come close to improving TiO2 photocatalyst is
to dope transition metals into TiO2, and the other is to
make coupled photocatalysts.[14] It assists obtaining a
longer electron lifetime by efficient charge separation.[22]
Although when the photocatalyst was blended, the decay
was great as evaluated with the single catalyst.
(III), was researched pending the last years.[27–31] These
matters suggest modified visible light sensibility via an
interfacial charge transfer (IFCT) procedure without pre-
sent extra impurity rates in the bandgap of the TiO2. In
electron transmission procedures, grafted transition
metal nanoclusters can swiftly drop a quick photoin-
duced charge dissociation whenever lowering the charge
transporter recombination speed owing to their signifi-
cant action on as electron acceptors. Iron (Fe) has
attracted intensive attention as a bone implant material
because of its inherent biodegradability, favorable bio-
compatibility, and mechanical properties.[32]
Nowadays, the application of magnetic nanocomposites
as heterogeneous catalysts is a fascinating investigation
zone. The surface functionalization of these matters is a
tasteful route to bridge the split among heterogeneous and
homogeneous catalyses.[33] Whenever research on the effi-
cacy of magnetic field on the solvent's confidants are com-
paratively scared, the efficacy of the magnetic field on the
characteristic of water has been detected in the early 1900s
by Danish Physicist Hendricks Anton Lorenz.[34] This green
technology is clean and has zero energy using up.[35] The
influence of the magnetic field on macroscopic features and
microscopic structures of water has been formerly studied
by Xiao-Feng and Bo.[36] They have discovered several
changes in the water confidants once imported to the mag-
netic field. The dynamic magnetization approach was
carried out for the magnetization of water. Magnetic field-
assisted arrangement of photocatalytic TiO2 particles on
membrane surface to enhance membrane antifouling for
water treatment was the performance by Sun et al.[37] and
preparation of magnetic and photocatalytic membranes
with improved performance by Liu et al.[38]
Therefore, a nanocomposite of TiO2 and ZnO (TiO2-
ZnO) has been prepared, surface was reclaimed with
Fe(III) nanoclusters until TiO2-P25-ZnO/Fe3+ was pre-
pared and the surveying photochemical workmanship
was researched. It is significant that the TiO2-P25 which
is protected by ZnO is developing the crowd of photo-
synthesized charge transporters owing to a synergistic
interaction, whenever surface grafted Fe(III) ions partake
in a poly-electron reduction procedure as well as
suppressing the recombination of eꢀ/h+ pairs. The redox
potential of the Fe3+/Fe2+ redox pair (0.77 V vs. SHE,
pH = 0) allows impressive IFCT procedures in this order.
Then nanophotocatalyst was used in the oxidation of aryl
alcohol to respective aldehydes and based on the
literature,[39] reduction of nitrate ion takes place via one
of the several equations as a photocatalytic reaction.
Then, in this research, we applied a magnetic field when
a photocatalytic reaction was done, and was compared
the presence and absence of magnetic field on the yield,
photoreaction time and selectivity.
There are many applications of metal–organic frame-
works (MOFs) and MOF-derived materials that receive
growing attention for fine chemical synthesis due to
their versatile tunability and high catalytic activity.[23]
The selective oxidation with an active interface between
Au-Pd alloy nanoparticles (NPs) and cobalt oxide sup-
ports via calcination of a composite of NPs encapsulated
in MOFs was performed by Liao et al.[24] Effectiveness
of using
a perovskite/Zr-MOFs heterojunction in
realizing efficient and stable inverted p–i–n perovskite
solar cells (PVSCs) is demonstrated by Lee et al.[25] The
MOFs and derivatives are used as catalysts for biomass
conversion.[26]
Imaginably, the surface affixation of TiO2 with
nanoclusters of, that is, Cu (II), Cr (III), Fe (III), and Ce

FALLAHNEZHAD AND AMOOZADEH
3
2 | EXPERIMENTAL
2.1 | Materials
rinsed by deionized water to pick up the soluble ions.
The humid powder received was dried at 100ꢁC in the
air to form the pioneers of the hetero-structured
TiO2(P25)-ZnO photocatalysts that were better calcin-
ated at 250ꢁC in air for 3 hr. The nanosized photo-
catalysts were collected in powder form labeled as Ti10-
Zn (Ti/Zn molar ratios of 10:1).
All chemicals that were used in this research were
bought by the Merck and Aldrich chemical companies
with no requirement for extra purgation. TiO2(P25)
(ca. 70% anatase, 30% rutile; BET area ca. 50
15 m2 gꢀ1) powder was reserved by Degussa Company.
Twice distilled water was applied for the procurement of
different solutions. The pH of the solutions was co-equaled
with 1 M HCl or 1 M NaOH. Progress of reactions was
assayed by thin-layer chromatography on commercial
sheets covered with silica gel and UV spectroscopy too.
Fourier transform infrared spectroscopy (FT-IR) was per-
formed on a Shimadzu FT-IR 8400 rig using Potassium
Bromide pressed powder sheets in the span of 400–4,-
000 cmꢀ1. X-ray diffraction (XRD) was done for the
TiO2(P25)-ZnO/Fe3+. powder instance was conducted on a
Siemens D5000 diffractometer (Siemens AG, Munich, Ger-
many) using Cu-Kα radiation of wavelength 1.54ꢁA.
Energy dispersive X-ray (EDX) spectra of the photo-
catalyst were attained by a Mira 3-XMU scanning electron
microscope (SEM). The X-ray fluorescence (XRF, Model
ARL PERFOMIR'X) was applied for the elemental analy-
sis. Diffuse reflectance spectroscopy (DRS, Model Sinco
S4100, Korea) was applied for the designation of the opti-
cal band split (Eg) of TiO2(P25)-ZnO and TiO2(P25)-ZnO/
Fe3+. SEM images were obtained with a BAL-TEC SCD
005 SEM appliance operating at 10 kV. The reagents
applied in this research were of analytical scale.
2.2.2 | Surface affixation of the TiO2(P25)-
ZnO nanocomposites with Fe(III) ions
(TiO2(P25)-ZnO/Fe3+)
The affixation of Fe(III) nanoclusters on the surface of
the synthesized TiO2(P25)-ZnO composite was done by
addendum, an easy impregnation manner that has been
reported formerly.[28] In summary, the suitable ratio
(0.005–0.3 wt% Fe) of the iron salt was augmented into
an aqueous TiO2-P25-ZnO suspension and stirred at 90ꢁC
for 1 hr for achieving Fe(III) nanoclusters on the surface
TiO2(P25)-ZnO. Afterward, the aqueous solution was
centrifuged three times after laundering with great values
of distilled water and exsiccated at 110ꢁC for 24 hr afore
laborious the resulting solid into a nice powder that
named Ti10-Zn/Fe3+
.
3 | RESULTS AND DISCUSSION
In expanse of our continuous plans on procurement of
new heterogeneous photocatalysts[40] for organic
reactions, we have proposed the procreation of
nanophotocatalyst named TiO2(P25)-ZnO/Fe3+ that was
made of surface modification of TiO2(P25)-ZnO. This
novel nanophotocatalyst was characterized via, XRD, EDX
spectroscopy, DRS, and SEM. Nanophotocatalyst was used
in the photoreaction with modification in terms of photo-
reaction. Then nanophotocatalyst was used in the oxida-
tion of aryl alcohol to respective aldehydes as a
photocatalytic reaction and was proofed the surface modi-
2.2 | Preparation of nanosized
photocatalysts
2.2.1 | Nanosized heterostructured
TiO2(P25)-ZnO photocatalysts
TiO2(25) and Zn (NO3)2ꢂ6H2O were applied as beginning
materials, and NaOH was applied as the precipitant
without major purification. Zn(NO3)2ꢂ6H2O was dis-
solved in a least value of deionized water with fixed stir-
ring up to a clear solution was catched and 1 M NaOH
solution was augmented, white amorphous precipitates
of Zn(OH)2 were obtained. The needed value of
TiO2(P25) was augmented with fixed stirring to the
preparation of the hetero-structured TiO2(P25)-ZnO
photocatalysts with the Ti/zn molar proportions of 10:1
holding pH 7. The precipitates were stirred for 20 hr for
homogeneous mixing. The precipitates were filtered and
fication of nanocomposite, TiO2(P25)-ZnO with Fe3+
,
decreased the time of photoreaction so that, the time of
photoreaction for TiO2(P25)-ZnO was 5.5 h but, the time
was decreased to 4 hr with TiO2(P25)-ZnO/Fe3+. It is
remarkable that the best prior time was 6 hr.[40] Then, we
applied a magnetic field (5,000 G), whereas with a photo-
catalytic reaction. The time of photoreaction decreased to
2 hr with TiO2(P25)-ZnO/Fe3+. Also, selectivity of this
photoreaction with photocatalyst was considerable. The
photoreaction did stop at the stage of aldehyde and no acid
was produced.

4
FALLAHNEZHAD AND AMOOZADEH
FIGURE 1 The FE-SEM images
of (a, b) TiO2(P25)-ZnO and (c, d)
TiO2(P25)-ZnO/Fe3+. (D:Particle
Diagonal)
3.1 | Characterization of TiO2(P25)-ZnO/
of nanophotocatalyst TiO2(P25)-ZnO powder before sur-
face modification and TiO2(P25)-ZnO/Fe3+, after surface
rectification are shown in (Figure 2). Alike summit sever-
ities of the TiO2(P25)-ZnO and TiO2(P25)-ZnO/Fe3+ indi-
cate the consistency of the crystalline phase of nano-
TiO2(P25) pending preparation and surface rectification.
According to the XRD, the pattern of TiO2(P25) was
observed in all crystallograms. This shows that Fe3+ did
not dope into the crystal structure. Because in this case,
the XRD pattern of TiO2(P25) would have changed. Of
course, high energy (such as laser) is required for doping,
which is not provided (in our case) by mixing, blending,
or sonicating. Also, based on the literatures[41,42] in these
cases, ESR spectroscopy at 77 k had been reported that
(Fe3+) species were grafted onto the crystal surface as
Fe3+
3.1.1 | Field emission scanning electron
microscopy
Field emission scanning electron microscopy (FE-SEM) is a
famous and impressive gadget for perusal of the morphology
of NPs. Conforming to the FE-SEM images of TiO2(P25)-
ZnO (Figure 1a,b), the middle measure of TiO2(P25)-ZnO
NP is within 15–30 nm. The FE-SEM images of TiO2(P25)-
ZnO/Fe3+ (Figure 1c,d) show the middle measure of
TiO2(P25)-ZnO/Fe3+ NP is within 18–30 nm. Spherical mor-
phology can be proven of the FE-SEM images.
So, Scherrer equation calculation of photocatalyst
proved that these particles were at nanoscale:
0:3198*3:14
β ¼
¼ 0:005578
450
180
Ti -Zn/Fe3+
350
250
150
50
10
0:9*0:154
0:005578*Cos 12:67
D ¼ Kλ=ðβ*CosθÞ ¼
¼ 25:469 nm
Ti -Zn
10
TiO(P25)
2
3.1.2 | X-ray diffraction
15
35
55
75
-50
position(2ꢀ)
XRD was made on crystals to study the phase sincerity
and crystal structure of the nanophotocatalyst. The XRD
FIGURE 2 The XRD image of TiO2(P25), TiO2(P25)-ZnO, and
TiO2(P25)-ZnO/Fe3+

FALLAHNEZHAD AND AMOOZADEH
5
FIGURE 3 The EDX patterns of the (a) TiO2(P25)-ZnO and (b) TiO2(P25)-ZnO/Fe3+
surface modification on the TiO2(P25). Accordingly,
photo-activity of TiO2(P25)-ZnO/Fe3+ would gain growth
visible wavelength.
3.1.5 | Recyclability
Recycling experiments. As responsiveness, increase about
environmental concerns, industries are looking for ways
to remove their pollution. This is where the recycling and
reusability of catalysts matter. So, the catalyst is required
to have wonderful catalytic activity and selectivity. Also,
actual stability during the cycles. Accordingly, the reus-
ability of TiO2(P25)-ZnO/Fe3+ was examined. As shown
in Figure 5, the catalyst was capable of performing six
consecutive runs, without significant loss of activity.
FIGURE 4 Bandgap of TiO2-P25@ZnO/Fe3+
amorphous with distorted structure and Fe3+ was not
doped into the crystal structure of TiO2(P25).
3.1.3 | Energy-dispersive X-ray spectroscopy
3.2 | Evaluation of the photocatalytic
activity
EDX spectroscopy as a useful interpretive method was
done for the elemental analysis or chemical description
of NPs. The EDX analysis displays the entity of oxygen,
titanium, and Zinc in the nanophotocatalyst TiO2(P25)-
ZnO, (Figure 4a). The EDX analysis proved the presence
of Fe in TiO2(P25)-ZnO addition to NPs of TiO2(P25)-
ZnO as well (Figure 3b).
The photo-activity of photocatalyst was appraised by
photocatalytic oxidation of aryl alcohol beneath visible
light radiancy. The photocatalytic oxidation of aryl alco-
hol tests was done in a 15 ml Pyrex glass armed with a
water whirling jacket to rein the temperature of reac-
tions. Photo-reactor was fixed at room temperature dur-
ing the experiments. Dummy radiation into the Pyrex
reactor was prepared via 4 ꢃ 3 W blue light-evolving
diode lamps as the visible light origin. Photocatalyst was
suspended in 5 ml acetonitrile, benzyl alcohol (150 μmol)
as reductant, and sodium nitrate (150 μmol) was added
as oxidant. Results were monitored with UV spectros-
copy. Benzyl alcohol produced benzaldehyde. So, we
followed increasing the absorbance of UV-Vis spectra
related the benzaldehyde had produced, until the
3.1.4 | Diffuse reflectance spectroscopy
The band split energies of TiO2(P25)-ZnO were improved
with Fe3+ as shown in Figure 4. As shown in Figure 4,
the band gap energy of these photocatalysts, TiO2(P25)-
ZnO/Fe3+ is 2.9 eV. So, it is obvious that a significant
decrease on band split energy and red shift occur by

6
FALLAHNEZHAD AND AMOOZADEH
Yield
98
97
95
94
100
90
80
70
60
50
40
30
20
10
0
93
91
sixth
fifth
forth
third
second
first
FIGURE 6 The emission spectrum of the blue LED lamp and
UV–Vis absorption spectrum of TiO2(P25)-ZnO/Fe3+
FIGURE 5 Recyclability of TiO2(P25)-ZnO/Fe3+ on the
oxidation of benzyl alcohol to corresponding aldehydes
Then TiO2(P25)-ZnO/Fe3+ was used and the time
decreased to 4 hr.
absorbance was stoped. This means that benzaldehyde
production was completed. Of course, we monitored
benzaldehyde production with TLC monitoring. The
results were the same.
For comparison of the effect of surface modification
with Fe3+, at first, was done the photoreaction with
TiO2(P25)-ZnO. The time of photoreaction was 5.5 hr.
Then we designed photoreaction in the magnetic field.
Therefore, a magnetic field 5,000 G prepared. Two magnets
(4 cm ꢃ 4 cm ꢃ 5 cm) 5,000 G with 3 cm space between
them were fixed in two holes of Teflon fixture. The results
were considerable and remarkable. The time of photoreac-
tion decreased to 2.5 hr with TiO2(P25)-ZnO/Fe3+
.
TABLE 1 Reaction conditions: magnetic field 5,000 G, 3 ꢃ 4w LED blue lamp, sodium nitrate as a solvent
Entry
Reactant
Photocatalyst
Product
Time
1
TiO2(P25)-ZnO/Fe3+
120 min
2
TiO2(P25)-ZnO/Fe3+
120 min
3
4
TiO2(P25)-ZnO/Fe3+
TiO2(P25)-ZnO/Fe3+
120 min
20 hr
5
TiO2(P25)-ZnO/Fe3+
20 hr

FALLAHNEZHAD AND AMOOZADEH
7
TABLE 2 The comparison of reaction efficiency for different catalytic systems under the optimized conditions
Entry
Catalyst
Light source
Blue LED
Blue LED
Blue LED
Blue LED
Blue LED
Blue LED
Blue LED
Blue LED
Blue LED
Time (hr)
Yielda/Sel. (%)
100/100
99/99
1
1
2
3
4
5
6
7
8
TiO2(P25)-ZnO/Fe3+
n-TiO2-P25-SO3H[40]
2
7
n-TiO2-P25@ECH@WO3–SO3H[39]
n-TiO2-P25@ECH@WO3
n-TiO2-P25@ECH@ZnO
n-TiO2-P25@ECH@ZrO2–SO3H
n-TiO2-P25@ECH@ZrO2
TiO2-P25@TDI@DES[41]
TiO2/Ag[42]
6
99/99
6
20/99
6
10/99
6
55/99
6
Trace/99
70/78
19
4
88/88
Note: Reaction conditions: benzyl alcohol (150 μmol), NaNO3 (150 μmol), acetonitrile (5 ml), N2 atmosphere, room temperature, and 4 ꢃ 3 W LED irradiation.
aYield was determined by UV/Vis spectroscopy.
The results were very good. The efficacy of the mag-
netic field on the progress of photoreaction was interest-
ing and valuable. Then, our research group modified the
amount of photocatalyst in the reaction performed by
the magnetic field. Finally, the best amount of
photocatalyst (0.1 g) was determined. The results were
phenomenal. Modified amount of photocatalyst is differ-
ent in the attendance or absence of a magnetic field. The
emission spectrum of the blue LED lamp and UV–Vis
absorption spectrum of TiO2(P25)-ZnO/Fe3+ proved that
the photoreaction was completed for 120 min. Remark-
able that the best prior time was 6 hr. Figure 6.
respective aldehydes below visible light irradiation in
entity of nitrate ion. Also, for the first time, such photo-
reaction was performed in the presence of an external
magnetic field (5,000 G) and excellent yield and valuable
results were observed. Also, the time of the photoreac-
tion decreased up to 65% comparing the same conditions
without external applied magnetic field. The use of
external magnetic field is a green technology and clean
and has zero energy using up. This manner has some
valuable benefits such as useful easiness, great photo-
catalytic performance, moderate reaction situation, easy
work-up without purification with column chromatog-
raphy, environmentally friendly, and reusability of the
photocatalyst for several continuous cycles with stable
activity.
Finally, derivatives of benzyl alcohol were used as
reductant and following results were observed (Table 1).
3.3 | Comparison of the characteristic of
new synthesized catalyst with some
reported catalysts
ACKNOWLEDGMENTS
The authors appreciatively thank the faculty of the chem-
istry of Semnan University, for suffering this research.
In Table 2, entry 1 (new synthesized catalyst) was com-
pared with some reported photocatalyst.
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How to cite this article: S. Fallahnezhad,
A. Amoozadeh, J. Chin. Chem. Soc. 2021, 1. https://
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