Proceeding Paper
A Novel Synthetic Approach of Functionalised GO and CNT to
Nanocomposite Containing Active Nanostructured Fillers for
Classical Isocyanate Curing †
Lina Jadhav 1 , Rahul Patil 1 , Nikhil Borane 1 , Satyendra Mishra 1 , Ganapati D. Yadav 2 , Dipak B. Patil 3
and Vikas Patil 1,2, *
Citation: Jadhav, L.; Patil, R.; Borane,
N.; Mishra, S.; Yadav, G.D.; Patil, D.B.;
Patil, V. A Novel Synthetic Approach
of Functionalised GO and CNT to
Nanocomposite Containing Active
Nanostructured Fillers for Classical
Isocyanate Curing. Chem. Proc. 2022,
8, 33. https://doi.org/10.3390/
ecsoc-25-11679
Academic Editor: Julio A. Seijas
Published: 13 November 2021
Publisher’s Note: MDPI stays neutral
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Copyright: © 2021 by the authors.
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This article is an open access article
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Attribution (CC BY) license (https://
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4.0/).
Chem. Proc. 2022, 8, 33. https://doi.org/10.3390/ecsoc-25-11679
1 University Institute of Chemical Technology, Kavayitri Bahinabai Choudhari North Maharashtra University,
Jalgaon 425001, India; lina.jadhav345@gmail.com (L.J.); rahul92ppatil@gmail.com (R.P.);
nikhilborane1990@gmail.com (N.B.); profsm@rediffmail.com (S.M.)
2 Institute of Chemical Technology, Mumbai 400019, India; gdyadav@yahoo.com
3 Departamento de Química, División de Ciencias Naturales y Exactas, Campus Guanajuato,
Universidad de Guanajuato, Noria Alta S/N, Guanajuato 36050, Mexico; patildip98@gmail.com
* Correspondence: vikasudct@gmail.com
† Presented at the 25th International Electronic Conference on Synthetic Organic Chemistry,
15–30 November 2021; Available online: https://ecsoc-25.sciforum.net/.
Abstract: A novel synthetic method has been developed by utilizing the chemical reactivity of
functionalized graphene and CNT with a covalent combination of chemically diverse GO/FCNT
and toluene diisocyanate, thereby yielding a synergistic polymer nanocomposite. Comprehensive
composite material has simultaneous covalent, as well as π-π, interactions confirming sp2-hybridized
frameworks of graphene oxide and MWCNTs by Raman absorption spectra at 1345 and 1590 cm−1 of
D and G bands, respectively. Toluene diisocyanate and GO/FCNT inspired polymeric formulation
was obtained by the classical curing reaction initiated by ultrasound sonication. This method allowed
50 wt.% doping of GO/FCNT without segregation and ensured good adhesion to the law steel surface.
The large surface area and morphological character of GO and FCNT by SEM and TEM ensure stable
and dispersed integrated molecules. This has advantages over high-temperature and hazardous
curing reaction, and overcomes the problem of graphene exfoliation. It also does not allow CNT
slipping within the bundle, which can cause falling apart at higher concentration.
Keywords: graphene; CNT; isocyanate; curing; filler; nanostructured
1. Introduction
Complimentary properties of organic and inorganic materials are combined to gener-
ate a new composite material, generating new hybrid composite materials. The new hybrid
composite material has combined properties of both organic and inorganic compounds [1].
Before compositing two chemically distinct species, synergy was installed by functionali-
sation of an essential component [2]. Functionalisation permits chemical response, which
improves mechanical, thermal, electrical, UV resistance, and abrasion properties in hybrid
organic-inorganic materials [3,4]. In polymer nano-composite, lack of covalent interac-
tions allows exfoliation of filler material into the complex matrix. This problem is further
overcome by chemical functionalisation and the subsequent covalent combination of nanos-
tructure filler into the polymeric matrix [5]. The isocyanate is a functional species ready
to be combined with chemically modified filler material, thereby enhancing the intrinsic
properties of the final composite material for application. Consequently, the final composite
material has reduced hydrophilic properties, due to the utilization of hydroxyl and acid
functionality of the filler, and forms new hydrophobic amide and carbamate ester linkages.
As a result of this, it is no longer exfoliated into the solvent, helping in the stably dispersed
https://www.mdpi.com/journal/chemproc
Chem. Proc. 2022, 8, 33 2 of 9

constructive formulation. Segregation has been observed at very low concentration of

0.1 vol% of graphene as filler in polystyrene. It was evidenced that there is no constructive
attraction between filler and polymer. Physical laying of filler into the polymer matrix
immediately segregates at high concentration [6,7].
Owing to the strong and inbuilt sustainable properties of CNT it is able to retain
five to ten times more load than steel. Compared to steel, CNT inclusion creates magical
properties due to the active large surface, 1/6 weight, 50–100 G Pa tensile strength and
1–2 T Pa modulus [8–11]. Next generation performing materials have multifunctionality
due to CNT and graphene, with unique mechanical, thermal, and surface properties. CNT
and graphene polymer nanocomposite coating binds synergy of film thickness, interparticle
spacing of the filler and thermomechanical properties [12]. Further 2 wt.% SWNTs added to
the coating results in 125% thermal conductivity and 3.5-factor increase in Vickers hardness.
To date, the use of CNTs and graphene nanocomposites has been limited by challenges
in processing, dispersion, and their prohibitively high cost. Ajayan et al. demonstrated
the preparation of epoxy composite by dispersing multiwall nanotubes in the epoxy under
ultrasonic force [13]. Higher concentrations of more than 5% nanotubes in composite
slip within the bundle and fall apart, which is responsible for poor load transfer within
the cured composite. This was supported by Raman spectra, tension and compression
analysis [14]. Sandler et al. tried to improve dispersion of SWNTs by ultrasonic application
and intense stirring. A slight improvement was observed in the configuration of nanotubes
but it still failed on the millimeter scale [15]. Irrespective of the sliding of the SWNTs,
into the ropes, continuous increase in Young’s modulus was observed with respect to
increasing concentration. Improper configuration slides SWNTs into the rope, and bending
of the rope decreases mechanical strength [16]. Furthermore, surfactants were also used to
improve the dispersion of nanotubes in epoxy. This retained the mechanical strength of
the composition [17]. Surfactant and ultrasonically dispersed epoxy-nanotube composition
appear to be finely dispersed, but microscopic. Analysis found there to be inhomogeneous
dispersion in the composition [18]. To overcome this, an integrated system was developed
upon functionalization of GO/FCNT, and exploited to induce curing of diisocyanate. The
composite was used as a corrosion resistive coating on low alloy steel [19,20]. Loading
of 50 wt.% filler achieved stable, mechanically strong and highly dispersed FCNT/GO
isocyanate composite for surface coating [21,22].

2. Experimental
2.1. Materials and Methods
Single-walled carbon nano tubes were purchased from Alfa Aesar. Graphene and
toluene diisocyanate precursor were purchased from Sigma Aldrich. Anhydrous THF
was used as a solvent in this process and functionalization was done by using NaNO3 ,
KMnO4, and H2 SO4 in deionized water. Low alloy steel for coating was used from a local
supplier in Mumbai, India. Functionalization of CNT and Graphene was performed by the
Hummer’s method [23]. Further composites were prepared and obtained fine dispersion.
Surface coating of nano-composite on low-alloy steel was performed by a simple bar coating
method. Formulations containing 50, 25, 10, 5 wt.% of filler content of average precision
film thickness were obtained.

2.2. Characterization of Structure and Surface Morphology

IRRA (infrared reflection absorption) spectra were utilized for the characterisation
of functional modification in CNT and graphene. IRRA was carried out by a Perkin
Elmer 100 FT-IR spectrophotometer with Olympus BX51 microscope attachment. Raman
spectroscopy was performed by Horiba Jobin Yvon Labram HR system with 514.5 nm laser
excitation. The surface morphology of composites was investigated by scanning electron
microscopy (SEM) on a Hitachi SU-70 instruments, operated at accelerating voltage of 20 kV.
Transmission electron microscopy (TEM) was used for dispersion study of the composite
by a JEOL-2010 instrument operated at 200 kV and 100 mA equipment. Film thickness was
Chem. Proc. 2021, 3, x FOR PEER REVIEW 3 of 9

Chem. Proc. 2022, 8, 33 electron microscopy (SEM) on a Hitachi SU-70 instruments, operated at accelerating 3 of 9
voltage of 20 kV. Transmission electron microscopy (TEM) was used for dispersion study
of the composite by a JEOL-2010 instrument operated at 200 kV and 100 mA equipment.
Film thickness
measured by shinwas measured
equipment, by shinThe
Mumbai. equipment, Mumbai.
rate of corrosion wasThe rate of
detected bycorrosion was
deep method
detected by deep method in 3.5%
in 3.5% NaCl solution for 2160 h. NaCl solution for 2160 h.

3.3. Results
ResultsandandDiscussion
Discussion
3.1.
3.1.Functionalisation,
Functionalisation,Dispersion
DispersionofofFCNT/GO
FCNT/GOand andCuring
CuringofofIsocyanate
Isocyanate
The
Theoverall
overallstrategy
strategyshown
shownin inFigure
Figure11depicts
depictsdispersion
dispersionof ofactive
activecarbon
carbonmaterial
material
in
inisocyanate.
isocyanate. The
The accessible
accessible functional
functional groups
groups on
on the
thesurface
surfaceofofcarbon
carbonmaterial
materialinduce
induce
cross-linking
cross-linkingtoto di-isocyanate.
di-isocyanate.Initial reports
Initial on a high
reports on adegree
high of functionalisation,
degree followed
of functionalisation,
by fluorination,
followed were employed
by fluorination, wereto obtain
employed largeto
dispersion and mechanical
obtain large dispersionstrength in epoxy
and mechanical
nanocomposite [24]. Thereby acid and fluorine covalently bind with
strength in epoxy nanocomposite [24]. Thereby acid and fluorine covalently bind active epoxy. An acid
with
functional group readily forms ester while diamine becomes an active
active epoxy. An acid functional group readily forms ester while diamine becomes spacer and readily
an
replaces side wall
active spacer andfluorine
readily [24,25].
replacesHere
side toluene di-isocyanate
wall fluorine [24,25]. was
Hereemployed as an active
toluene di-isocyanate
crosslinking
was employed bifunctional
as an activespacer betweenbifunctional
crosslinking two nano-materials. The induced
spacer between cross-linking
two nano-materials.
was
The induced cross-linking was materialised by excessive probe sonication. Theparticle
materialised by excessive probe sonication. The overall challenge of nano overall
segregation
challenge ofand nano constant
particledispersion
segregation inand
a solvent wasdispersion
constant overcomein bya reactive sites,overcome
solvent was both on
the
by nanomaterial
reactive sites, and
boththeon diisocyanate
the nanomaterialprecursor.
and the diisocyanate precursor.

Figure1.1.Schematic
Figure of graphene
Schematic CNT functionalization,
of graphene compositecomposite
CNT functionalization, formation with toluene with
formation diisocyanate.
toluene
diisocyanate.
Structural changes in the composite were noted and analyzed by characteristic IRRA
peaks.Structural
GO@isocyanate
changesshowed a specific broad
in the composite absorption
were noted peak at 3407
and analyzed cm−1 (FigureIRRA
by characteristic 2b).
While
peaks. GO@isocyanate showed a specific broad absorption peak at 3407 cm−1 (Figure 2a).
CNT@isocyanate showed relatively small absorbance in the same region (Figure 2b).
Separate −1 and 3528 cm−1 arose in toluene diisocyanate and confirmed a
peaks at 3298 cmshowed
While CNT@isocyanate relatively small absorbance in the same region (Figure
urethane link peaks
2a). Separate N=C (Figure 2a).−1 Broad
at 3298 cm and 3528absorbance atin
cm−1 arose 3400 cm−diisocyanate
toluene
1 was absent completely in
and confirmed
the pure toluene
a urethane di-isocyanate.
link N=C (Figure 2a).InBroad
pure toluene di-isocyanate,
absorbance at 3400 cm C-H
−1 wasstretching
absent absorption
completely in
spectra were observed at 2987 cm −1 and further strongly recognised in both composites
the pure toluene di-isocyanate. In pure toluene di-isocyanate, C-H stretching absorption
of GO/FCNT@isocyanate, due to the influence of non-stacking with the surface, and
non-hydrogen bonding. Sharp absorption bands were observed in the fingerprint re-
gion, whereas, for pure toluene di-isocyanate, a bundle of peaks was observed in this
region. Peaks were commonly observed at close to 1377 cm−1 in all spectra, explaining
 GO/FCNT@isocyanate, due to the influence of non-stacking with the surface, and
hydrogen bonding. Sharp absorption bands were observed in the fingerprint r
whereas, for pure toluene di-isocyanate, a bundle of peaks was observed in this r
Chem. Proc. 2022, 8, 33
Peaks were commonly observed at close to 1377 cm−1 in all spectra, explaining 4 of 9
the
group of toluene diisocyanate carried forward in composite formation. The aro
nature of toluene diisocyanate compound was confirmed by absorption peaks at 117
and
the1534
–CH3cm −1. The IR absorption spectra at 1130 cm−1 for GO@isocyanate, and 116
group of toluene diisocyanate carried forward in composite formation. The
foraromatic
FCNT@isocyanate,
nature of toluenecorresponded to the C-C-O
diisocyanate compound ether linkage.
was confirmed Absorption
by absorption peaks at at 934
1170 cm −1 and 1534 cm−1 . The IR absorption spectra at 1130 cm−1 for GO@isocyanate, and
for the GO@isocyanate and 927 cm for FCNT@isocyanateis C-H stretch vibratio
−1
1164 cm−1 for FCNT@isocyanate, corresponded to the C-C-O ether linkage. Absorption
methylene were attributed to at least one aliphatic fragment or center. The broad p
at 934 cm−1 for the GO@isocyanate and 927 cm−1 for FCNT@isocyanateis C-H stretch
2291 cm was
−1
vibrations observed
of methylene wereforattributed
the toluene
to at diisocyanate, which
least one aliphatic is a or
fragment specific
center. isocyanate
The
confirmation
broad peak at 2291 −
further, 1
cm was which completely
observed vanished
for the toluene in which
diisocyanate, both isGO@isocyanate
a specific
isocyanate bond confirmation
FCNT@isocyanate composites.further, which completely
It confirmed that vanished in bothofGO@isocyanate
the purpose curing the isocyan
and FCNT@isocyanate composites. It confirmed that the purpose of curing the isocyanate
nano-imbedded particles, like FCNT and GO, was successfully achieved. Signi
by nano-imbedded particles, like FCNT and GO, was successfully achieved. Significant
change
changewas observedin in
was observed thethe
IRRAIRRA absorption
absorption spectraspectra of theincorporated
of the surface, surface, incorporated
with
active
activefunctional nanoparticles
functional nanoparticles and and only isocyanate
only isocyanate as such. as such.

IRRA spectra
Figure2.2.IRRA
Figure spectra(a)(a)
toluene di-isocyanate
toluene withoutwithout
di-isocyanate doping on steel surface
doping (b) GO@isocyanate
on steel surface (b) GO@isoc
50 wt.% (c) FCNT@isocyanate 50
50 wt.% (c) FCNT@isocyanate 50 wt.%.wt.%.

3.2. Interface Chemistry between GO/FCNT@isocyanatematrix

3.2. Interface Chemistry
Kozlowski between
and Jones GO/FCNT@isocyanatematrix
et al. suggested synergy in a two phasic system was due to
interfacial physical
Kozlowski and and covalent
π-πJones chemical compatibility
et al. suggested synergy in[26,27].
a two The interfaces
phasic system of was d
GO/FCNT become more compatible by simultaneously strong covalent and π-π interaction
interfacial physical π-π and covalent chemical compatibility [26,27]. The interfa
with the diisocyanate host. Few covalently unbounded GO/FCNT interfaces have strong
GO/FCNT become
π-π interaction more
and remain compatible
dispersed withoutby simultaneously
agglomeration (Figure 1).strong covalent and
In situ reaction
interaction with the diisocyanate
helps in non-agglomeration host. Few
and phase separation covalently
of the polymer andunbounded GO/FCNT inte
GO/FCNT. Hydroxyl
have strong ᴫ-ᴫ interaction and remain dispersed without agglomeration
and carboxylic acid functional groups grafted onto the GO/FCNT provide a way for in situ(Figure
chemical integration of the GO/FCNT into the isocyanate system.
situ reaction helps in non-agglomeration and phase separation of the polyme
As mentioned previously, simultaneously strong covalent and π-π interactions are
GO/FCNT.
involved inHydroxyl andinterfaces
facilitating the carboxylic acidthe
between functional groups
nanostructured grafted
filler onto the GO/F
and isocyanate
provide
matrix. aElectron
way formicroscopy
in situ chemical integration fine
further corroborated of the GO/FCNT
dispersion of theinto the isocyanate sy
nanostructure
As mentioned
carbonaceous materialpreviously, simultaneously
in the isocyanate. strong covalent
The properly dispersed and π-πover
GO and MWCNTs interactio
isocyanate in the coating is shown by SEM images in Figure 3 on low-alloy steel.
involved in facilitating the interfaces between the nanostructured filler and isocy The sample
was cryo-fractured in liquid nitrogen and a cross section SEM image was captured, which
matrix. Electron microscopy further corroborated fine dispersion of the nanostru
indicates well dispersed oxidised MWCNTs and GO. There was no clue for the segregation
carbonaceous
of MWCNTs and material in the
GO in SEM. isocyanate.caps
Hemispherical Theofproperly
the MWCNTsdispersed GO andThe
were observed. MWCNT
isocyanate
evidence ofin the coating
covering is shown
of the polymeric by SEM
matrix images in
to nanomaterial wasFigure 3 on low-alloy
also observed in SEM. stee
Figure 3a depicts MWCNT@isocyanate, while GO@Isocyanate is shown
sample was cryo-fractured in liquid nitrogen and a cross section SEM image was capin Figure 3a. The
which indicates well dispersed oxidised MWCNTs and GO. There was no clue f
 observed in SEM. Figure 3a depicts MWCNT@isocyanate, while GO@Isocyanate
in Figure 3a. The swelling of the polymeric matrix observed with nanomateria
rough surface were observed in the coating. Similarly, Figure 3d shows graphe
sheets embedded within the isocyanate matrix. The carbon nanomaterial on is
Chem. Proc. 2022, 8, 33 5 of 9
was evaluated with TEM images. Figure 4a,b show complete dispersion of the s
GO sheet and oxidised nanotubes in isocyanate. In Figure 4b’s TEM of high re
complete
swelling covering
of the polymeric was observed
matrix observed i.e.,
withwrapping of the
nanomaterials andpolymeric matrix
a rough surface were to the M
indicating
observed in thesimilar observation
coating. of graphene
Similarly, Figure 3d shows oxide
graphenewrapping in isocyanate
oxide sheets embedded matrix
within the isocyanate matrix. The carbon nanomaterial on
4c). Despite extensive functionalisation, the crystalline order of some isocyanate was evaluated
graphene o
with TEM images. Figure 4a,b show complete dispersion of the separated GO sheet and
preserved, shown in Figure 4d in selected area electron diffraction pattern.
oxidised nanotubes in isocyanate. In Figure 4b’s TEM of high resolution, complete covering
hybridized
was frameworks
observed i.e., wrapping ofof the graphene
polymericoxidematrix and
to theMWCNTs were confirmed
MWCNTs, indicating similar by ab
in Raman spectra at 1345 and 1590 cm −1 of D and G bands, respectively
observation of graphene oxide wrapping in isocyanate matrix (Figure 4c). Despite extensive (Figure 5
functionalisation,
noted that the the crystalline
positions order
of the DofandsomeG graphene
bands are oxide wasdisturbed
finely preserved, while
shown composit
in
Figure 4d in selected area electron diffraction pattern. The sp2-hybridized frameworks of
the isocyanate matrix. The intensity of the D and G bands are much more affecte
graphene oxide and MWCNTs were confirmed by absorption in Raman spectra at 1345 and
andcmafter
1590 −1 ofcompositing.
D and G bands, In the isocyanate
respectively (Figure 5).matrix, the intensity
It was noted of the of
that the positions G theband was
Ddeclined
and G bands rather than in
are finely MWNTs
disturbed alone.
while Furtherwith
compositing the Dtheband becomes
isocyanate comparably
matrix. The i
with the G band for graphene oxide in isocyanate, and comparable increase in int
intensity of the D and G bands are much more affected before and after compositing. In the
isocyanate
the G band matrix,
forthe intensity ofwas
MWCNTs the G band was slightly
observed. declined after
As expected, ratherfunctionalisation,
than in MWNTs int
alone. Further the D band becomes comparably intensive with the G band for graphene
the 2D band no significant change in the MWCNTs was
oxide in isocyanate, and comparable increase in intensity of the G band for MWCNTs
observed, due to the di
of observed.
was p-conjugation arising
As expected, afterfrom the doubleintensity
functionalisation, bond resonance
of the 2D bandprocess, which was
no significant
promising
change for graphene
in the MWCNTs oxide. due
was observed, Thetocompatibility
the disruption ofofp-conjugation
nanostructure filler
arising fromand ho
the double bond resonance process, which was no more promising
was due to the dual modality of the covalent bond and π-π interactions, for graphene oxide. The illus
compatibility of nanostructure filler and host matrix was due to the dual modality of the
Figures 1, 3 and 5. There are other ways to have compatibility in nanostructure f
covalent bond and π-π interactions, illustrated in Figures 1, 3 and 5. There are other ways
toa have
polymeric matrix.
compatibility To the best of
in nanostructure ourand
filler knowledge,
a polymericand with
matrix. To reference
the best of toourliteratu
the sole example for coating application using graphene oxide and
knowledge, and with reference to literature, this is the sole example for coating application oxidised MW
using graphene
curing agents. oxide and oxidised MWCNTs as curing agents.

Figure
Figure 3. Cross
3. Cross section
section SEM images
SEM images of GO@isocyanate
of (a,b) for (a,b) for GO@isocyanate 50 FCNT@isocyanate
50 wt.% (c,d) for wt.% (c,d) for FCNT@i
5050
wt.%.
wt.%.
Chem. Proc. 2021, 3, x FOR PEER REVIEW 6 of 9
Chem. Proc. 2021, 3, x FOR PEER REVIEW 6 of 9
Chem. Proc. 2022, 8, 33 6 of 9

Figure 4. TEM (a,b) for FCNT@isocyanate 50 wt.% (c) for GO@isocyanate 50 wt.% and (d) image is
selected
Figurearea
Figure 4. electron
4. TEM
TEM (a,b)
(a,b)diffraction
for
for (SAED) 50
FCNT@isocyanate
FCNT@isocyanatepattern
wt.% acquired
(c)
50 wt.% for for for the 5050 wt.%
(c)GO@isocyanate wt.%
GO@isocyanate graphene-
50and (d) and
wt.% image
(d)is
oxide@iscocyanate
selected area composite.
electron diffraction (SAED) pattern acquired for the 50 wt.% graphene-
image is selected area electron diffraction (SAED) pattern acquired for the 50 wt.% graphene-
oxide@iscocyanatecomposite.
oxide@iscocyanate composite.

Figure 5. Raman spectra of pure GO and FCNT and isocyanate composite with GO and FCNT.
Figure 5. Raman spectra of pure GO and FCNT and isocyanate composite with GO and FCNT.
Figure
3.3. 5. Raman
Corrosion spectra of
Inhibition pure GO
Endowed byand FCNT and isocyanate
Nanocomposite Coatings composite with GO and FCNT.
3.3. Corrosion Inhibition Endowed by Nanocomposite Coatings
The digital photograph in Figure 6 depicts exposer of 50, 25, 10, and 5 wt.% GO/
3.3.
The Corrosion
FCNT@isocyanate Inhibition
digital photograph Endowed
in 3.5% in
NaCl by
Figure Nanocomposite
6 depicts
solution Coatings
exposer
for 2160 of 50,
h. Strong 25, 10, to
resistance and 5 wt.%was
corrosion
GO/FCNT@isocyanate
The digital in 3.5%
photographNaCl solution
in Figure for
6 2160 h.
depicts Strong resistance
exposer of 50, to
25,corrosion
10, and
observed at higher loading, i.e., 25 and 50 wt.%, while at 5 and 10 wt.% significant corrosion was
5 wt.%
observed at higher
GO/FCNT@isocyanate
was loading,
observed after longin i.e., 25
3.5% NaCl
exposer and 50 wt.%,
solution
to salt while at 5 and 10 wt.% significant
for 2160 h. Strong resistance to corrosion was
solution.
corrosion was observed
observed at higher after long i.e.,
loading, exposer to salt
25 and 50 solution.
wt.%, while at 5 and 10 wt.% significant
corrosion was observed after long exposer to salt solution.
Chem. Proc. 2021, 3, x FOR PEER REVIEW 7 of 9
Chem. Proc. 2022, 8, 33 7 of 9

Figure 6. Corrosion measurement

Figure in salt
6. Corrosion water (NaCl
measurement 3.5%)
in salt of GO@isocyanateand
water FCNT@isocyanate).
(NaCl 3.5%) of GO@isocyanateand FCNT@isocyanate).

3.4. Mechanical Properties

Mechanical properties
Mechanical properties ofofisocyanate
isocyanatecomposites
composites have beenbeen
have tested for impact
tested resis-
for impact
tance, pencil
resistance, hardness,
pencil scratch
hardness, hardness,
scratch adhesion,
hardness, cracking
adhesion, resistance
cracking and and
resistance flexibility. The
flexibility.
results
The are summarized
results are summarizedin Table 1. It shows
in Table goodgood
1. It shows resistance to cracking
resistance (flexibility).
to cracking The
(flexibility).
pencil
The hardness
pencil is 5Hisfor
hardness 5Hallfor
theall
coating, except except
the coating, 5 wt.%5GO/FCNT@isocyanate.
wt.% GO/FCNT@isocyanate. Simi-
larly, adhesion
Similarly, of coating
adhesion was fairly
of coating goodgood
was fairly at meeting the standards.
at meeting Adhesion
the standards. of 5 wt.%
Adhesion of 5
GO/FCNT@isocyanate was 4B, while the rest of the coating samples had
wt.% GO/FCNT@isocyanate was 4B, while the rest of the coating samples had 5B. Further, 5B. Further, all
the samples were found to have good resistance over scratch hardness. The
all the samples were found to have good resistance over scratch hardness. The average average scratch
hardness
scratch was 2.9 was
hardness Kg. 2.9 Kg.

Mechanical
Table 1.properties
Table 1. Mechanical of properties of polymer
polymer films films with
with various %wt various %wt of GO/FCNT@isocyanate.
of GO/FCNT@isocyanate.

%Weight
%Weight of GO/FCNT@isocyanate
of GO/FCNT@isocyanate
GO@isocyanateFCNT@isocyanate
GO@isocyanateFCNT@isocyanate
5 10 25 50 5 10 25 50
5 10 25 50 5 10 25 50
Impact
Impact Resistance
Resistance Pass PassPass Pass Pass Pass Pass Pass Pass Pass PassPass Pass
Pass Pass
Pass
Pencil
Pencil hardness
hardness 4H 4H 5H 5H 5H 5H 5H 5H 5H 5H 5H 5H 5H5H 5H
5H
Flexibility
Flexibility Pass PassPass Pass Pass Pass Pass Pass Pass Pass PassPass Pass
Pass Pass
Pass
Adhesion 3B
Adhesion 3B 5B 5B 5B 5B 5B
5B 5B 5B 5B 5B 5B
5B 5B
5B
Scratch Hardness (Kg) 2.8 2.9 3.0 3.0 2.8 2.9 2.9 3.0
Scratch Hardness (Kg) 2.8 2.9 3.0 3.0 2.8 2.9 2.9 3.0

4. Conclusions
4. Conclusions
The concept
The concept of
of aa chemical
chemical reaction
reaction between
between twotwo phase
phase materials
materials GO/FCNT
GO/FCNT with with
isocyanate was
isocyanate was executed
executed and
and utilized
utilized as
as aa corrosion
corrosion resistive
resistive coating
coating material.
material. Chemically
Chemically
activated carbonaceous nanomaterial was integrated into the core structurepolymer
activated carbonaceous nanomaterial was integrated into the core structure of the of the
matrix, united
polymer by united
matrix, covalent,byascovalent,
well as π-π, chemical
as well combination.
as π-π, It allows loading
chemical combination. about
It allows
50 wt.% of nanofiller into polymer matrix to deliver better surface and mechanical
loading about 50 wt.% of nanofiller into polymer matrix to deliver better surface and proper-
ties. The general
mechanical problem
properties. at high
The loading
general of graphene
problem at high exfoliation
loading of and sleeping
graphene of nanotubes
exfoliation and
was overcome by the covalent bonding approach and formed a stable
sleeping of nanotubes was overcome by the covalent bonding approach and formed a dispersion.
stable dispersion.
Author Contributions: V.P. is contributed for conceptualization, L.J. for experimental part, R.P. and
N.B. for methodology, G.D.Y. and S.M. for supervision and D.B.P. for original draft preparation. All
Author Contributions: V.P. is contributed for conceptualization, L.J. for experimental part, R.P. and
authors have read and agreed to the published version of the manuscript.
N.B. for methodology, G.D.Y. and S.M. for supervision and D.B.P. for original draft preparation. All
authors
Funding: have
Thisread and agreed
research to no
received theexternal
published version of the manuscript.
funding.
Funding: ThisReview
Institutional research received
Board no external
Statement: funding. part does not involve human or animal study.
Experimental
Institutional Review
Informed Consent Board Statement:
Statement: Experimental part does not involve human or animal study.
Not Applicable.
Informed ConsentStatement:
Data Availability Statement:Not
Notapplicable.
Applicable.
Data Availability Statement: Not applicable.
Chem. Proc. 2022, 8, 33 8 of 9

Acknowledgments: Vikas Patil is thankful to UGC for Faculty Recharge Program and Start Up grant
and INDO-US Science and Technology Forum for Post-Doctoral Visiting Fellowship. We thank group
of Sarabjit Banerjee and Robert Dennis for analytical support at University at Buffalo. Vikas Patil
is thankful to DST India for Waste Management Technology (WMT) project of Technology Transfer
Division (TTD) (DST/TDT/WMT/Agwaste/2021/09(G) & (C). Lina Jadhav is thankful to MHRD
TEQIP-III for financial support.
Conflicts of Interest: We confirm that there are no conflict of interest associated with this publica-
tion and there has been no significant financial support for this work that could have influenced
its outcome.

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