Waste Management 100 (2019) 296–305

Contents lists available at ScienceDirect

Waste Management
journal homepage: www.elsevier.com/locate/wasman

Applications of functionalized polyethylene terephthalate aerogels from

plastic bottle waste
Duyen Khac Le a,1, Ryan I.H. Leung a,1, Alan S.R. Er a, Xiwen Zhang b, Xiang J. Tay a, Quoc Ba Thai a,
Nhan Phan-Thien a, Hai M. Duong a,c,⇑
a
Department of Mechanical Engineering, National University of Singapore, 9 Engineering Drive 1, Singapore 117576, Singapore
b
Singapore Institute of Manufacturing Technology, A*STAR, 73 Nanyang Drive, Singapore 637662, Singapore
c
Ton Duc Thang University, 19 Nguyen Huu Tho Street, Ho Chi Minh City 758307, Vietnam

a r t i c l e i n f o a b s t r a c t

Article history: Millions of tons of plastic are produced annually, but less than 10% are reported to be recycled. This work
Received 23 May 2019 sets out to transform environmental plastic (polyethylene terephthalate – PET) waste into aerogels for
Revised 14 August 2019 high-value engineering applications, primarily to enhance the monetary incentive in recycling plastics.
Accepted 22 September 2019
Coating techniques, using silicone ceramic (SCC) and (3-aminopropyl)triethoxysilane (APS, or APTES)
Available online 27 September 2019
solutions, are successfully devised to enhance the thermal stability and CO2 adsorption capability of
rPET aerogel. The rPET/SCC aerogel exhibits improved thermal stability (up to 600 °C), enhanced thermal
Keywords:
insulation (thermal conductivity Kavg = [31.8–34.9] mW/m
K), hydrophobic characteristics (up to 144.7°
Plastic aerogel
Adsorption
in contact angle) and enhanced rigidity (Young modulus Eavg = [4.5–124.8] kPa), while maintaining an
Flame retardant ultra-low density (qa = [14–62] g/cm3) and a high porosity (Uavg = [95.6–99.0]%). Moreover, the amine-
Thermal property functionalised rPET aerogel achieves a CO2 adsorption capacity of up to 0.44 mmol CO2/g, superior to sev-
Polyethylene terephthalate eral commercial physio-sorbents. These promising results obtained demonstrate that the rPET aerogel is
a versatile material suitable for a wide variety of high-value engineering applications, including thermal
insulation and direct CO2 capture applications.
Ó 2019 Elsevier Ltd. All rights reserved.

1. Introduction
Polyethylene terephthalate (PET) bottle was patented in 1973
(Wyeth and Roseveare, 1973), and has been popularly used for
the production of disposable soft drink bottles since the 1980s. In
1987, more than 700 million pounds of PET were consumed in
their production. Due to the diverse applications in an extensive
range of consumer products, a high volume of PET waste is gener-
ated annual. With 348 million tons (Statista, 2019) of plastic pro-
duced globally in 2017 and only 9% of them are recycled (Geyer
et al., 2017), there is an urgent concern for the mounting post-
consumer plastics as most plastics are non-biodegradable
(Jankauskaite et al., 2008). PET is no exception, as the presence of
the aromatic ring in its chemical structure makes it extremely
stable and therefore, insensitive to hydrolytic degradation
(Muller et al., 2001). Current strategies adopted to manage plastic
waste includes landfills, recycling, and combustion (Subramanian,
2000). Landfills are commonly practised worldwide, but the prac-
⇑ Corresponding author.
E-mail address: mpedhm@nus.edu.sg (H.M. Duong).
1
Equal contribution.
tice is not sustainable as available landfill sites are running out,
and notably, the resultant landfill leachate causes pollution and
grave environmental implications (Salem et al., 2008). Plastic solid
waste is also incinerated to generate energy. However, the emis-
sion of air pollutants-such as carbon dioxide (CO2), nitrous oxides
(NOx), and sulphur oxides (SOx)-from often incomplete combustion
processes poses health and safety concerns (Al-Salem et al., 2009).
Recycling of plastic waste effectively reduces waste volume, but
recycling levels worldwide remain lacklustre due to difficulties in
processing post-consumer plastic and the lack of monetary incen-
tives (Nikles and Farahat, 2005).
The primary two methods employed to obtain recycled PET
(rPET) from the post-consumer PET are mechanical recycling and
chemical recycling (Dutt and Soni, 2013). Mechanical recycling
involves the physical sorting of plastics, according to type and col-
our, and the removal of contaminants to obtain clean plastic pallets
ready to be reprocessed into various forms (Awaja and Pavel,
2005). In chemical recycling, PET is de-polymerised to recover syn-
thesis monomers, which could be re-polymerised to produce virgin
PET (Awaja and Pavel, 2005; Dutt and Soni, 2013). rPET is generally
unsuitable for food packaging, as the temperatures associated with
the recycling process is below the level necessary for effective ster-

https://doi.org/10.1016/j.wasman.2019.09.031
0956-053X/Ó 2019 Elsevier Ltd. All rights reserved.
 D.K. Le et al. / Waste Management 100 (2019) 296–305
ilization. As such, rPET is commonly used to produce lower grade
plastic products such as non-food plastic containers and synthetic
fibres (Dutt and Soni, 2013). Notably, the use of rPET fibres to rein-
force concrete is an example of a high-value application of rPET
(Siddique et al., 2008). With more high-value products derived
from PET waste, there would be a more significant commercial
influence to recycle PET. Besides, it would be better to convert
the low plastic recycling levels globally.
Excessive greenhouse gas emission has been recognized as a
critical contributor towards the rising global mean temperature
and consequently the rising mean sea levels; it is projected that
based on existing trends, by the end of the 21st century, the global
mean temperature and sea level would increase by up to 2.5 °C and
[40–63] cm respectively, as compared to beginning of the 20th
century (United Nations, n.d.). In response to the dire environmen-
tal situation, the Paris Agreement was enacted in 2015 with the
ambitious aim to maintain the global temperature rise below
1.5 °C. Noteworthily, the Paris Agreement stresses the importance
of technology in global efforts to reduce greenhouse gas emission
(United Nations, 2015). Between 2014 and 2017, global energy-
related CO2 emissions remained relatively flat (1% increase) despite
growth in the global economy (3%); the observed reduction in CO2
intensity could be attributed to the rapid expansion of the renew-
able energy technologies (International Energy Agency, 2017a).
However, carbon-based energy sources remain the primary source
of energy supply (81.4% (International Energy Agency, 2017b)) due
to its accessibility and relatively lower cost; where the global
energy-related CO2 emission is projected to increase 10% from
32.5 gigatons (International Energy Agency, 2018) in 2017 to
35.7 gigatons (International Energy Agency, 2017c) by 2040.
CO2 capture from flue gas emitted by power stations offers a
solution to reduce the atmospheric CO2 concentration (Sanz-
Pérez et al., 2016). The adsorbed CO2, in turn, could be either used
as intermediates to synthesis high-value products—such as hydro-
gen fuel (Nikulshina et al., 2006) and salicylic acid (Gruber, 2001)—
or fed to a greenhouse (Sanz-Pérez et al., 2016). Currently, liquid
absorbents—aqueous amines such as monoethanolamine (MEA)—
are widely used in the industry to capture post-combustion CO2
(Sanz-Pérez et al., 2016). However, these aqueous amines are cor-
rosive and require high energy consumption in the regeneration
process (up to 20% energy penalty (Oyenekan and Rochelle,
2007)). To this end, the use of solid sorbents could enhance the
contact area between CO2 and the scrubbing agent. Besides, it also
improves energy efficiency during the regeneration process as liq-
uid solvents are eliminated (Gauvillé et al., 2008). Various amine-
functionalised mesostructured material-including metal–organic
framework (MOF) (McDonald et al., 2012), nanofibrillated cellulose
(Gebald et al., 2011), carbon nanotubes, activated carbons, and zeo-
lites (Lu et al., 2008)-have been developed and initial results are
promising as cyclic capacity of up to 0.696 mmol CO2/g (Gebald
et al., 2011) have been achieved.
One novel high-value application of rPET is the production of
aerogel using recycled polyester. Aerogels are a class of highly-
porous ([70–99]%) materials which exhibit low density ([7–26]
kg/m3), large specific surface area ([520–1590] m2/g), excellent
thermal insulation ([0.01–0.05] W/mK), and outstanding acoustic
properties (Gesser and Goswami, 1989), making them ideal for
many high-value application such as drug delivery in pharmaceu-
tical sciences (Stergar and Maver, 2016), filters for pollutants
(Ahmed and Attia, 1995; Cooper, 1989), and also building insula-
tion materials (Baetens et al., 2011). The two critical steps in aero-
gel production are gel formation and drying (Pierre and Pajonk,
2002), where methods adopted to replace the gel’s liquid phase
with air include the hazardous supercritical drying, the slow ambi-
ent pressure drying, and the cost-effective freeze-drying
(Soleimani Dorcheh and Abbasi, 2008). Current literature on aero-
297
gels is dominated by silica aerogels (Mazraeh-Shahi et al., 2013;
Soleimani Dorcheh and Abbasi, 2008), but silica aerogels are extre-
mely brittle and non-human friendly (Cuce et al., 2014). To this
end, an environmentally friendly rPET aerogel developed by Koh
et al. (Koh et al., 2018) overcomes some limitations of silica aero-
gels as it is flexible while exhibiting ultra-low density ([0.007–
0.026] g/cm3), excellent hydrophobic properties (water contact
angle of [120.7–149.8]°), high elasticity (Young’s modulus of
[1.16–2.87] kPa), and superior thermal insulation ([0.035–0.038]
W/mK), suitable for insulation (acoustic and thermal) and filtration
(oil and CO2) applications.
Expanding on the work of (Koh et al., 2018), this project aims to
transform environmental waste (PET) into materials (aerogels) for
high-value engineering applications. The coating agents, silicone
ceramic coating and (3-aminopropyl)triethoxysilane, are applied
to rPET aerogel to improve its thermal and adsorption properties
through cost-effective and straightforward coating methods. The
morphology and property control-including hydrophobicity,
mechanical properties, thermal conductivity and CO2 capture of
modified rPET aerogels are investigated for other novel high-
value applications, specifically heat insulation and CO2 filter
materials.
2. Experimental
2.1. Materials
Recycled PET staple fibres, 3D deniers and 64 mm in length, are
purchased from Foshan Rongsheng Furniture Material Co. Ltd.
(Guangdong, China). Sodium hydroxide (NaOH), hydrochloric acid
(HCl, 37%), polyvinyl alcohol (PVA), glutaraldehyde (GA, 25% in
H2O), methoxytrimethylsilane (MTMS), (3-Aminopropyl)
triethoxysilane (APS, or APTES) and absolute ethanol (EtOH) are
purchased from Sigma-Aldrich Pte. Ltd. (Singapore) and used as
received. Silicone ceramic coating (SCC) is obtained from commer-
cially. All chemicals are used in their original state and without fur-
ther purification.
2.2. Fabrication of the rPET aerogels
Aqueous PVA (5.0 wt% concentration) solution is prepared by
dissolving PVA pallets into warm deionised (DI) water using a mag-
netic stirrer, at temperatures below 80 °C. The gel solution is pre-
pared by adding different concentrations of functionalized rPET
fibres (1.0, 2.0 and 3.0 wt% inside the gel mixture) and cross-
linkers–polyvinyl alcohol (PVA) (5.0 wt% concentration) and glu-
taraldehyde (GA) (25 wt% concentration)–into DI water using a
fixed weight ratio of rPET fibres: PVA: GA (10:1:0.02). The pH of
reaction media is controlled at 3 by adding aqueous HCl (37%) solu-
tion to facilitate the crosslinking reaction (Baetens et al., 2011; Koh
et al., 2018). The resulting gel solution is sonicated for 30 min at
400 W using a high surface sonication probe (UIP2000hdT,
Hielscher-Ultrasound Technology, Teltow, Germany) to obtain a
homogeneous gel solution free of bubbles. Ageing/curing of the
gel solution is then conducted in an oven for 3 h at 80 °C. Upon
completion of the ageing process, the gel solution is frozen and
transformed into the rPET aerogel using a freeze dryer (TPV-50F
Vacuum Freeze Dryer, Toption, China); during freeze-drying, the
solvent in the gel is removed by direct sublimation leaving behind
a highly-porous aerogel structure (Sudant et al., 2004).
2.3. Surface modification of rPET aerogels
A simple coating technique is devised to enhance the thermal
stability of rPET aerogels. The SCC solution is prepared by first dis-
298 D.K. Le et al. / Waste Management 100 (2019) 296–305

solving different concentrations of SCC (varying weight ratio of
SCC: rPET aerogel) in EtOH and stirring the mixture to ensure
homogeneity. The rPET aerogel is then submerged in the SCC solu-
tion to absorb the ceramic coating until saturation. Subsequently,
the rPET aerogel is removed from the solution and left to dry at
room temperature.
Another coating technique is also developed to coat APS on the
rPET aerogels for CO2 capture applications. The method involves
adding different concentrations of APS solutions (10, 20, 30, and
40 wt% concentration) into the gel solution before the sonication
of the gel mixture. All the steps in the proceeding and following
the preparation of the gel solution remains unchanged.
2.4. Characterization of the rPET aerogels
The structure and morphology of the aerogels are examined
under the material analysis microscope (Leica DM2500 M, Leica,
Wetzlar, Germany) and field-emission scanning electron micro-
scope (FE-SEM, Model S-4300 Hitachi, Japan). For FE-SEM, the sam-
ples are first coated with a thin film of gold for 90 s at 20 mA using
a sputter coater (Cressington 108auto, Cressington Scientific
Instruments Ltd., Watford, UK) to enhance its surface sensitivity
to electron beams (Castle and Zhdan, 1997). Fourier transform
infrared (FTIR) spectroscopy, performed in a VERTEX 80v FTIR
spectrometer (Bruker, Germany), is used in order to study the sur-
face modification of the rPET aerogel by SCC and APS/APTES coat-
ing. The resolution used is 4 cm1 and the spectra scanned range
is 4000–400 cm1.
The bulk density of the samples is obtained by measuring the
mass and volume of the cylinder-shaped aerogels using a micro
weighing scale and Vernier caliper, respectively. The porosity (U)
is a measure of void spaces in a material, and it is commonly
expressed as a percentage of total volume (Cervin et al., 2012).
The densities of the aerogel (qa), rPET fibres (qf = 1.39 g/cm3),
and porosity could be determined using the following relationship:
U ¼ ð1  qa =qf Þ:
Water contact angle test is conducted to analyse the hydropho-
bicity of rPET aerogels using a video contact angle (VCA) goniome-
ter (VCA Optima, AST Products Inc., Massachusetts, USA). Here,
1.0 mL of water is dispensed from a syringe onto an aerogel flat sur-
face, where the bundled software analyses the image and calcu-
lates the water contact angle (H).
The compressive modulus (E) of the rPET aerogels is obtained by
conducting the compressive test using a load frame machine (Ser-
ies 5500, Instron, Massachusetts, USA); test specimens are sub-
jected to a load cell of 1000 N at a constant loading rate of
1 mm/min.
The thermal conductivity of rPET aerogels is obtained using a
thermal conductivity analyser (C-Therm TCi Thermal Conductivity
Analyzer, C-Therm Technologies, Canada), where specimens are
subjected to a modified transient plane source (TPS) test method
at ambient temperature (~24 °C) (Mathis, 2000).
To evaluate the thermal stability of the aerogels, the thermal
gravimetric analysis (TGA) test is performed using the DTG60H
thermogravimetric analyser (Shimadzu, Japan). The specimens
are gradually heated in air from 30 °C to 800 °C, at a constant rate
of 10 °C/min.
The Quantachrome iQ3 (Quantachrome, Florida) automated gas
sorption analyser is used to measure the CO2 sorption isotherms.
At the beginning of the test, the sample (50 mg) is first degassed
for 10 h by heating it to 80 °C under reduced pressure condition
(<10 Pa). Once the sample is degassed, ultra-high purity (UHP)
grade CO2 will be passed into the test chamber where the pressure
of the test chamber is gradually increased from 10 Pa to atmo-
spheric pressure (1 MPa) at a constant temperature of 25 °C.
3. Results and discussion
3.1. Morphologies and structure of rPET aerogels
The morphology and the structure of rPET aerogel are tabulated
in Table 1 and shown in Fig. 1. The rPET aerogel’s high porosity
(Uavg = [98.1–99.6]%) and ultra-low density (qa = [11–26] mg/
cm3) are attributed to the sizeable voids observed in the FE-SEM
images. Up to a fibres concentration of 2.0 wt%, the density of the
rPET aerogel is generally directly proportional to the fibres concen-
tration. At higher fibres concentration (>2.0 wt%), the resultant
aerogel tends to expand beyond the desired volume (up to 25%)
if no external force is exerted to compact the rPET fibres. The
developed rPET aerogels in this work show similar properties com-
pare to the rPET aerogel synthesized by Koh et al. (Koh et al., 2018)
with a high porosity of [98–99.5]% and a low density of [14–26] g/
ð1Þ
cm3.
The reaction mechanism between the rPET fibres and cross-
linkers is proposed by Koh et al. (Koh et al., 2018). PVA added
during the preparation of the gel solution is responsible for the
hydrogen bonds–between the hydroxyl groups of the rPET and
PVA chain, and ester bonds between the rPET’s carboxyl group
and PVA chain’s hydroxyl group form after curing. On the other
hand, GA contributes to the formation of acetal bridges between
the rPET and PVA chain; thereby reinforcing the rPET-PVA
matrix.
The FE-SEM images of the rPET aerogel, rPET/SCC aerogel, and
amine-functionalised rPET aerogels of different fibres concentra-

Table 1
Physical properties of rPET aerogels, rPET/SCC aerogels and amine-functionalised rPET aerogels at different fibres concentration ([1.0–3.0] wt.%), various levels of SCC (1–4 ratio of
SCC and rPET), and a variety of APS concentration ([10–40] wt.%).

Sample Composition Fibres Conc. (wt.%) Density, qa (mg/cm3) Porosity, Uavg (%) Fibre diameter, (lm)
PA1 1.0 wt% rPET 1.0 11 ± 2 99.2 ± 0.2 21.6 ± 0.1
PA2 2.0 wt% rPET 2.0 20 ± 2 98.5 ± 0.2 21.7 ± 0.2
PA3 3.0 wt% rPET 3.0 26 ± 2 98.1 ± 0.2 21.6 ± 0.3
PA4 1.0 rPET/SCC1 1.0 14 ± 2 99.0 ± 0.3 23.2 ± 0.2
PA5 1.0 rPET/SCC2 1.0 16 ± 2 98.9 ± 0.4 24.8 ± 0.1
PA6 1.0 rPET/SCC4 1.0 20 ± 2 98.6 ± 0.6 26.4 ± 0.2
PA7 2.0 rPET/SCC4 2.0 46 ± 4 96.7 ± 0.4 27.2 ± 0.4
PA8 3.0 rPET/SCC4 3.0 62 ± 3 95.6 ± 0.5 27.8 ± 0.3
PA9 1.0 rPET-APS20 1.0 12 ± 2 99.1 ± 0.2 24.1 ± 0.2
PA10 2.0 rPET-APS20 2.0 20 ± 2 98.5 ± 0.3 24.3 ± 0.3
PA11 3.0 rPET-APS10 3.0 50 ± 2 96.3 ± 0.3 23.8 ± 0.2
PA12 3.0 rPET-APS20 3.0 52 ± 2 96.1 ± 0.2 24.5 ± 0.3
PA13 3.0 rPET-APS30 3.0 54 ± 2 96.0 ± 0.3 24.8 ± 0.2
PA14 3.0 rPET-APS40 3.0 58 ± 3 95.7 ± 0.4 25.3 ± 0.4
 D.K. Le et al. / Waste Management 100 (2019) 296–305
tions (1.0, 2.0 and, 3.0 wt%) are shown in Fig. 1. As evident from
Fig. 1 (a, b, c), a highly porous (macropores >50 nm) network is
formed by the overlapping PVA-bonded rPET fibres. As the rPET
fibres concentration increases (from 1.0 wt% to 3.0 wt%), the size
of the voids between the rPET fibres decreases, resulting in a
denser structure. Interestingly, longer bundles of PVA strands
are observed to form around the intersection of the rPET fibres
at lower rPET fibres concentrations. This phenomenon could
have arisen due to the expansion of the rPET fibres to fill the
gel solution uniformly during curing. Stresses might have been
induced on the PVA to maintain the bonds between rPET fibres,
where such effects will be more pronounced at lower fibres con-
centration as the rPET has to fill up the same volume with less
material.
Modification rPET aerogel by SCC at different fibres concentra-
tions ([1.0–3.0] wt.%, PA6–8, respectively), despite being coated
with the same concentration of SCC solution (weight ratio of rPET
and SCC solution as 1:4), is carried out to enhance the aerogels’
thermal property. It is observed that for the rPET/SCC aerogel, the
SCC forms a protective layer (thickness of [1.0–3.0] lm) over the
rPET fibres and the PVA, as the fibre diameter increases, Fig. 1 (d,
g). Apart from the triangular ‘sail’ shape structures form at the
intersections of the rPET fibres, the rPET/SCC aerogel remains
highly porous. A dehydrocoupling reaction between SiAH (SCC)
and CAOH groups on the surface of rPET aerogel occurs in the pres-
ence of acid catalyst (EtOH), leading to the formation of SiAOAC
bond and resulting in an increase of the fibre diameter from
21.6 lm to about [23–28] lm. FTIR results indicate a replacement
AOH groups by silane groups, after modifying by SCC, occurs. The
Fig. 1. Structure of rPET aerogels with different fibres concentration (a)-1.0 wt%, (b)-2.0 wt%, (c)-3.0 wt%; (d)-rPET/SCC aerogels; (e)-amine-functionalised rPET aerogel; (f),
(g), (h)-fibres diameter of rPET, rPET/SCC and amine-functionalised rPET aerogel, respectively. (i) Appearance of rPET aerogel.
299
difference spectra of the rPET aerogel and rPET/SCC aerogel are
shown in Fig. 2a. The band in the region of [3200–3400] cm1 illus-
trates that the presence of AOH groups has almost disappeared,
indicating that all AOH groups have been replaced on the surface
of the rPET/SCC aerogel. In the range of [1000–1200] cm1, the
band near 1030 cm1 is related to the SiAOASi asymmetric
stretching bonds, and the bands near 1065 cm1 and 1105 cm1
are attributed to the SiAOAC asymmetric stretching (Bellamy,
2013; Bengtsson and Oksman, 2006). The presence of a new band
at 700 cm1 corresponds to the SiAOASi symmetric stretching
(Valadez-Gonzalez et al., 1999). The small band near 1240 cm1
can be assigned to the stretching of SiACH3 bonds (Jing et al.,
2002) and the band at 1440 cm1 corresponds to CH2 bending of
the silane propyl chain (Gebald et al., 2011). These results demon-
strate that the surface of the rPET aerogel has been successfully
modified by SCC solution. SCC coating on the rPET aerogel also
leads to an increase in the aerogel’s density (up to 2.4-fold) and
consequently a reduction in porosity (up to 3.5% reduction). Never-
theless, the rPET/SCC aerogel still exhibit relatively high porosity
(Uavg = [95.6–99.0]%) and ultra-low density (qa = [14–62] mg/
cm3) as compare to silica aerogel (U = [59–91]% and qa = [374–
902] mg/cm3) (Mazraeh-Shahi et al., 2013).
Similarly, the coating of APS on the aerogels slightly reduces
porosity (Uavg = [95.7–99.2]%) and marginally increases the aero-
gel’s density (qa = [11–58] mg/cm3). Furthermore, while maintain-
ing the rPET aerogel’s highly porous structure, the amine-
functionalised rPET aerogel is APS uniformly coated (thickness
[0.5–2.0] lm) on the rPET fibres and the PVA, Fig. 1(e, h). The FTIR
spectrum of the amine-functionalised rPET aerogel shows a suc-
300 D.K. Le et al. / Waste Management 100 (2019) 296–305
Fig. 2. (a) FTIR spectra of the rPET aerogel, amine-functionalised rPET aerogel and rPET/SCC aerogel. (b) Visualisation of water contact angle measurement.
cessful grafting of APS on the rPET aerogel through NH2 bending at
[1550–1660] cm1 (Fig. 2a) (Bacsik et al., 2011; Gebald et al.,
2011). The band at [1550–1660] cm1 can be assigned to aminosi-
lane used here and is associated with asymmetric NH+3 deforma-
tion, formed through the interaction of primary amines with
water or hydroxide groups on the surface of the rPET aerogel
(Bacsik et al., 2011; Danon et al., 2011). The new band at
1192 cm1 is related to CAN stretching bonds (Kang et al., 2016).
The bands in the region of [2900–2950] cm1 are attributed to
CAH stretching and the band at 1440 cm1 corresponds to CH2
bending of the silane propyl chain (Bacsik et al., 2011; Gebald
et al., 2011). The grafting conditions employed are sufficient for
covalent bonding of silane molecules and the rPET aerogels by
the appearance of signals associated with vibration from silicon-
based linkages at 1240 cm1 (SiAC), 1030 cm1 (SiAOASi asym-
metric) and 700 cm1 (SiAOASi symmetric) (Bellamy, 2013; Jing
et al., 2002; Valadez-Gonzalez et al., 1999).
3.2. Hydrophobicity of rPET aerogels
Fig. 2b illustrates a typical image obtained from the water con-
tact angle test conducted on the rPET aerogel and rPET/SCC aerogel
surface. As shown in Table 2, rPET aerogels are hydrophilic
(Havg = 0°) as the water droplets sank into the aerogel. The hydro-
philic nature of the rPET aerogels could be attributed to the pres-
ence of polar hydroxyl groups in the PVA chain, which attracts
water (Giovambattista et al., 2007).
Notably, SCC coated on the rPET aerogel has a secondary effect
of turning the aerogel hydrophobic (Havg = [130.5–144.7]°). SCC,
with SiAOASi structure (Colombier and Cuer, 1991), is innately
hydrophobic as the bonding between the surface oxygen and water
is weaker than the intermolecular bonding in water (Skipper et al.,
1989). Therefore, the coating of SCC on the rPET aerogel will form a
layer of non-polar SCC over the polar hydroxyl groups and alter its
hydrophobicity. Regarding to Table 2 (PA4-6), varying the amount
of SCC coated on a fixed weight percent rPET aerogel have a pro-
portional effect on the resultant hydrophobicity of the rPET aero-
gel; where a high concentration of SCC applied on the aerogel
would correspond to a higher water contact angle, Havg. Moreover,
it can be observed from Table 2 (PA6-8) that applying similar con-
centrations of SCC coating solution (weight ratio of SCC solution:
rPET fibres = 4:1) on different fibres concentration ([1.0, 2.0, 3.0]
wt.%) of rPET aerogel yielded similar hydrophobicity (Havg =
[144.3–144.7]°). Thus, it can be deduced that SCC’s effect on
hydrophobicity is independent of the rPET fibres concentration
(as measured by the contact angle).
3.3. Mechanical properties of rPET aerogels
Mechanical properties indicate the durability of the rPET aero-
gels. Therefore, the compressive test is conducted on the rPET aero-
gel and rPET/SCC aerogel to determine their respective
compressive Young’s modulus (E). Evident from Table 2 and
Fig. 3, the compressive Young’s modulus of the rPET aerogel is very
low (Eavg = [1.2–3.2] kPa), where the increase in rPET fibres concen-
tration is proportional to the resultant Young’s modulus. The
increase in Young’s modulus at higher fibres rPET concentrations
could be attributed to the greater number of cross-fibres support
sites in rPET aerogels with higher fibres concentrations, which
enhances the rigidity of the aerogel structure.
Moreover, with reference to Table 2, it can be observed that the
coating of SCC on the rPET aerogels significantly increase the rPET/
SCC aerogel’s Young modulus (Eavg = [4.5–124.8] kPa), where for a
fixed weight percentage (e.g., 1.0 wt%) rPET/SCC aerogel, the
amount of SCC coated is proportional to the compressive Young’s
modulus (refer to Fig. 4a). The increase in Young’s modulus could
be attributed to the SCC, which coats on the PVA and reinforces
the rPET-PVA bonds.
Furthermore, from Fig. 4b, it is observed that rPET aerogels with
higher fibres concentrations yield a greater improvement in
Young’s modulus when coating with similar concentrations of
SCC solution (weight ratio of SCC: PET fibres = 4:1). This phe-
nomenon could be attributed to the greater number of cross-
fibres support sites and higher SCC coating efficiency of rPET aero-
gels with higher fibres concentrations. Together, the two factors
have a multiplier effect in enhancing the rigidity of the aerogel
structure.
3.4. Thermal property of rPET aerogels
3.4.1. Thermal conductivity of rPET aerogels
The thermal conductivities (at Trm = 25 °C) of the rPET aerogels
and rPET/SCC aerogels are tabulated in Table 2. rPET aerogels exhi-
bit ultra-low thermal conductivities (kavg = [34.4–37.7] mW/m
K),
which is comparable with conventional insulation materials such
as foams and wools (k = [20–55] mW/m
K (Cuce et al., 2014)).
 D.K. Le et al. / Waste Management 100 (2019) 296–305 301

Table 2
Water contact angle, mechanical property and thermal property of rPET aerogels and rPET/SCC aerogels at different fibres concentration ([1.0–3.0] wt.%), various levels of SCC (1–
4 ratio of SCC and rPET).

Sample Composition Fibres Conc. (wt.%) Water Contact Angle, Havg (°) Young’s Modulus, Eavg (kPa) Thermal Conductivity, Kavg (mW/mK)
PA1 1.0 wt% rPET 1.0 0 1.2 ± 0.1 36.0 ± 0.2
PA2 2.0 wt% rPET 2.0 0 2.5 ± 0.1 36.7 ± 0.2
PA3 3.0 wt% rPET 3.0 0 3.2 ± 0.1 37.7 ± 0.2
PA4 1.0 rPET/SCC1 1.0 130.5 ± 1.7 4.5 ± 0.2 34.9 ± 0.1
PA5 1.0 rPET/SCC2 1.0 137.7 ± 1.3 7.3 ± 0.3 32.5 ± 0.2
PA6 1.0 rPET/SCC4 1.0 144.7 ± 1.7 14.6 ± 1.1 31.8 ± 0.1
PA7 2.0 rPET/SCC4 2.0 144.3 ± 1.0 47.9 ± 4.9 32.3 ± 0.4
PA8 3.0 rPET/SCC4 3.0 144.5 ± 0.8 124.8 ± 3.5 32.9 ± 0.2

Fig. 3. Compressive stress-strain curves of rPET aerogels at varying of rPET fibres concentration ([1.0–3.0] wt.%).

Given that air and rPET at room temperature have a thermal con-
ductivity of approximately 26.4 mW/m
K (Lemmon and Jacobsen,
2004) and 280 mW/m
K (Kalácska et al., 2016) respectively, the
ultra-low thermal conductivity of the rPET aerogel can be attribu-
ted to its highly porous structure (Uavg = 98.1–99.6%). Note-
worthily, the thermal conductivity of the rPET aerogels rises with
increasing fibres concentrations ([1.0–3.0] wt.%) as the aerogel
becomes less porous; hence, the aerogel thermal conductivity is
proportional to its fibres concentration.
SCC coating on the rPET aerogel decrease its thermal conductiv-
ity by up to 12.7%, with a thermal conductivity of Kavg = [31.8–34.8]
mW/m
K. Moreover, for a fixed weight percentage rPET aerogel, it
is observed that its thermal conductivity decreases with increasing
SCC quantity. As the measured average thermal conductivity (at
Trm = 25 °C) of the cured SCC wafer is 46.8 W/m
K, the lower ther-
mal conductivity observed for the rPET/SCC aerogel can be attribu-
ted to the coated SCC. SCC has a significantly lower thermal
conductivity than rPET fibres (K = 280 mW/m
K (Kalácska et al.,
2016)), and when coated over the rPET fibres would enhance the
aerogel’s thermal insulative properties.
3.4.2. Thermal stability of PET aerogel
Fig. 5 shows the TGA and DTA curves for rPET aerogel and rPET/
SCC aerogels at varying levels of SCC. The rPET aerogel (rPET/SCC0)
contains cross-linked rPET/PVA, and it decomposes in two steps.
Evident from the DTA curves, the first peak occurs at approxi-
mately 300 °C, and it corresponds to the initial decomposition of
the cross-linker PVA (Yang et al., 2012). The second peak occurs
at approximately 480 °C, and it corresponds to the decomposition
of the PET polymer.
The coating of SCC onto the rPET aerogel improves the thermal
stability of the aerogel as it delays the final aerogel decomposition
from 480 °C to 600 °C. The greater initial weight change observed
for the rPET/SCC aerogel could be attributed to the SCC additives
which accelerates the decomposition (TA Instruments, n.d.), and
also the charring of SCC which forms a protective layer over the
rPET fibres and PVA to provide additional thermal protection.
Heated above 600 °C, the remaining weight of the rPET/SCC aerogel
corresponds to the remaining SCC. Noteworthily, the quantity of
SCC coated on the aerogel is proportional to the final decomposi-
tion temperature of the aerogel. The improvement in thermal sta-
bility observed might be due to a thicker silicone layer coated over
the rPET fibres, which has a positive effect on the thermal stability
of the aerogels.
3.5. CO2 adsorption capability of rPET aerogel
Fig. 6 shows the CO2 adsorption curve of the rPET aerogel and
the amine-functionalised rPET aerogel. As evident from Fig. 6, the
amine coating enhances the CO2 adsorption capability of the rPET
aerogel by up to 3-fold. As proposed by Chaikittisilp et al.
(Chaikittisilp et al., 2011), the APS grafts onto the surface of the
hydroxyl groups of its host. Therefore, for the rPET aerogel, the
APS grafts onto the surface of the hydroxyl groups present in the
rPET aerogel. It is observed that an increase of fibres concentration
([1.0–3.0] wt.%) results in an increase of CO2 absorption with
remaining of APS concentration of 20 wt%. Noteworthily, for a fixed
fibres concentration (3.0 wt%), increasing the amount of APS (10–
40 wt%) added to the gel solution during the fabrication of the rPET
aerogel have a proportional effect on the resultant CO2 adsorption
302 D.K. Le et al. / Waste Management 100 (2019) 296–305

Fig. 4. Compressive stress–strain curves of (a) 1.0 wt% rPET/SCC aerogels with different SCC levels (1–4 ratio of SCC and rPET), and (b) varying fibres concentration ([1.0–3.0]
wt.%) rPET/SCC aerogels at the same concentration of SCC solution (rPET:SCC = 1:4).

capability of the aerogel. A plausible explanation is the curing of
the APS with the gel solution allows for more APS to be covalently
bonded to the rPET fibres and PVA. The reversibility is studied in
detail at low pressure. The results confirm that it is reversible with
pressure; all CO2 can be removed by decreasing the pressure
(Fig. 6c) with some hysteresis. Moreover, CO2 adsorption with
amine-based adsorbents includes both physical adsorption within
pores and chemical adsorption on amine groups (Liu et al., 2015).
The physical adsorption of CO2 on materials gradually reverses
when the temperature increases (Martín et al., 2016). Because of
the chemical adsorption of CO2 is an exothermic process (Wang
et al., 2015), the chemically adsorbed CO2 can easily escape from
the amine as the temperature is raised. Therefore, the adsorbed
CO2 on the rPET aerogel can be desorbed by increasing
temperature.
The mechanism for CO2 sorption on amine-functionalised mate-
rials is proposed by Bacsik et al. (Bacsik et al., 2011) and Hahn et al.
(Hahn et al., 2015). Ammonium carbamate ion pairs and hydrogen-
bonded carbamic acids form rapidly on the surface of sorbent
when contacting with dry CO2. When contacted with CO2 for a sig-
nificant time under dry conditions, an additional moiety form
results. This ester does not form when water is present during
the CO2 uptake. The highest CO2 adsorption (0.44 mmol CO2/g) is
achieved by the rPET aerogel 3.0 wt% coated with 40.0 wt% APS
(PA14). Noteworthily, PA14 performs better than several commer-
cial physiosorbents, such as the metal-organic framework (MOF) –
including HKUST-1 (0.05 mmol CO2/g) and Mg-MOF-74
(0.14 mmol CO2/g) (Kumar et al., 2015; Sanz-Pérez et al., 2016).
However, the CO2 adsorption capability of the amine-
functionalised rPET aerogel remains inferior to other amine-
 D.K. Le et al. / Waste Management 100 (2019) 296–305 303

Fig. 5. Thermal stability (TGA and DTA curves) of the rPET/SCC aerogel at varying
levels of SCC solution compare to rPET aerogel (rPET/SCC0).

functionalised physiosorbents. Gebald et al.’s (Gebald et al., 2011)

amine-based nanofibrillated cellulose adsorbent achieves a CO2
adsorption capacity of 1.39 mmol CO2/g. The lower CO2 adsorption
capacity of the rPET aerogel could be attributed to the large pore
size (>50 lm) of the 3.0 wt% rPET aerogel as compared to the
nanofibrillated cellulose (<10 lm (Gebald et al., 2011)); thus mak-
ing it more difficult for the former to trap CO2. Moreover, the
degree of amine groups on the surface of sorbent also influences
the adsorption capacity. The highest CO2 uptakes are achieved by
sorbents with the highest concentrations of amine equivalents
(Hahn et al., 2015). The lower adsorption capacity of the rPET aero-
gel could be caused by the low degree of APS impregnated on
aerogels. Fig. 6. CO2 uptake of amine-functionalised rPET aerogel at 298 K with (a) different
rPET fibres concentration ([1.0–3.0] wt.%), and APS 20 wt%; (b) various APS
concentration ([10–40] wt.%) with the rPET aerogel 3.0 wt%; (c) Adsorption and
desorption isotherms of CO2 at 25 °C on PA-ASP40 aerogel.
4. Conclusions

Coating techniques are successfully devised to enhance the
thermal stability and CO2 adsorption capability of the rPET aerogel.
The effects of SCC and APS/APTES on the rPET aerogel’s morphology
and properties are probed systemically. The rPET/SCC aerogel exhi-
bits improved thermal performance—thermal stability of up to
600 °C and enhanced thermal insulation (Kavg = [31.8–34.9] mW/
m
K)—while maintaining an ultra-low density (qa = [14–62] mg/
cm3) and a high porosity (Uavg = [95.6–99.0]%) of the aerogel struc-
ture. Moreover, the coating of SCC has a secondary effect of turning
the rPET/SCC aerogel hydrophobic (up to 144.7° in contact angle)
and enhance the rigidity of the aerogel structure (Eavg = [4.5–
124.8] kPa). Furthermore, 3.0 wt% rPET aerogel has a maximum
CO2 adsorption capacity of 0.15 mmol CO2/g. The coating of APS
on the rPET aerogel further enhances the CO2 adsorption capacity
of the rPET aerogel by up to 300%, achieving a maximum capacity
of 0.44 mmol CO2/g. The promising results obtained demonstrate
that rPET aerogel is a versatile material suitable for a wide variety
of high-value engineering applications.
Declaration of Competing Interest
There are no conflicts to declare.
Acknowledgements
The authors would like to thank FB (C-265-000-049-001) fund-
ing support and the lab officers in Materials Division, Department
of Mechanical Engineering, National University of Singapore for
their significant help on characterizations.
304 D.K. Le et al. / Waste Management 100 (2019) 296–305

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