CELLULOSE CHEMISTRY AND TECHNOLOGY

REGENERATED CELLULOSE-BASED COMPOSITE STRENGTHENED WITH

POST-CONSUMER POLYESTER GARMENTS

MOHAMMAD ABUL HASAN SHIBLY,*,** PALASH KUMAR SAHA,***

MD. ABDUL GAFUR** and BASIT ABDUL****
*
Center for Research and Industrial Relations, Department of Textile Engineering, National Institute of
Textile Engineering and Research, University of Dhaka, Dhaka-1000, Bangladesh
**
Pilot Plant and Process Development Center, BCSIR, Dhaka-1205, Bangladesh
***
Department of Nanoscience and Biomedical Engineering,
South Dakota School of Mines and Technology, South Dakota, USA
****
Turkey Nanotechnology Research and Application Center, Sabanci University, Turkey
✉Corresponding author: M. A. H. Shibly, [email protected]

Received December 8, 2022

Polyester garments have an extensive availability nowadays. However, most post-consumer garments are burned and
landfilled, leading to extreme pollution and significant waste of resources. Therefore, sustainably and economically
recycling this post-consumer polyester (PCP) fabric waste for essential value-added products is meaningful and
necessary. In this study, waste polyester fabrics obtained from PCP garments have been utilized in the development of
composite materials. First, PCP fabric was dissolved in a methanol and sodium hydroxide solution. Then, the polyester
paste was regenerated on regenerated cellulose-based fabric (viscose), constructing a viscose-based composite. The
physical, thermal, chemical, morphological, and mechanical properties were examined for the viscose and viscose-
polyester (VP) composites. FTIR, XRD, SEM, and percent add-on confirmed the presence of polyester in the
composite. In addition, an add-on percentage of 10.71, higher crystallinity of 55.20%, thermal stability, and about 21%
higher tensile strength were observed. The results, as mentioned above, ensured that the PCP waste can be used as a
matrix for composite materials.

Keywords: viscose fabric, post-consumer polyester fabric, composite, recycling

INTRODUCTION
In recent years, the tremendously increasing Pre-consumer, post-consumer, and industrial
living standards and population growth have wastes are all included in textile waste streams.
boosted consumer demand for fabric. To meet the The European Union produces almost 5.8 million
fabric demand, the textile industry has raised tons of post-consumer textile waste annually.6 In
annual fibre and fabric production.1 Currently, the addition, polyester materials generate a
global yearly fibre production is 82 million tons, considerable amount of waste (fibres, filaments,
of which 60% is synthetic.2 Presently, fast fashion fabrics, films, bottles, and other molded articles).7
is controlled by synthetic textiles, especially Almost half of all fibre waste comes from the
polyester, with a yearly production of polyester spinning industry alone, which accounts for
exceeding 55.1 million metric tons.3 Furthermore, nearly all waste fibre output.8 Similarly, waste
more than 30% of the clothes purchased in from the apparel industry and post-consumer
Europe have not been worn for at least one year apparel is increasing rapidly. Global fashion
due to fast fashion trends.4 Thus, the higher waste reached 92 million tons in 2015 and is
manufacturing capacity of textile industries and expected to reach 148 million tons by 2030.9
extensive use of polyester leads to higher Hence, the development of processes that utilize
production of textile waste. Given these economic fabric and fibrous wastes and transmute them into
and environmental issues, a growing interest has significant products to mitigate the increasing
been developed in turning textile waste into impact of suchlike non-biodegradable material on
valuable goods.5 the environment.

Cellulose Chem. Technol., 57 (3-4), 409-417(2023)

MOHAMMAD ABUL HASAN SHIBLY et al.

Polyester materials represent a threat for the method of composite manufacturing and
environment because of their non-biodegradable decreases the effect of polyester garment waste.
nature.2 The polyester material can pollute land, Thus, a suitable solvent was used first to liquefy
waterways, and air.10 Polyester fabric in landfills the polyester fabric. A viscose fabric was then
is alarming, as it releases dyes and chemicals into covered with a regenerated layer of this solution.
the soil. This leads to soil contamination.11 The The polyester particles take a position on the
air is also polluted through the fly-off produced inner and outer surface of the viscose fabric,
by small and light polyester fibres during giving high abrasion and washing resistance. The
manufacturing.2 Numerous studies have revealed environmental and health risks were considered
that synthetic fibres account for a sizable portion when choosing the solvent.
of the microplastic found in water and are
frequently cited as the leading cause of pollution. EXPERIMENTAL
Plastic Soup Foundation has revealed that more Materials
than 4,500 fibres can release after washing one The 100% viscose plain-woven fabric used in
gram of garments.12,13 Microfibers are so tiny that constructing the composite was collected from the
they can readily pass through wastewater weaving setup of a textile plant. The structure of the
treatment plants and easily bind with molecules of plain ( ) fabric was (75 × 70 / 32 × 30) × 56, 140
harmful elements in wastewater. These gram per square meter (GSM), dyed with reactive
dyes. The regenerated cellulose-based (viscose) fabrics
microfibers are then consumed by plankton and
had a thickness of around 0.6 mm. PCP garments,
small fish, concentrating toxins and going up the treated as post-consumer textile waste, were also
food chain.14-17 The effects on the human body collected for this study. Methanol was utilized to
need to be investigated and clarified. Hence, dissolve the PCP garments; acetic acid and sodium
proper recycling of waste polyester material can hydroxide pellets were bought from M/S Nasir
reduce environmental and human burdens by Chemicals, Dhaka, Bangladesh. The composite
decreasing the flow of waste polyester. development processes and drying with a small-scale
A lot of research has been performed on framework for holding the treated fabric were brought
recycling polyester materials. Hydrolysis,18 to pass on a laboratory-scale rubber-coated padding
glycolysis along with microwave irradiation,19,20 mangle and Mathis drying machine, respectively.
and electron beam radiation21 methods have been
Methods
developed for the recycling of polyester bottles. Specimen preparation
Some researchers have separated polyester from a Dark blue dyed viscose fabric and white coloured
polyester wool blend using static electricity, PCP garment were taken to identify polyester
fusing, hydrolyzing, and enzymatic degradation components in the viscose-polyester (VP) composite.
methods.22,23 Various procedures, such as using First, the viscose fabric was cut into pieces with
ionic solvent,1,24 a two-step method of acid dimensions of 10×10 inches and washed for one hour
treatment,25 and phosphoric acid,26 have been at 50 °C. Thus, dust was removed and the extra dye
carried out for recycling cotton polyester blends. was washed out from the fabric surface. Next, the
A few studies have been performed to make collected polyester garments were washed with
detergent to remove dust, dirt, and oil from the apparel
composites from wasted polyester fabric. Ozen et
and thoroughly cleaned with tap water. Subsequently,
al.27 have made epoxy composites by the vacuum- the washed fabric and garment were sun-dried for
assisted resin transfer molding method, using approximately 48 h. After that, the dried PCP garment
waste polyester fabric. Sharma et al.2 have made was cut into small pieces. An image of the dried
cotton composites reinforced with waste chopped PCP is presented in Figure 1 (b).
polyester. These researchers used waste polyester
fibre found from spinning and m-cresol as Composite development
solvent. Their research focused on analyzing the Chopped polyester fabric, viz. 3% (w/v) was
mechanical properties of a cotton composite by dissolved in acetic acid (CH3OH) and sodium
using environmentally friendly solvents and waste hydroxide (NaOH) solution according to the AATCC
test method 20A-2017.28 Amounts of 18 g of NaOH
polyester fibre.
and 200 mL of CH3OH were added in a 250 mL
In the present work, we presented a technique Erlenmeyer flask. The solution was heated to 65 °C for
for using polyester fabric waste collected from mixing thoroughly. The specimen was then placed in
end-users of polyester garments and the Erlenmeyer flask and stirred using a magnetic
manufacturing a composite by chemically treating stirring bar for 5 min. After that, the solution was
the garment waste. This procedure offers a new poured into a Petri dish to introduce viscose fabric into

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the methanol solution for about a minute. Figure 1 (d) used to dry and cure the fabric.29 The fabrics were
shows the liquefied polyester in methanol solutions. treated at 80 °C for 3 min and 110 °C for 2 min for
Afterward, the viscose fabric was removed from the drying and curing, respectively. Then, the fabrics were
solution and run through a rubber-coated padding released from the stretch condition and kept for one
mangle to eliminate the residual solution and allow the hour at room temperature for relaxation. The VP
solution to penetrate deeply into the viscose fabric. The composite fabric was then cleaned with regular water
padding procedure was repeated four times to acquire and neutralized with a 0.1% CH3COOH solution. In
appropriate solution penetration inside the viscose addition, the VP composite was submerged into a
fabric and ensure a four-dip-four-nip process. solution with 2 g/L neutral detergents at 100 °C for
Once outside the padding, the treated VP composite about 10 min. Following a normal wash, the treated
was attached to a fixed tray in a stretch condition to sample was dried in an electric dryer.30 Figure 1
permit the utmost opening of the VP composite in the depicts the stages of the composite preparation
stretched condition. A Mathis curing machine was procedure.

(a (b) (c) (d)

(e) (f) (g) (h)

Figure 1: Viscose fabric (a), cut polyester pieces (b), polyester dissolution (c), dissolved polyester paste (d), padding
mangle (e), drying and curing (f), neutralization (g), and VP composite fabric (h)

Characterization Spectroscopic characterization (FTIR)

Weight change of the fabric Fourier transform infrared (FTIR) spectroscopy
The weight change of the viscose fabric was was performed to observe how viscose fabric and
determined from the difference in gm-2 (GSM) before polyester interacted. FTIR spectra of viscose,
and after the composite preparation. A GSM cutting polyester, and VP composite were recorded in the
device from James H. Heal & Co. Ltd., England, was wavenumber range of 4000 to 400 cm-1 at the
used to determine the fabric’s GSM according to the resolution of 2.0 cm-1, with 32 scans for each
ASTM-D-3776 method.31 specimen, using a FTIR-8400S (Shimadzu
Corporation, Japan) spectrometer.32
Percent add-on
The VP composite was developed with ratios of X-ray diffraction (XRD) analysis
reinforcing viscose fabric and polyester matrix. The The XRD of the viscose fabric and VP composite
composite fabric weight was measured after curing, was performed on a Bruker AXS D8 diffractometer,
and the add-on percentage of the matrix was obtained Germany, using Cu Kα radiation ( = 1.5405 Å). The
based on the oven-dry weight of the viscose fabric: operating conditions were the following: V = 40 kV
The add-on percentage of the polyester-coated and I = 40 mA in symmetrical reflection within the
viscose fabric was established using Equation (1): (2θ) range of 10° to 50°.

Thermal analysis
(1) Thermogravimetric analysis (TGA) of the samples
was performed to determine the thermal behavior of

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MOHAMMAD ABUL HASAN SHIBLY et al.

the samples, using an SDT650 thermal analyzer, TA integrated reflectance spectrophotometer. The
Instruments, USA. 5 mg samples were used for the CIELAB colour coordinates were determined: CIE L*,
TGA experiment. The TGA was performed under N2 a*, b*, C*, h*.2,31 The colour difference, , was
(g) atmosphere with 30 mL/min of gas flow, a constant measured using Equation (4):
heating rate of 10 °C/min, in the temperature range (4)
from room temperature to 600 °C.33
where ∆E* is the total colour difference on the
CIELAB chart; ∆a, ∆b, and ∆L are the difference in
Moisture content
red/green, yellow/blue, and lightness/darkness axis,
After conditioning at 105 °C, the water content of
respectively.
the VP composite specimen was measured using a
moisture analyzer, according to the standard method
ASTM D2495. A 5 g specimen was used according to RESULTS AND DISCUSSION
the standard atmospheric conditions for testing – at 20 Weight change and add-on percent
°C ± 2 °C and 65% ± 2% RH. With a 15 min interim, The changes in fabric weight (GSM) and add-
the weight of the specimen was measured until there on percent were determined to confirm the
was 0.1% less variation in sample weight between incorporation of the polyester particles into the
gradual weighing.34 The weight variations of the viscose fabric. Based on the obtained results
sample between testing under atmospheric shown in Table 1, it can be noticed that the fabric
conditioning and after oven drying determine the GSM increased from 140 to 155 in the composites
moisture content of the composite. The following
formed utilizing 3% concentrations of polyester in
equation was used to compute the moisture content
percentage of the samples:35 the solution, compared to the neat viscose fabric.
This weight change is likewise related to the
(2)
increase in the add-on % to 10.71%. During the
where M, W1, and W2 denote the moisture content in first phase of padding, the dissolved polyester
percentage and specimen weight before and after penetrated into the spaces among the fibres due to
drying in grams, respectively. the squeezing operation accomplished using the
padding mangle. Subsequently, the polyester
Morphology analysis
solution gets enduringly sealed onto the viscose
The surface morphology of the viscose fabric and
VP composite samples was examined with a Zeiss Evo
fibre. This is reflected in the high add-on percent
18 Scanning Electron Microscope. Before testing, the of the coated fabric, compared to the viscose
specimens were coated with a thin layer of gold, fabric.
during 3 to 4 min, using a sputter coater at electron
accelerating voltage of 10 kV. Likewise, a Jiusion Spectroscopic characterization (FTIR)
microscope was used for the optical analysis of the The FTIR analysis was used to determine
specimens (1000x), according to standard ISO 25178. whether polyester particles were present in the
composites, and the spectra recorded for the
Mechanical properties materials are presented in Figure 2. The bands at
The tensile strength, Young’s modulus, elongation
3424 and 1015 cm-1 are attributed to
at break, and energy at break of the viscose fabric and
VP composite were calculated as per the ASTM
intermolecular -OH bound to C=O groups and
D3822–07 standards, using an H10KS testing machine OH out-of-plane bending in the terminal
(Hounsfield, UK), with a crosshead speed of 20 carboxylic groups in the polyester chains,
mm/min.36 Ten samples were tested, and the mean respectively.37 The band at 1710 cm-1 is attributed
results were recorded. Statistical analysis of tensile to the presence of the carboxylic group.
strength was performed by Weibull probability Anhydride groups are responsible for the
distribution using Minitab 18 software. The tensile polyester absorption band that emerges at 1953
strength was determined by Equation (3): cm-1.38
(3) Well-defined bands with typical cellulose
structures can be seen in the FTIR spectrum of the
where , , and denote the specimen tensile
viscose fabric at 3327, 2903, 1423, 1365, 1162
strength, maximum force at break, and cross-sectional
and 1016 cm-1.36,37 All characteristic peaks of the
area, respectively. The elongation at break and
Young’s modulus were determined from the test data.
viscose fabric experienced red shift intensity after
the incorporation of polyester. Although the peak
Spectrophotometry analysis at 1718 cm-1 assigned to the carbonyl group was
Colour difference tests of viscose and VP absent in the spectrum of the viscose fabric, it was
composite fabric were performed using a computer redshifted in the spectrum of the VP

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composite.39,40 Strong C-H bending (721 cm-1), determined using X-ray diffraction analysis. The
modest C-H stretching (2956 cm-1), and relatively recorded XRD patterns are shown in Figure 3.
significant C-C out-of-plane bending vibrations of The peaks typical of viscose are recorded at 2θ =
the benzene rings are all visible in the FTIR 15.38 and 29.74.41 As regards the composite, the
spectrum of polyester (871 cm-1). A characteristic diffraction peak at 2θ = 21.5° and plane 002 are
peak at 837 cm-1 in the VP composite and usually characterized by a narrowing of the peak
polyester FTIR fingerprint region was similarly intensity, typically indicating a highly ordered
absent from the spectrum of the pure viscose crystalline area.2 The results revealed that the
fabrics. In this approach, the composite fabric crystallinity of the VP composite was higher
began to behave similarly to polyester upon the (55.20%) than that of the viscose fabric (50.22%).
incorporation of polyester particles into the This can be explained by the fact that, upon the
viscose. The decreased peak intensity at 1112 cm- addition of polyester particles, they formed
1
, which is characteristic of viscose, also crystal structures after regeneration in the
demonstrates the reduced viscose-like behavior. amorphous regions of the base viscose fabric. In
this way, the incorporation of polyester improved
X-ray diffraction (XRD) study the crystallinity of the initial viscose.
The crystalline and amorphous characteristics
of the base viscose and of the VP composite were

Table 1
Physical and mechanical properties and moisture content of viscose and VP composite

Physical properties Mechanical properties

Moisture
Tensile Elongation Young’s Energy
Sample Matrix Add-on content
GSM strength at break modulus at break
weight (g) (%) (%)
(MPa) (%) (N/mm2) (J)
Viscose fabric 140 - - 11.14 113 19 8.55 0.4064
VP composite 155 15 10.71 13.10 136.5 17.5 8.5 0.38575

Figure 2: FTIR spectra of polyester, viscose and VP Figure 3: XRD patterns of viscose and VP composite
composite fabrics fabric

Thermal analysis absorbed moisture from the viscose. This weight

The thermal stability of the viscose and its loss represented 29% and 13.18% for the base
composite was investigated by thermogravimetric viscose and polyester-incorporating viscose
analysis (TGA) and derivative thermogravimetry composite, respectively. The difference in the
(DTG), as shown in Figures 4 (a and b), weight loss percentage is explained by the
respectively. The thermal degradation of the VP hydrophobic nature of polyester, as opposed to
composite is impacted by polyester deposition.2 the hydrophilicity of the viscose. The results also
According to the TG curves, an intial weight loss show that the viscose sample and VP composite
was observed in both samples in the range of 50– started to degrade at about 225 °C and 289 °C,
250 °C, which was due to the evaporation of the respectively, with significant thermogravimetric

413
MOHAMMAD ABUL HASAN SHIBLY et al.

peak maxima occurring at about 359.5 °C and SEM micrographs of the base viscose and VP
311.5 °C. The thermal stability of the viscose composite specimens are presented in Figure 5 (a)
fabric was high due to the cellulose content.42 and (b). It may be seen that the incorporation of
Also, the weight losses of the base viscose and the polyester into viscose fabric modifies the surface
VP composite at Tdmax were of 59.46% and morphology of the fibres. The viscose fabric
11.98%, respectively. initially shows typical smooth longitudinal fibrils,
with some light deposits of white particles,
Moisture content probably due to chemical residues (Fig. 5 (a)). On
The moisture content of the polyester- the other hand, the surface of the polyester-
incorpotating composite fabric was influenced by incorporating composite material reveals larger
the hydrophobic polyester incorporated in the deposits of polyester particles, which make the
viscose fabric. Thus, the moisture content of the surface appear rougher (Fig. 5 (b)). Similar results
samples was reduced from 13.10% to 11.14%, were also found in optical images taken with a
upon incorporation of the polyester particles. This laser microscope (Fig. 5 (c), (d)). The viscose
signifies that the hydrophilic viscose fabric has fabric serving as the base material has a striking
marginally turned hydrophobic, and the normally dark blue colour, while polyester particles are
characteristic hydrophilic property of the viscose white. As a result, the composite VP fabric
is not considered for the composite. appears to have a lighter shade than the base
viscose fabric.
Morphology analysis

(a) (b)

Figure 4: TGA (a) and DTG (b) curves of viscose fabric and VP composite samples

Mechanical properties (113.1 MPa), reaching a maximum tensile

The stress vs strain and tensile strength strength of 136.6 MPa. The elongation at break,
elongation percentages are shown in Figure 6 (a) on the other hand, droppted from 19% (for the
and (b), respectively, for the initial viscose and viscose) to 17.50% (for the VP composite). This
composite fabric samples. As expected, the can be explained by the presence of the polyester
addition of polyester boosted the tensile strength, particles on viscose fabric, which helped to
while reducing the elongation at break of the improve the tensile strength and reduce the
initial viscose. It is clear from Figure 6 (a) that the elongation percentage, while also enhancing the
tensile strength of the composite increased by crystallinity of the initial viscose, as discussed
20.80%, compared to the initial viscose specimen above.

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 Composites

(a) (b)

(c) (d)

Figure 5: SEM images of viscose (a) and VP composite (b); laser microscopic images of viscose (c)
and VP composite fabric (d)

(a) (b)

Figure 6: Stress vs. strain curve (a), tensile strength and elongation percentage (b) of viscose and
VP composite fabrics

The region of the elongation percentage and samples. The tensile strength results can be
the tensile strength of the materials have an observed to be within bounds and suit the
impact on the energy at break. The viscose fabric distributions entirely. The Weibull distribution
demonstrates the necessary energy at break, confirms that the tensile strength values are close
which is higher than that of the composite to the calculated mean values by this statistical
(0.038575 J), namely 0.04046 J. It may be analysis.
inferred from this experiment that the energy at
break, shown in Table 1, increases with the Visual appearance
elongation percentage. The change of fabric colour was measured
Figure 7 shows the study of the Weibull using the CIELAB computer colour-matching
probability distribution line for the tensile technique under illuminate D64 and U3500, and
strength of the viscose and VP composite the results obtained are presented in Table 2.

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MOHAMMAD ABUL HASAN SHIBLY et al.

Clearly, it may be noticed that the colour shade of composite material is influenced by the colour of
the viscose fabric decreased upon the addition of the polyester particles, which were initially white,
polyester, as shown by the drop in the values of affecting the values of the colour coordinates
∆L*, ∆a*, and ∆b*. Certainly, the colour of the determined for the composite sample.

Probability Plot of the 10 Viscose and VP Composite sample's Tensile Strength (MPa)
Normal - 95% CI
99
Variable
Viscose
95 VP Composite

90 Mean StDev N AD P
113.1 1.645 10 0.480 0.179
80
136.6 2.612 10 0.267 0.602
70
Probability

60
50
40
30
20

10

1
120 140
Tensile Strength (MPa)

Figure 7: Weibull probability distribution plot for tensile strength

Table 2
Color characteristics of viscose and VP composite specimens

Illum/Obs ∆L*/ISL ∆a* ∆b* ∆c*/cSc ∆H*/SH ∆Ecmc

D65 10 Deg -0.43 -0.37 -0.86 0.60 0.05 0.74
U3500 10 Deg -0.59 -0.44 -1.16 0.72 0.08 0.93

CONCLUSION support to conduct the study, and the National

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