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An eco-friendly microwave assisted recycling of cellulosic fabric

dyed with reactive red CL4BN and reactive black PLS

Taqdees Zahira, Sadia Noureen, Shaukat Ali, Hina Haq, Mubashar

Alam, Anam Akhtar, Muhammad Abdullah

PII: S0141-8130(25)03434-8
DOI: https://doi.org/10.1016/j.ijbiomac.2025.142882
Reference: BIOMAC 142882

To appear in: International Journal of Biological Macromolecules

Received date: 30 January 2024

Revised date: 25 March 2025
Accepted date: 4 April 2025

Please cite this article as: T. Zahira, S. Noureen, S. Ali, et al., An eco-friendly microwave
assisted recycling of cellulosic fabric dyed with reactive red CL4BN and reactive black
PLS, International Journal of Biological Macromolecules (2024), https://doi.org/10.1016/
j.ijbiomac.2025.142882

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© 2025 Published by Elsevier B.V.

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An Eco-friendly Microwave Assisted Recycling of Cellulosic Fabric Dyed

with Reactive Red CL4BN and Reactive Black PLS

Taqdees Zahiraa, Sadia Noureenb*, Shaukat Alia*, Hina Haqa, Mubashar Alama, Anam Akhtara,
Muhammad Abdullahc
a
Department of Chemistry, University of Agriculture, Faisalabad, Pakistan.
b
Department of Chemistry, University of Management and Technology, Sialkot, Pakistan
c
School of Sciences, National Textile University, Faisalabad 37610, Pakistan

Corresponding author email: Sadia Noureen: [email protected] Shaukat Ali :

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[email protected]

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Postal address: Department of Chemistry, University of Management and Technology, Sialkot,
Pakistan, Department of Chemistry, University of agriculture, Faisalabad, Pakistan.
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Graphical Abstract
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Abstract

The study was aimed to retain the quality of recycled cotton fabric by microwave-assisted color
stripping of faulty dyed cotton and waste of garments industry. Microwave assisted method
reduces the chemical consumption and coverts stripping time from hours to seconds.
Additionally, this is an eco-friendly approach as it also reduces the chemical wastes into
environment due to much less usage of chemicals in this process compare to conventional
stripping methods. Cotton fabric dyed with Reactive Red CL4BN and Reactive Black PLS dye
was subjected to acid and alkali hydrolysis followed by reductive and oxidative stripping in a
sequential manner. The sequential stripping resulted in up to 97-98% stripping efficiency. The

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tear strength of microwave-assisted acid hydrolysed sequentially stripped fabric increased by
17.7% and 24.1% in warp and weft wise directions respectively for Reactive Red CL4BN while

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for Reactive Black PLS which is increased by 14.5% and 29.3% in warp and weft-wise
direction respectively. The microwave-assisted alkali hydrolysed sequentially stripped fabric
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was found to be better in terms of tear strength and weight loss as compared to its respective
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conventional method. Additionally, using Fourier transform infrared spectrometry, the color
stripping was successfully investigated and validated through variations in cellulose and dye
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structures.

Keywords: Microwave-assisted, cellulose, recycling

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Introduction
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Global population expansion along with changes in people's lifestyles and fashion
culture has resulted in an increased demand for textile fabric (Hole and Hole 2020). Coloration
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or dyeing is the most significant process for manufacturing and decorating textiles with several
colors and colorful patterns (dos Santos et al. 2004; Maryam et al. 2019). In order to manage the
challenges in the competitive field of marketing, nearly one million tons of synthetic dyes are
being produced and used to dye the textile fabric to enhance its colorfulness and attractiveness
by industries around the globe (Chatha et al. 2012). The reactive group of the dye molecule
forms a strong covalent bond with the terminal hydroxyl group of the cellulose in the presence
of an alkali. Carbon atom of the dye molecule and oxygen atoms of the hydroxyl group in the
cellulose takes part in the formation of covalent bond (Rahman et al. 2015). Besides
conventional dyeing, many studies have been conducted to evaluate the resulting dyeing
properties by the effect of different radiations on the dye and fabric. Cotton fabric and reactive
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dye solution irradiated to UV radiations result in increased dye strength and improved dyeing
properties (Bhatti et al. 2014). Cotton and polyester fabric irradiated to UV radiations dyed
with UV irradiated reactive and dispersed dyes results in enhanced color strength of the fabric
(Bhatti et al. 2016). The effect of gamma radiations has been studied on cotton and Lawson dye
that extracted from leaves of henna. The effect of gamma radiations on cotton and dye solution
results not only in increased color strength but also in increased fastness properties rating
(Rehman et el. 2012). Ultrasonic radiation on wool and dye extracted from coconut coir called
Cocos nucifera results in better color yield and increased fastness ratings of the dyed wool
(Adeel et el. 2020). Polyester fabric and dispersed dye solution heated with microwave
radiations to evaluate the effect of microwave treatment on dyed polyester. The results show

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that microwaves increased washing, rubbing, fastness to light, and other color characteristics

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meanwhile reducing the dyeing conditions of dyed polyester fabric (Adeel et el. 2018). The dye
extracted from Arjun bark for dyeing of wool irradiated with microwaves gives darker shade.
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Microwaves also improve the functional behavior of the dye (Adeel et el. 2019).
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Nonetheless, many unwanted faults and defects often occur during the dyeing process in
textile dyeing industries (Oğulata and Balci 2007), due to variations in temperature and
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pressure, dyes variety, the change in pH of dyeing solution, change in auxiliaries, water
resources along with some missing operations and even certain difficulties of dyeing machines
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etc (Long et al. 2017; Xie et al. 2010). Consequently, faults and defects in dyeing including
color spots and dots, off-shade as well as various differentiations in color shades always occur
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and result in extremely low quality and worth of final textile products (Eren et al. 2016; Mariam
et al. 2024). Moreover, Small pieces of fabric are left as by-products from yarn and fabric
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manufacturing and also generated in garment cutting processes. This fabric scrap is recycled
after removing dye from it and converted into white cotton balls through various processes into
fabric twine and rope (Haslinger et al. 2019). Therefore, those faulty textile products that do not
fulfil color requirement norms must be amended (Alam et al. 2023; Akhtar et al. 2024; long et
al. 2017).

In general, the methods to correct the faulty dyed or recyclable fabric are determined by
the type of color flaw or defect. A levelling or continuous coloring process is often used for
minimal color difference and relatively uniform shade over the substrate surface. However,
most of the time, there is total unevenness in the shade of dyed products or they have huge
deviations in hue color, particularly for certain darker shades that are entirely incompatible with
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the standard of the product. As a result, in these circumstances, a color stripping process is
required to amend these defectively dyed or recyclable items (long et al. 2017; He at el. 2019;
Noureen et al. 2023). Stripping of dyes is a valued method generally used to erase dye from
recyclable and unequally dyed fabrics in textile industries (Mariam et al. 2024). Rendering to
the stripping treatment consequences on molecules of the dyes in the substrate matrix,
traditional color stripping techniques for textiles are largely split into two types (He et al. 2019;
Bhatia et al. 2017; Noureen et al. 2022 ). Destructive stripping is one of these stripping methods
in which destruction of the chemical structures of dye molecules occurs through a sequence of
chemical processes to remove the color on the substrates. The second is named as desorption

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stripping, that involves the desorption of the molecules of the dyes from dyed fabric by certain
types of surfactants and solvents without distortion of the conjugated chemical system of the

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dye molecule (Bhatia et al. 2017; Uddin et al. 2015). Nonetheless, destructive stripping is the
most commonly employed stripping method in actual fabrication. However, this regular and
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enormously used stripping approach generally requires high amounts of several oxidizing and
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reducing agents in an individual stripping method involving thiourea dioxide, sodium
hydrosulfite, decroline, sodium formaldehyde sulfoxylate, hydrogen peroxide, chlorine dioxide,
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dichromate salts and sodium hypochlorite (Chatha et al. 2012). Colorfulness of reactive dyes is
dissolved by breaking chemical bonds of chromophoric groups present in reactive dyes. Strong
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covalent bonds exist between fiber and reactive dye, therefore reactive dyes cannot be stripped
from cellulose fabric completely (Uddin et al. 2015). As cotton is a polymer, cellulose groups
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are intermingled and not fully exposed, therefore some of the ethereal linkages between
cellulose and some components of dyes like aromatic amines are retained. Due to retaining of
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these ethereal linkages, the crystallinity of the fabric is reduced, and the redyeing ability of
polymeric material is restricted because the sites are already occupied by previous dye
components and new dye molecules cannot attach with the cellulose to full extent. Furthermore,
these conventional stripping approaches often include high temperature, high liquor ratio and
longer exposure time with chemicals, all of which offer major threats to the fabric strength
(Long et al. 2017). As a result, developing some environmentally benign and long-lasting
stripping method is inevitable with high stripping efficiency and less damage to fabric for
improving the defects and faults in dyeing practices.

In current research, we have focused on environmental factor related to cotton waste

management. Because, Reusing waste cotton fabric from the garment industry and faulty dyed
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fabric from the dyeing industry after the color stripping process can have several important
benefits for both the environment and the industries involved: Textile industries generate a
significant amount of waste, including leftover fabric scraps and faulty dyed fabric. By reusing
these materials instead of disposing of them, the amount of waste sent to landfills is reduced,
mitigating the environmental impact of textile production. Reusing waste cotton fabric and
faulty dyed fabric reduces the need for virgin materials, such as raw cotton and dyes. This
conserves natural resources like water, energy, and land, which are all used in the production of
textiles. Reprocessing waste materials generally requires less energy than producing new
materials from scratch. By reusing cotton fabric and faulty dyed fabric, the energy required for
harvesting raw materials, manufacturing processes, and transportation is minimized, leading to

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overall energy savings and reduced greenhouse gas emissions. Reusing waste materials in

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textile production contributes to the development of a circular economy model, where materials
are kept in use for as long as possible, and waste and emissions are minimized. This sustainable
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approach helps to create a more resilient and environmentally friendly textile industry.
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This study involves the effectiveness of an alternate microwave-assisted process that consists of
a sequential acid and alkaline hydrolysis, sodium dithionite reductive and hydrogen peroxide
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oxidative treatments as a latent method for stripping of reactive dyes. The microwave radiations
being used for stripping is a time-saving technique. Microwaves are distributed evenly,
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providing uniform contact to any item that passes through them as compared to normal heating
because the dielectric substances with large dielectric constants are robustly affected by the
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rotation and vibration of permanent dipoles in the microwave field. The microwaves can easily
penetrate deeply into particles inside and they can be heated instantaneously giving even and
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efficient stripping in a short time. The fabric would be less damaged in a microwave-assisted
system because the contact time of fabric with chemicals shortens many folds as compared to
conventional treatment. Microwave heating stands out for its notable efficiency, benefiting both
reaction duration and product yield. By swiftly raising temperatures and ensuring uniformity
throughout the reaction mixture, it participate in remarkable acceleration in chemical reactions.
Consequently, products are obtained with heightened yields and within abbreviated timeframes.
The concept of microwave heating operates through the interaction between matter and
electromagnetic (EM) radiation. EM radiation consists of alternating electric and magnetic field
components, propagating perpendicular to each other. When electric fields interact with charged
particles, they induce rotation of the particles, a phenomenon typical in microwave radiation.
This rotation causes the charged particles to align themselves based on the polarity of the
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electric field, resulting in dielectric polarization. As the applied electric fields oscillate, dipoles
continuously realign, dissipating energy in the form of heat. This mechanism, known as the
"dielectric heating effect," forms the basis of microwave heating. Microwave radiation induces
rotational movement in polar molecules, aligning them according to the polarity of the
alternating electric field. As the electric field oscillates, the molecules continue to rotate and
realign. In liquids and solids containing polar molecules, this interaction leads to rapid changes
in molecular direction due to the concerted force exerted by the electric and magnetic fields.
This rapid movement generates internal friction and dielectric loss, manifesting as heat and
causing a rapid increase in temperature. This mechanism results in indirect heating. This has
prompted its deliberate adoption as an alternative energy source for empowering reaction

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processes (Rahman et al. 2015).

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The efficiency of microwave-assisted sequential treatment is evaluated with an outlook
to maximum removal of color characterised by colorimetric data, stripping efficiency, weight
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loss and tear strength of the microwave-assisted and conventionally stripped fabric and their re-
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dyeing ability. Additionally, using Fourier transform infrared spectrometry, the color stripping
was successfully investigated and validated through variations in cellulose structures and dye
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molecules.

1. Experimental
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2.1 Materials and chemicals

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Cellulosic cotton fabric was purchased from Noor Fatima Textile Industry, Faisalabad,
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Pakistan. Reactive Red CL4BN, Reactive Black PLS and Reactive Yellow C4GL dyes were
provided by Archroma, Faisalabad, Pakistan. Chemicals and reagents including sodium
hydrosulphite, sodium hydroxide, sodium sulphate, sodium bicarbonate, sodium silicate,
hydrochloric acid and hydrogen peroxide used were, of commercial grade. The microwave used
for stripping purpose was HD-36100E, 230V~50Hz and 2450MHz.

2.2 Dyeing of cotton with Reactive Red CL4BN and Reactive Black PLS dye

White cellulosic cotton fabric was dyed with 1% shade of Reactive Red CL4BN and
Reactive Black PLS dye based on fabric weight, keeping the fabric to liquor ratio 1:15. The
structure of Reactive Red CL4BN and Reactive Black PLS dye is given in figure 1 and 2
respectively. The dye solution was prepared with 50 g/L sodium sulphate (Na2SO4) salt and 75
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g/L sodium bicarbonate (Na2CO3) alkali. Exhaust dyeing method was used for dyeing at 80 oC
for 40 minutes. After dyeing, the fabric was cold washed and hot washed to remove any excess
dye.

Figure 1 Structure of Reactive Red CL4BN dye (C.I. number: 292775)

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Figure 2 Structure of Reactive Black PLS dye (C.I. number: 20505)

Dyeing mechanism of reactive dye:

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The dyeing of cellulose with reactive dye occurs in 3 steps:-

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1. Exhaustion or absorption
2. Fixation
3. wash-off
Dye absorption:
An electrolyte such as NaCl is introduced when cotton fabric is immersed in dye liquid to assist
the absorption of the dye. The electrolyte helps neutralize the negative charge formed on the
surface of the fabric and gives additional energy to enhance the absorption of the dye.
Therefore, when the fabric is immersed in dye liquor, the dye is exhausted onto the fabric.

Fixation:
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Fixation of dye refers to the reaction between the terminal –OH group of cellulose with the
reactive group of dye thus resulting a strong covalent bond with the cellulose. This important
phase is controlled by maintaining optimum pH with the addition of alkali like soda ash or
NaHCO3. It maintains proper pH in the dye bath and acts as the dye-fixing agent. The reaction
is as follows:

Alkali
D-SO2-CH2-CH2-OSO3Na + OH-Cell ————-→ D-SO2-CH2-CH2-O-Cell + NaHSO3
pH 10-12.5

Wash-off:

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Once the dyeing is finished, the material should be thoroughly washed to remove any excess or

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unfixed dye from the surface. This is required for level dyeing and high wash fastness. It is
completed through a succession of hot, cold, and soap solution washes.
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2.3 Stripping
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Various microwave-assisted chemical stripping methods were used for the stripping of
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Reactive Red CL4BN and Reactive Black PLS dye from cotton fabric including acid and alkali
hydrolysis, reductive stripping and oxidative stripping. The dyed fabric was sequentially
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stripped at optimized conditions of each treatment. Liquor ratio of 1:15 was kept in each
experiment and sample was continuously stirred throughout the treatment. Conventional
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treatments were also carried out for comparison.

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2.3.1 Alkali hydrolysis

Cotton fabric dyed with Reactive Red CL4BN and Reactive Black PLS dye was
hydrolysed with 8% sodium hydroxide (NaOH) for 20, 40, 60, 80, 100 and 120 seconds in
microwave. The dyed fabric was also conventionally hydrolysed with 8% sodium hydroxide
(NaOH) for 30 minutes.

2.3.2 Acid hydrolysis

Cotton fabric dyed with Reactive Red CL4BN and Reactive Black PLS dye was
hydrolysed with 4% hydrochloric acid (HCl) for 20, 40 and 60 seconds in microwave. The dyed
fabric was also conventionally hydrolysed with 4% hydrochloric acid (HCl) for 2 minutes.
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2.3.3 Reductive stripping

Cotton fabric dyed with Reactive Red CL4BN and Reactive Black PLS dye was
reductively stripped for 20, 40, 60, 80, 100 and 120 seconds in microwave. Reductive stripping
was carried out by using 30 g/L sodium dithionite and 20 g/L sodium hydroxide (Alam et al.
2023; Bigambo et al. 2020). Sodium dithionite was used as the reducing agent because of its
extensive use in both research laboratories and industries for reduction and stripping processes
(Bigambo et al. 2018). Reductive stripping was also carried out by conventional heating for 15
minutes.

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2.3.4 Oxidative stripping

Cotton fabric dyed with Reactive Red CL4BN and Reactive Black PLS dye was

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oxidatively stripped for 20, 40, 60, 80, 100 and 120 seconds in microwave. Oxidative stripping
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was carried out with 97.8 ml (35% vol.) hydrogen peroxide, 1.2 g/L sodium hydroxide, 7 g/L
sodium silicate and 1.8 g/L sodium carbonate (Alam et al. 2023; Bigambo et al. 2020).
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Oxidative stripping was also carried out by conventional heating for 30 minutes.
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2.3.5 Microwave-assisted sequential stripping

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Microwave-assisted sequential stripping was carried out on optimized pre-treated

samples of the alkali and acid hydrolysis. The optimized acid and alkali pre-treated samples
were first treated at optimized conditions of the reductive stripping and then treated at optimized
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conditions of the oxidative stripping. Sequential stripping was also carried out with
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conventional heating for comparison.

2.4 Measurements and Testing

2.4.1. Colorimetric analysis

The colorimetric data of stripped fabric was assessed by Spectra flash

Spectrophotometer (SF-650) at Government College University, Faisalabad, Pakistan. The color
can be demonstrated by means of three aspects including lightness, hue and saturation. In this
study, CIELAB was used for the color model and CMC was used for the tolerance system.
CIELAB consist of the values L*, a* and b* whereas CMC is a system of color difference
consisting of L*, h° and C*. L* symbolizes lightness, a* symbolizes red/green, b* symbolizes
yellow/blue, C* represents chroma and h° represents hue angle. h° is assessed in degrees around
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the circle, 0° being red, 90° being yellow, 180° being green and 270° being blue. The level of
saturation of a specific hue is defined by chroma. It indicates that how far a specific hue from a
neutral in the color space having similar lightness. Lightness determines the nearness of a
particular color to white. It is a sense of reflectance or the quantity of light reflected from a
surface, that distinguishes white items from grey and bright-colored objects from dark-colored
objects. The greater L* value represents a light color and a lower value of L* represents a dark
shade (Aleem et al. 2013).

2.4.2. Stripping percentage

Color strength of stripped cotton fabric was assessed by Spectra flash

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Spectrophotometer (SF-600). The K/S vales were determined at maximum absorption
wavelength λmax 550nm. K/S value was used to measure the color strength of dyed and stripped

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fabric which indicates the light absorption and light reflection ratio. The following formula was
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used to calculate the stripping percentage of stripped fabric (Bigambo et al. 2018).
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K K
value before stripping − value after stripping
% Stripping = S S x100
K
before stripping
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2.4.3. Quality of fabric

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The quality of microwave-assisted and conventionally stripped fabric was assessed by the
following tests.
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2.4.4. Weight loss

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Weight loss of microwave-assisted and conventionally stripped fabric was calculated by

measuring the fabric weight before and after the stripping treatment using an analytical balance.
The weight loss percentage was determined by using the following equation.

weight before stripping − weight after stripping

% weight loss = x100
weight before stripping

2.4.5. Tear strength

The tear strength of microwave-assisted and conventionally stripped fabric was

measured at National Textile University (NTU), Faisalabad following the method of the
International Organization for Standardization (ISO 13934-2: 2014) using UTS tester, 2019.
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The tear strength is used to determine the ability of the fabric to endure consequences of tearing
and cuts under tension.

2.4.6. FT-IR Analysis

The dyed fabric and microwave-assisted sequentially stripped cotton fabric was compared and
analysed using FT-IR. The FT-IR spectra of dyed and microwave-assisted sequentially stripped
fabric was obtained using KBr pellets, from 4000 cm-1 to 600 cm-1.

2.4.7. Re-dyeing

Microwave-assisted and conventionally stripped fabric was re-dyed to evaluate the re-

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dyeing ability of stripped fabric at National Textile University (NTU), Faisalabad. 2% shade of

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Reactive Yellow C4GL dye was used for the re-dyeing purpose. The structure of Reactive
Yellow C4GL is given in figure 3. The dye solution was prepared with 50 g/L sodium sulphate
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(Na2SO4) salt and 75 g/L sodium bicarbonate (Na2CO3) alkali and carried out in an HT dyeing
machine for 40 minutes at 80oC, keeping fabric to liquor ratio 1:15. Re-dyeing ability was
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assessed on the basis of color strength K/S values and colorimetric data.
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Figure 3. Structure of Reactive Yellow C4GL

4. Results and discussion

4.1 Colorimetric analysis

The colorimetric data of the untreated, microwave-assisted and conventional alkali and
acid hydrolysed, reductively and oxidatively stripped samples dyed with Reactive Red CL4BN
is given in table 1 and the colorimetric data of the untreated, microwave-assisted and
conventional alkali and acid hydrolysed, reductively and oxidatively stripped samples dyed with
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Reactive Black PLS is given in table 2. The value of L* ranges from 0 to 100. If the value of L*
is 0, it represents black and if L* has value of 100, it indicates white. The L* is a significant
colorimetric factor to assess the efficiency of stripping method and competence of the stripping
process (Oğulata and Balci 2007; Ghosh et al. 2018). The L* value of Reactive Red CL4BN
dyed fabric was 62.78 and L* value of Reactive Black PLS dyed fabric was 28.56. It is evident
from the tables, that L* value of microwave-assisted alkali hydrolysed fabric dyed with
Reactive Red CL4BN and Reactive Black PLS was increased by increasing the treatment time.
The increase in L* values shows that the lightness of treated fabric increased by increasing the
treatment time. It means that the dye molecules attached to the OH group of the cellulose might
be effectively removed by alkali leading to the higher L* values. The difference between L*

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values of microwave-assisted and conventionally stripped fabric was negligible for both the

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dyes. The acid hydrolysis showed no significant increase in L* values indicating that the acid
hydrolysis has no significant effect on the lightness. On the other hand, microwave-assisted
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reductive stripping showed abrupt increase in L* values even at low treatment time and L*
increased by increasing treatment time indicating the reductive effect of sodium dithionite on
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both dye molecules. Reductive stripping showed the highest lightness index among all the
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treatments. The effect of oxidative stripping on the lightness of Reactive Red CL4BN dyed
fabric was negligible as shown in table 1, but the effect of oxidative stripping on the lightness of
Reactive Black PLS was considerable as shown in table 2. Conventional oxidative stripping of
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Reactive Black PLS was remarkably increased. The L* values of oxidatively stripped fabric
indicated the inertness of Reactive Red CL4BN dye molecules to peroxide while Reactive Black
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PLS dye molecule is affected by peroxide.

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Table 1 Colorimetric data of microwave-assisted and conventionally stripped cotton fabric

dyed with Reactive CL4BN Red

Time
Treatment L* a* b* C* h°
(Sec)

0 62.78a 43.11a -10.98a 44.49a 345.71a

20 63.49b 38.46b -11.2b 40.06b 343.76b

40 71.01b 28.22b -8.47b 29.46b 343.29b

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Alkali 60 71.65b 25.59b -7.27b 26.6b 344.14b

hydrolysis
80 81.78b 9.36b 1.58b 9.49b 9.57b

100 83.0b 7.8b 2.61b 8.23b 18.52b

120 85.82b 1.7b 6.53b 6.75b 75.38b

30 min 86.58c 0.34c 7.95c 7.95c 87.52c

20 62.29b 45.06b -10.71b 46.32b 346.64b

40 62.43b 44.51b -10.48b 45.73b 346.75b

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Acid hydrolysis
60 63.03b 43.85b -10.53b 45.1b 346.49b

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2 min 63.45c 42.97c -10.43c 44.78c 346.45c

20 85.36b
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0.37b 16.68b 16.68b 88.72b

40 86.13b 0.05b 14.17b 14.17b 89.79b

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60 86.1b -0.15b 13.61b 13.61b 90.64b

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Reductive
80 86.76b -0.04b 13.15b 13.15b 90.19b
stripping
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100 86.74b -0.18b 12.65b 12.65b 90.82b

120 86.03b 0.23b 11.08b 11.08b 91.19b

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15 min 85.93c 0.57c 14.3c 14.32c 87.7c

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20 62.5b 41.5b -11.57b 43.09b 344.43b

40 62.22b 42.27b -12.2b 44b 343.9b

60 62.49b 42.47b -12.73b 44.34b 343.31b

Oxidative
80 61.85b 42.87b -12.04b 44.53b 344.3b
stripping
100 62.94b 41.84b -12.64b 43.71b 343.19b

120 62.83b 41.31b -12.06b 43.03b 343.73b

1 hr 64.74c 40.32c -12c 41.3c 342.23c

a
Untreated Dyed Fabric; b Microwave Assisted Stripped Fabric; c Conventionally Stripped
Fabric
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Table 1 shows that a* value of Reactive Red CL4BN dyed fabric i.e 43.11 was
enormously decreased by increasing the treatment time for alkali hydrolysis indicating shift
towards green, but as shown in table 2, a* value of Reactive Black PLS dyed fabric i.e -0.58
was increased by increasing the treatment time for alkali hydrolysis indicating shift towards red.
At the same time, the b* values of alkali hydrolysed fabric gradually increased from -10.98 for
untreated Reactive Red CL4BN dyed sample to 6.53 at 120 seconds indicating shift towards
blue and for Reactive Black PLS dyed sample b* values of alkali hydrolysed fabric increased
randomly showing blue shift. For acid hydrolysis, a* values increased leading the red shift and
b* values indicated no significant variation from untreated fabric for both dyes. Reductive
stripping of Reactive Red CL4BN dye resulted in green shift as it caused an immense decrease

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in a* values and reductive stripping of Reactive Black PLS caused an increase in a* values

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resulted in red shift. The b* values of reductively stripped fabric increased by increasing the
treatment time leading to blue shift of both dyes. Oxidative stripping of Reactive Red CL4BN
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resulted in no significant change in a* values while the b* values decreased leading to
yellowness. Oxidative stripping of Reactive Black PLS resulted in increased a* values and
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random increase in b* values.
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The C* value of Reactive Red CL4BN and Reactive Black PLS dyed fabric was 44.49
and 3.73 respectively. It is evident from table 1, that the C* values of alkali hydrolysis and
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reductive stripping of Reactive Red CL4BN decreased by increasing the treatment time
indicating that the saturation of samples has decreased where’s the C* values of acid hydrolysis
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and oxidative stripping of Reactive Red CL4BN slightly increased by increasing the treatment
time indicating that the saturation of samples has increased. Table 2 shows that the C* values of
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alkali hydrolysis and reductive stripping of Reactive Black PLS increased by increasing the
treatment time and acid hydrolysis resulted in slight decrease in C* values. Oxidative stripping
of Reactive Black PLS show random change in saturation.

Table 2 Colorimetric data of microwave-assisted and conventionally stripped cotton fabric

dyed with Reactive Black PLS

Time
Treatment L* a* b* C* h°
(Sec)

Alkali 0 28.56a -0.58a -3.68a 3.73a 260.97a

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hydrolysis
20 31.29b -0.94b -4.10b 4.2b 257.02b

40 59.90b 0.70b 0.19b 3.73b 14.91b

60 62.75b 2.72b 2.53b 3.71b 42.95b

80 70.63b 5.09b 6.20b 8.02b 50.63b

100 75.46b 4.73b 6.24b 7.83b 52.81b

120 80.03b 2.84b 4.46b 5.29b 57.44b

40 min 84.59c 0.86c 5.34c 5.4c 80.85c

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20 27.92b -0.15b -3.43b 3.43b 267.52b

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40 28.58b -0.22b -3.62b 3.62b 266.57b
Acid hydrolysis -p
60 28.24b 0.09b -3.53b 3.53b 271.48b

2 min 28.14c -0.03c -3.32c 3.32c 269.56c

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20 62.57b 7.94b -1.50b 8.08b 349.34b

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40 64.51b 7.66b -1.32b 7.77b 350.25b

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60 73.39b 4.00b -1.04b 4.13b 345.47b

Reductive
80 78.30b 1.62b 0.46b 1.69b 16.01b
stripping
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100 80.33b 0.68b 4.72b 4.77b 81.74b

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120 83.77b 0.75b 2.39b 2.50b 72.55b

15 min 0.1608c 85.04c -1.83c 2.40c 3.02c

20 28.30b 0.13b -3.86b 3.86b 268.1b

40 30.67b 0.42b -4.57b 4.59b 275.3b

60 32.50b 2.44b -2.53b 3.51b 313.95b

Oxidative
stripping
80 36.37b 4.25b 0.03b 4.25b 320.43b

100 32.33b 2.10b -1.74b 2.73b 320.48b

120 36.33b 3.45b 0.13b 3.45b 320.18b

 Journal Pre-proof

40 min 62.39c 18.79c 25.60c 31.75c 53.73c

a
Untreated Dyed Fabric; b Microwave Assisted Stripped Fabric;c Conventionally Stripped
Fabric
Value of ho of Reactive Red CL4BN and Reactive Black PLS dyed fabric was 345.71
and 260.97 respectively. Alkali hydrolysis decreased the ho values by increasing the treatment
time where’s acid hydrolysis resulted in a slight increase in h* values in both dyes. Reductive
stripping of Reactive Red CL4BN resulted in a major decrease in ho values where’s ho values of
Reactive Black PLS increased at low treatment time and decreased at hight treat time with
reductive stripping. Oxidative stripping caused a slight decrease in h o values for Reactive Red
CL4BN dye and caused an increase in ho values of microwave-assisted stripping and a major

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decrease in conventional stripping as shown in table 1 and 2.

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Table 3 Colorimetric data of sequentially stripped fabric
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Dye Treatment L* a* b* C* ho
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Untreated 62.78a 43.11a -10.98a 44.49a 345.71a
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Reactive Red acid 87.02b 0.27b 10.15b 10.16b 88.49b

hydrolysis+
CL4BN
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reduction+
87.37c 1.81c 2.16c 2.82c 50.16c
oxidation
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acid
87.05b 0.46b 3.58b 3.61b 82.63b
Reactive Black hydrolysis+
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reduction+
PLS
oxidation 86.97c 0.62c 4.54c 4.58c 82.18c

Reactive Red alkali

88.3b 0.27b 3.9b 3.9b 88.34b
hydrolysis+
CL4BN
reduction+
oxidation 88.9c 0.25c 1.9c 1.92c 82.4c

alkali
88.30b 0.04b 2.66b 2.66b 89.18b
Reactive Black hydrolysis+
reduction+
PLS
oxidation 88.24c 0.24c 1.89c 1.90c 82.70c
a
Untreated Dyed Fabric; b Microwave Assisted Stripped Fabric; c Conventionally Stripped
Fabric
 Journal Pre-proof

The colorimetric data of the microwave-assisted and conventional acid and alkali
hydrolysed sequentially stripped fabric dyed with Reactive Red CL4BN and Reactive Black
PLS are given in table 3. The comparison of the L* values of acid and alkali hydrolysed
sequentially stripped fabric dyed with Reactive Red CL4BN and Reactive Black PLS to their
respective untreated fabric indicates that the L* value of stripped fabric has remarkably
increased and slightly more for alkali hydrolysed sequentially stripped fabric. It means that
the dye molecules attached to the OH group of the cellulose may be effectively removed
leading to the higher L* values. The difference between L* values of microwave-assisted and
conventionally stripped fabric was negligible for both dyes. The a* value of acid and alkali
hydrolysed sequentially stripped fabric dyed with Reactive Red CL4BN was enormously

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decreased leading to green shift while a* value of acid and alkali hydrolysed sequentially

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stripped fabric dyed with Reactive Black PLS was slightly increased leading to red shift.
While b* values of acid and alkali hydrolysed sequentially stripped fabric increased for both
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dyes, indicating shift towards blue. The shift towards blue was more for acid hydrolysed
sequentially stripped fabric. The values of C* and ho decreased after acid and alkali
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hydrolsed sequential stripping indicating that the saturation of samples has decreased for
both dyes.
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2.5 Stripping percentage

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The figure 4 shows stripping percentage by alkali hydrolysis of Reactive Red CL4BN and
Reactive Black PLS evaluated by spectra flash spectrophotometer. The stripping efficiency of
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stripped fabric for each treatment time was calculated by using formula of stripping efficiency.
Alkali hydrolysis of the dyed fabric caused an enormous decrease in K/S value, demonstrating
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the sensitivity of the dye chromophores of Reactive Red CL4BN and Reactive Black PLS and
their covalent bonding to cellulose fabric, to alkaline hydrolysis. The K/S value of untreated
fabric was 1.9331 and 6.7134 for Reactive Red CL4BN and Reactive Black PLS dyed fabric
respectively. It is evident from figure 4 that the K/S values of both dyes decreased by alkali
hydrolysis. Microwave-assisted alkali hydrolysis of Reactive Red CL4BN and Reactive Black
PLS resulted in maximum stripping efficiency of 95.5% and 96.03% respectively at 120
seconds. Conventional alkali hydrolysis of Reactive Red CL4BN and Reactive Black PLS dyed
fabric for 30 mintues resulted in 96.2% and 97.12% stripping respectively.
 Journal Pre-proof

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Figure 4: Stripping percentage of Alkali hydrolysis with 8% sodium hydroxide (NaOH)
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The figure 5 shows the stripping percentage by acid hydrolysis of Reactive Red CL4BN
and Reactive Black PLS. Acid hydrolysis of both dyes showed negligible change in K/S values
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demonstrating the resistance of the dye chromophores of Reactive Red CL4BN and Reactive
Black PLS and their covalent bonding to cellulose fabric, to acid hydrolysis. Microwave-
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assisted acid hydrolysis of Reactive Red CL4BN resulted in stripping efficiency of 2.07% at 60
seconds and conventional acid hydrolysis for 2 muntiues resulted in 1.86% stripping efficiency.
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Acid hydrolysis of Reactive Black PLS resulted in an increased K/S values from dyed fabric.
Microwave-assisted acid hydrolysis of Reactive Black PLS resulted in stripping efficiency of -
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0.6% at 60 seconds and conventional acid hydrolysis for 2 minutes resulted in -2.78% stripping
efficiency.
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Figure 5: Stripping percentage of Acid hydrolysis with 4% Hydrochloric acid (HCl)
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The figure 6 shows the K/S values of oxidative stripping of Reactive Red CL4BN and
Reactive Black PLS evaluated by spectra flash spectrophotometer. Oxidative stripping of the
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dyed fabric resulted in a small decrease in K/S value, demonstrating the effect of hydrogen
peroxide on the dye chromophores of Reactive Red CL4BN and Reactive Black PLS and their
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covalent bonding to cellulose fabric. Microwave-assisted oxidative stripping of Reactive Red

CL4BN and Reactive Black PLS resulted in maximum stripping efficiency of 9.29% and 32.6%
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respectively at 120 seconds. Conventional oxidative stripping of Reactive Red CL4BN and
Reactive Black PLS dyed fabric for 1 hour resulted in 40.7% and 67.19% stripping respectively.
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 Journal Pre-proof

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Figure 6: Stripping percentage of oxidative stripping
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The fiure 7 shows the K/S values of reductive stripping of Reactive Red CL4BN and
Reactive Black PLS evaluated by spectra flash spectrophotometer. Reductive stripping of the
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dyed fabric caused an enormous decrease in K/S values, demonstrating the sensitivity of the dye
chromophores of Reactive Red CL4BN and Reactive Black PLS and their covalent bonding to
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cellulose fabric, to reductive stripping. The K/S value of untreated fabric was 1.9331 and 6.7134
for Reactive Red CL4BN and Reactive Black PLS dyed fabric respectively. It is evident from
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Figure 7 that the K/S values of both dyes decreased by reductive stripping. Microwave-assisted
reductive stripping of Reactive Red CL4BN and Reactive BlackPLS resulted in maximum
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stripping efficiency of 88.2% and 97.42% respectively at 120 seconds. Conventional reductive
stripping of Reactive Red CL4BN and Reactive Black PLS dyed fabric for 15 minutes resulted
in 84.9% and 96.08% stripping respectively. Reductive stripping of Reactive Black PLS showed
more stripping efficiency than Reactive Red CL4BN.
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Figure 7: Stripping percentage of Reductive Stripping
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The figure 8 shows the stripping percentage of sequential stripping of Reactive Red
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CL4BN and Reactive Black PLS dyed fabric. Acid hydrolysis of Reactive Red CL4BN dyed
fabric for 60 seconds resulted in minimal decrease in K/S values, from 1.9331 to 1.893 resulting
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in 2.07% stripping. Acid hydrolysis of Reactive Black PLS dyed fabric for 60 seconds resulted
in an increased K/S value from 6.7134 to 6.7543. The increased K/S value by acid treatment is
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due to the fact that acid causes chromophores to appear on the surface of the fabric leading to
increased color strength. When cotton cellulosic fibers are treated with acid, the glycosidic
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linkages in the cellulose are broken and the degree of polymerization (DP) declines. Acid
hydrolysis of cotton is affected by hydrogen bonding existing in the macrostructure of
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crystalline cellulose as supramolecular structures of cellulose are built on several types of

hydrogen bonds between OH groups. Hydrogen bonding is considered to be main aspect
controlling the physical properties and structure of cotton cellulosic fabric. The cellulose
structure has various types of hydrogen bonding including intermolecular and intramolecular
hydrogen bonding present between the cellulose surface and molecules of water. Intramolecular
hydrogen bonding has shown to contribute to some physical features of cellulosic fabric
including solubility and crystallinity in different polar solvents as well as relative reactivity of
cellulosic fabric. Because of the strength of these hydrogen bonds, cellulose is resistant to
assault by acidic catalytic components in aqueous solution. The hydrogen bonds resist the
release of glucose by hindering the contact of the catalyst to the active site of cellulose. The
hydrogen bonds become weak when glycosidic bonds of cellulose are being randomly attacked
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by hydronium ions in liquid in the catalytic process of acid hydrolysis. Glucose and oligomers
are rapidly liberated to bulk liquid when hydrogen and glycosidic bonds are broken. Acids act
as dehydrogenated agents, thus remove water molecules from fabric and helps the dye
molecules to appear on the surface from bulk and result in the burning of the fabric. The
appearance of dye molecules on the surface makes it easier to strip off the dye with further
treatment (Xiang et al. 2003).

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Figure 8 Stripping percentage of microwave-assisted and conventional sequential color

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stripped fabric
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Alkali hydrolysis of Reactive Red CL4BN dyed cotton fabric for 120 seconds caused an
enormous decrease in K/S value, demonstrating the sensitivity of the dye chromophores of Red
CL4BN reactive dye and their covalent bonding to cellulose fabric, to alkaline hydrolysis. The
alkali hydrolysis decreased the K/S value of the cellulose fabric from 1.9331 to 0.0797 resulting
in 95.9% stripping. Alkali hydrolysis of Reactive Black PLS dyed cotton fabric for 120 seconds
caused an enormous decrease in K/S value from 6.7134 to 0.2664 resulting in 95.9% stripping.
Reactive dyes form covalent bonds with glucoside hydroxyls in cellulose. Therefore, reactive
dyes are very difficult to extract or destruct among all other dye types. Alcoholic groups present
in the subunits of glucose in the backbone of cellulose get ionized in an alkaline environment
behaving as a weak acid. When cellulose is dyed, the -OH groups in alcohols are occupied by
molecules of reactive dyes. During alkaline hydrolysis, cellulose gives the maximum number of
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-OH groups which has been engaged in covalent bonding with the cotton cellulose because of
the dye reduction reaction of NaOH on the cotton cellulose. Moreover, it also attacks the
crystalline area of cellulose and results in enhancing the probability of -OH groups (Uddin et al.
2015).

However, subsequent alkaline dithionite reductive stripping for 120 seconds on acid
hydrolysed fabric dyed with Reactive Red CL4BN substantially lowered the K/S value to
0.0579 resulting in 97.0% stripping. Subsequent alkaline dithionite reductive stripping for 120
seconds on alkali hydrolysed fabric dyed with Reactive Red CL4BN substantially lowered the
color strength of fabric leading to K/S value of 0.0571 resulting in 97.04% stripping. And

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subsequent alkaline dithionite reductive stripping for 120 seconds on acid hydrolysed fabric
dyed with Reactive Black PLS substantially lowered the color strength leading to K/S value to

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0.1519. Subsequent alkaline dithionite reductive stripping for 120 seconds on alkali hydrolysed
fabric dyed with Reactive Black PLS substantially lowered the color strength of fabric leading
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to K/S value of 0.121. The reductive potential of sodium dithionite is related to the dithionite
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radical anion. This radical anion is formed by the homolytic breakdown of the S-S bond. This
bond breaking results in the formation of a free radical anion, that seems to be the initial
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transient specie in dithionite oxidation and remains in equilibrium with the dithionite ion as
represented in the following Equation. The formation of transient specie of dithionite free
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radical anion has been proved by electron spin resonance (ESR) spectroscopy (Housecroft et al.
2008).
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Sodium dithionite having reducing properties results in the destruction of the conjugated
system of the dye molecules. Hence, dithionite reduces the azo groups and converts them into
colorless amines by giving electrons. The reduction of one azo group requires two moles of
dithionite as follows (Jozi et al. 2022).

Further treatment of oxidative hydrogen peroxide for 120 seconds on acid hydrolysed
and reductively stripped fabric dyed with Reactive Red CL4BN resulted in further decrease in
K/S values to 0.0493 giving the stripping percentage of 97.44%. Further treatment of oxidative
hydrogen peroxide for 120 seconds on alkali hydrolysed and reductively stripped fabric dyed
 Journal Pre-proof

with Reactive Red CL4BN resulted in further decrease in K/S values to 0.0491 giving the
stripping percentage of 97.46%. And further hydrogen peroxide oxidative stripping for 120
seconds on acid hydrolysed and reductively stripped fabric dyed with Reactive Black PLS
resulted in further decrease in K/S values to 0.1443 giving the stripping percentage of 97.85%.
Further hydrogen peroxide oxidative stripping for 120 seconds on alkali hydrolysed and
reductively stripped fabric dyed with Reactive Black PLS resulted in further decrease in K/S
values to 0.1066 giving the stripping percentage of 98.41.

The hydrogen peroxide oxidative treatment caused a very little reduction in the values of
K/S. There are more than one functional group in the dye (Benkhaya et al. 2020). As a result,

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more than one potential bond with the hydroxyl group of cellulose is formed. As a result, it's
conceivable that the treatment will only break one or two of the dye-fiber bonds, leaving the

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remaining bonds connected to the cellulose fiber and preventing degradative chemicals to
access the chromophore (Yang et al. 2021). Therefore, oxidation treatment resulted in relatively
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less reduction in color strength.
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In the conventional method of acid hydrolysed sequential stripping of Reactive Red
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CL4BN dyed fabric, acid treatment for 2 minutes decreased the K/S value of Reactive Red
CL4BN dyed fabric to 1.897 resulting in 1.86% stripping and successive alkaline dithionite
reductive stripping for 15 minutes considerably lowered the color strength of fabric resulting in
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a K/S value of 0.0657 resulting in 96.6% stripping. Additional hydrogen peroxide oxidative
treatment for 1 hour caused further decrease in K/S value to 0.0641 giving the stripping
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percentage of 96.68%. In the conventional method of acid hydrolysed sequentially stripped

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fabric, acid treatment of Reactive Black PLS dyed fabric for 2 minutes increased the K/S value
from 6.7134 to 6.9007. Further alkaline dithionite reductive stripping for 15 minutes
considerably lowered the color strength of fabric resulting in a K/S value of 0.1774. Additional
hydrogen peroxide oxidative treatment for 1 hour caused further decrease in K/S value to
0.1436 giving the stripping percentage of 97.86%.

In the conventional method of alkali hydrolysed sequential stripping of Reactive Red

CL4BN dyed fabric, alkali hydrolysis for 15 minutes resulted in K/S of 0.0734 resulting in
96.2% stripping and successive alkaline dithionite reductive stripping lowered the color strength
of fabric resulting in a K/S value of 0.0694 resulting in 96.4% stripping. Additional hydrogen
peroxide oxidative stripping caused further lowering of the value of K/S to 0.0459 giving the
stripping percentage 97.68%. In the conventional method of alkali hydrolysed sequential
 Journal Pre-proof

stripping of Reactive Black PLS dyed fabric, alkali hydrolysis for 15 minutes resulted in K/S of
0.1927 and successive alkaline dithionite reductive stripping lowered the color strength of fabric
resulting in a K/S value of 0.1355. Additional hydrogen peroxide oxidative stripping caused a
further lowering of the value of K/S to 0.1041 giving the stripping percentage 98.45%.

Figures 9 and 10 show the visual results of the microwave-assisted and conventionally
stripped fabric. The stripping efficiency clearly demonstrates that microwave-assisted stripping
in both experiments, shows better results than conventional treatments in less treatment time.

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Figure 9 Visual presentation of microwave-assisted and conventionally stripped fabric dyed

with Reactive Red CL4BN
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(a). Untreated dyed fabric (b). Microwave-assisted acid hydrolysis (c). Microwave-assisted acid
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hydrolysis + reduction (d). Microwave-assisted acid hydrolysis + reduction + oxidation (e).

Conventional acid hydrolysis (f). Conventional acid hydrolysis + reduction (g). Conventional acid
hydrolysis + reduction+ oxidation
(h). Microwave-assisted alkali hydrolysis (i). Microwave-assisted alkali hydrolysis + reduction (j).
Microwave-assisted alkali hydrolysis + reduction + oxidation (k). Conventional alkali hydrolysis (l).
Conventional alkali hydrolysis + reduction (m). Conventional alkali hydrolysis + reduction +
oxidation.
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Figure 10 Visual presentation of microwave-assisted and conventionally stripped fabric dyed

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with Reactive Black PLS
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(a). Untreated dyed fabric (b). Microwave-assisted acid hydrolysis (c). Microwave-assisted acid
hydrolysis + reduction (d). Microwave-assisted acid hydrolysis + reduction + oxidation (e).
Conventional acid hydrolysis (f). Conventional acid hydrolysis + reduction (g). Conventional acid
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hydrolysis + reduction+ oxidation
(h). Microwave-assisted alkali hydrolysis (i). Microwave-assisted alkali hydrolysis + reduction (j).
Microwave-assisted alkali hydrolysis + reduction + oxidation (k). Conventional alkali hydrolysis (l).
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Conventional alkali hydrolysis + reduction (m). Conventional alkali hydrolysis + reduction +

oxidation.
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4.3 Weight loss

The quality of microwave-assisted and conventionally stripped fabric dyed with

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Reactive Red CL4BN and Reactive Black PLS was also assessed by calculating the weight loss
percentage (Chatha et al. 2011). The weight loss of microwave-assisted and conventional, acid
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hydrolysed sequentially stripped cellulose fabric dyed with Reactive Red CL4BN was observed
to be 1% and 1.75% respectively and weight loss of microwave-assisted and conventional, acid
hydrolysed sequentially stripped cellulose fabric dyed with Reactive Black PLS was observed to
be 1.25% and 1.75% respectively as shown in figure 11. Where’s, weight loss for microwave-
assisted and conventionally, alkali hydrolysed sequentially stripped cellulose fabric dyed with
Reactive Red CL4BN was observed to be 0.25% and 2.75% respectively and weight loss of
microwave-assisted and conventional, alkali hydrolysed sequentially stripped cellulose fabric
dyed with Reactive Black PLS was observed to be 0.1% and 2.5% respectively. This statistical
study shows that the weight loss in conventionally stripped fabric was substantially more as
compared to microwave-assisted treatment for both dyes.
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Figure 11 Weight loss of microwave-assisted and conventionally stripped fabric
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(A). Microwave-assisted acid hydrolysis followed by reduction and oxidation
(B). Conventional acid hydrolysis followed by reduction and oxidation
(C). Microwave-assisted alkali hydrolysis followed by reduction and oxidation
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(D). Conventional alkali hydrolysis followed by reduction and oxidation

4.4 Tear strength

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Tear strength is described as the amount of force in newtons required to initiate or to

linger to tear the fabric, in either warp-wise or weft-wise direction, under certain conditions.
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The tear strength or tear resistance test is used to assess that how much the fabric can endure the
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cuts or tearing effects under tension.

Table 4 Tear strength of untreated, microwave assisted and conventional sequentially stripped
fabric

Dye Treatment Warp Weft

Standard 6.2a 5.8a

7.3b 7.2b
Reactive Red Acid+ Reduction+
CL4BN Oxidation
5.6c 5.3c
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7.4b 6.8b
Reactive
Black PLS
5.9c 5.7c

6.3b 5.9b
Reactive Red
CL4BN
5.2c 4.9c
Alkali+ Reduction+
Oxidation
7.1b 7.5b
Reactive
Black PLS
6.1c 5.7c

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a
Untreated Dyed Fabric; b Microwave Assisted Stripped Fabric; c Conventionally Stripped
Fabric

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Table 4 illustrates the tear strength of fabric in both warp-wise and weft-wise directions.
It is clear from the data that warp and weft values of the fabric varied for every treatment. Tear
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strength depends on the yarn strength and yarn mobility in the fabric structure. The yarn
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mobility further depends on the yarn twist, fiber and yarn smoothness. Fabric weave being same
has effect in this work. For standard fabric, warp-wise value and weft-wise value was 6.2 N and
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5.8 N respectively. It is evident that the warp-wise tear strength of the cellulose is more than the
tear strength of cellulose in weft-wise direction which indicates that the warp yarns are much
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greater than weft yarns, leading to the greater strength of warp yarn as compared to the weft
yarn. Hence, the cellulose fabric in the warp-wise direction is more stable.
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Microwave assisted acid hydrolysed sequential stripping increased the tear strength
values for both Reactive Red CL4BN and Reactive Black PLS in both warp and weft-wise
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direction as shown in Table 4. This has increased by 17.7% and 24.1% for Reactive Red
CL4BN and 19.3% and 17.2% for Reactive Black PLS for both directions respectively.
Contrarily, conventional acid hydrolysed sequential stripping decreased the tear strength values
for both Reactive Red CL4BN and Reactive Black PLS in both warp and weft-wise direction.
This has decreased by 9.6% and 8.6% for Reactive Red CLB4BN and 4.8% and 1.7% for
Reactive Black PLS for both directions respectively.

On the other hand, similar trend was observed for alkali hydrolysed sequential stripping.
Microwave assisted alkali hydrolysed sequential stripping increased the tear strength values for
both Reactive Red CL4BN and Reactive Black PLS in both warp and weft-wise direction as
shown in Table 4. This has increased by 1.6% and 1.7% for Reactive Red CL4BN and 1.6% and
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29.3% for Reactive Black PLS for both directions respectively. Conventional alkali hydrolysed
sequential stripping decreased the tear strength values for both Reactive Red CL4BN and
Reactive Black PLS in both warp and weft-wise direction. This has decreased by 16.1% and
15.5% for Reactive Red CLB4BN and 1.6% and 1.8% for Reactive Black PLS for both
directions respectively.

It is evident from the above data that microwave-assisted treatment increased the yarn
strength which raised the tear strength in both warp and weft directions whereas conventional
treatment reduced the tear strength. Cotton fabric shrinks due to the tension that is applied to its
yarn, the tension is released by the microwave heat which causes the fabric to be reduced to its
natural size, therefore, tear resistance of the fabric increased (El-Sayed et al. 2020). The

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comparatively less increase of tear strength in alkali hydrolysed sequentially stripped fabric was

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due to the high concentration of alkali as compared to acid concentration as we used 4%
concentration of acid and 8% concentration of alkali. While in conventional stripping, the
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contact time of chemicals with the fabric was very long, the fabric gets weakened by long time
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exposure to chemicals and its strength decreased.

4.5 Exploring the microwave-assisted color stripping by FT-IR characterization

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As a result of the experiments and discussions above, it was discovered that the
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microwave-assisted stripping technique was extremely effective at removing the dye from
Reactive Red CL4BN dyed cotton substrate. The further exploration of some fundamental
knowledge regarding microwave radiations used for color stripping reactive dyed substrates and
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their impact on fiber macrochains is therefore quite intriguing. As a result, an FT-IR

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characterization for the samples dyed with Reactive Red CL4BN and Reactive Black PLS dye
before and after being stripped at the defined conditions in the microwave-assisted alkali
hydrolysed sequential stripping system was carried out. Evident changes in the FT-IR spectra
of the microwave-assisted sequentially stripped cotton samples were seen by comparing them to
the dyed sample (He et al. 2021).
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A
B
102

1627
100

98 3338

1421
96 2848
% Transmittance

2914 1366 1312

94

92

90

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88

86

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84

4000 3500 3000

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2500 2000 1500 1000

Wavenumber cm-1
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Figure 12 FT-IR spectra of Reactive Red CL4BN dyed and alkali hydrolysed microwave-
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assisted sequentially stripped cotton fabric

(A). Reactive Red CL4BN dyed fabric

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(B). Microwave-assisted alkali hydrolysed sequentially stripped fabric

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A
100 B

98 1363

3314
1641

96 1420

2918 2849
1363 1313
% Transmittance

94

92

90

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86 -p
4000 3500 3000 2500 2000 1500 1000
-1
Wavenumber cm
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Figure 13 FT-IR spectra of Reactive Black PLS dyed and alkali hydrolysed microwave-assisted
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sequentially stripped cotton fabric

(A). Reactive Black PLS dyed fabric

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(B). Microwave-assisted alkali hydrolysed sequentially stripped fabric

As shown in Figure 12 and 13, the adsorption band of Reactive Red CL4BN dyed fabric
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at 3338 cm-1 and adsorption band of Reactive Black PLS dyed fabric at 3314 cm-1 that is
primarily attributed to the stretching vibration of the hydroxyl groups (OH, nOH) from the
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cotton substrate as well as an association of NH (nNH) stretching vibration from the fixed
reactive dyes (Long et al. 2017) , was widened and shifted (or even split) to a higher
wavenumber for microwave-assisted stripped fabric (Alam et al. 2023; Akhtar et al. 2024).
These variations clearly demonstrate that a number of microwave-assisted reactions through
some attacks from those active oxidation species actually took place on the reactively dyed
cotton substrate for the breakdown of the molecules of Reactive Red CL4BN and Reactive
Black PLS dye and also showed some influence on the functional groups, i.e the hydroxyl
groups (-OH) in the cellulose. Specifically, these potent species may react and oxidize the imino
(-NH-) groups present in the Reactive Red CL4BN and Reactive Black PLS dye molecules and
also the chromophores of the fixed Reactive Red CL4BN dye and Reactive Black PLS into
small fragments or even into inorganic components with a subsequent departing away from the
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substrate. Since the hydroxyl groups (-OH) and imino (-NH-) groups from dye molecules were
stripped at different rates, the hydrogen bonding system could be interrupted and their
intermolecular and intramolecular interactions could also be weakened or decreased. As a result,
this band widened and shifted to a higher wavenumber (He et al. 2019). However, a very small
variation in the positions of bands at 2914 cm-1 and 2848 cm-1 for the Reactive Red CL4BN
dyed sample were obtained in case of microwave-assisted alkali hydrolysed sequentially
stripped fabric. For the Reactive Black PLS dyed fabric, absorption band at 2918 cm-1 and 2849
cm-1 slightly shifted towards higher wavenumber by microwave-assisted alkali hydrolysis
sequential stripping. These bands were primarily referred to the symmetrical and asymmetrical
stretching vibrations of the CH2- and _C_H- chains in the macrochains of the cellulose fibres

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(Long et al. 2017). The highly inert properties of the -CH2- groups in the color stripping

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system, however, may be the reason why less or no change in these adsorption bands was seen
on the substrates before or after a color stripping. As depicted in Figure 12, a weak adsorption
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peak at 1627 cm-1 was found for the Reactive Red CL4BN dyed sample and a weak adsorption
peak at 1641 cm-1 was found for the Reactive Black PLS dyed sample. This peak was likely
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caused by the fixed reactive dye molecules' stretching vibrations of - C=N- (υC=N) as well as
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bending and deformation vibrations in the plane of N-H (δN–H). Then, a continuous increase in
the height of adsorption peak and an evident shift of the peak position to 1642 cm-1 was
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observed with the alkali hydrolysed sequential stripping for Reactive Red CL4BN. For
microwave-assisted alkali hydrolysed sequentially stripped fabric dyed with Reactive Black
PLS adsorption peak shifted to 1652 cm-1. These results demonstrate that some interactions
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between the Reactive Red CL4BN and Reactive Black PLS dye molecules and the species
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created by microwave-assisted sequential stripping resulted in the formation of additional amino

(-NH2), imino (-NH-), _C=N-, and even amide groups (-C(=O)-NH-) on the stripped samples.
Therefore, the increased and combined bending, deformation vibrations of N–H (δN–H), the
stretching vibrations of – C=N– (υC=N) and even C=O (υC=O) from amide groups, resulted in the
increased intensity of adsorption peak and its shift to higher wavenumber. Moreover, a weak but
obvious peak split was also observed on microwave-assisted sequentially stripped samples,
which inferred to a series of oxidation reactions followed by a prolonged stripping interval on
the fabric. Thus, the band splitting was caused by more complex fragments or intermediates that
were produced and remained on the substrate (Hurtubise et al. 1960). Furthermore, at 1421 cm1,
the strong absorption band was mainly due to the scissoring vibration of the _CH2- groups on
the cellulose macrochains that were vulnerable to variations in the chemical environment of the
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side group _C- in the cellulose polymeric networks. Additionally, its nearby absorption band at
1366 cm-1 and 1366 cm-1 was assigned to the bending vibration of the _CH2- groups in the
plane, which usually did not or was less affected by some external interferes and significantly, it
was most appropriate to specify the crystallinity of the substrate. Moreover, the absorption band
at 1312 cm-1 and 1317 cm-1 was attributed to wagging vibration of the _CH2- groups in the plane
(He et al. 2021).

4.6 Re-Dyeing

Table 5 Colorimetric data of re-dyed fabric with Reactive Yellow C4GL to assess the re-
dyeability of stripped fabric

of
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Dye Treatment K/S L* a* b* C* ho

White Untreated
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3.0299a 82.04a -8.69a 54.62a 55.3a 99.04a
fabric fabric
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Reactive 3.8316b 82.24b -5.96b 68.65b 68.9b 94.96b

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Red Acid+
CL4BN 2.8495c 82.18c -7.01c 61.71c 62.11c 96.48c
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Reduction+
Reactive 3.5081b 83.35b -7.92b 56.01b 56.57b 98.05b
Black Oxidation
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PLS 2.9191c 78.56c -7.13c 48.08c 48.60c 98.44c

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Reactive 2.668b 83.12b -7.91b 61.38b 61.89b 97.34b

Red Alkali+
CL4BN 2.4355c 82.61c -9.31c 57.91c 58.65c 99.13c
Reduction+
Reactive 3.9087b 84.07b -8.45b 62.82b 63.39b 97.66b
Black Oxidation

PLS 3.6411c 83.77c -8.57c 60.57c 61.17c 98.05c

a
Untreated Dyed Fabric; b Microwave Assisted Stripped Fabric; c Conventionally Stripped
Fabric

Table 5 shows the colorimetric data of re-dyed fabric. L* value of standard fabric dyed
with Reactive Yellow C4GL dye was 82.04. The L* value of re-dyed fabric of microwave-
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assisted and conventional acid hydrolysed sequentially stripped cotton fabric dyed with
Reactive Red CL4BN was 82.24 and 82.1 respectively. L* value of re-dyed fabric of
microwave-assisted and conventional acid hydrolysed sequentially stripped cotton fabric dyed
with Reactive Black PLS was 83.35and 78.56 respectively. L* values of re-dyed fabric of
microwave-assisted and conventional alkali hydrolysed sequentially stripped cotton fabric dyed
with Reactive Red CL4BN was 83.12 and 82.61 respectively and for Reactive Black PLS, it
was 84.07 and 83.77 for microwave-assisted and conventional treatments. The L* values of re-
dyed samples were very similar to the standard fabric dyed with Reactive Yellow C4GL dye.
The a* value of standard dyed fabric was -8.69 and decreased for re-dyed fabric indicating shift
towards green. At the same time, the b* values of re-dyed fabric of all the treated samples

of
increased from standard dyed fabric leading towards blue shift. Chroma has increased for

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sequentially stripped and re-dyed fabric from standard one indicates that the saturation of
samples has increased. Values of ho for redyed fabrics are decreased from dyed fabric. The
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visual representation of re-dyed fabrics is given in figure 14.
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Figure 14 Re-dyed fabric with Reactive Yellow C4GL

(a). Untreated dyed fabric (b). Microwave-assisted acid hydrolysed sequentially stripped and re-dyed
fabric (c). Conventional acid hydrolysed sequentially stripped and re-dyed fabric (d). Microwave-
assisted alkali hydrolysed sequentially stripped and re-dyed fabric (e). Conventional alkali hydrolysed
sequentially stripped and re-dyed fabric
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Table 5 shows the K/S values of untreated and sequentially stripped fabric dyed with
2% Reactive Yellow C4GL dye. The K/S value of standard fabric was 3.0299. The K/S value
of re-dyed fabric of microwave-assisted and conventional acid hydrolysed sequentially stripped
cotton fabric dyed with Reactive Red CL4BN was 3.8316 and 2.8495 respectively. The K/S
value of re-dyed fabric of microwave-assisted and conventional acid hydrolysed sequentially
stripped cotton fabric dyed with Reactive Black PLS was 3.5081 and 2.9191 respectively. It is
clear that the microwave-assisted treatment increased the K/S values while the conventional
method resulted in lowering the K/S values. The K/S value of re-dyed fabric of microwave-
assisted and conventional alkali hydrolysed sequentially stripped cotton fabric dyed with
Reactive Red CL4BN was 2.668 and 2.4355 respectively. The K/S value of re-dyed fabric of

of
microwave-assisted and conventional alkali hydrolysed sequentially stripped cotton fabric dyed

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with Reactive Black PLS was 3.9087 and 3.6411 respectively. Microwave-assisted sequentially
stripped fabric has more K/S value conventionally stripped fabric (Alam et al. 2023). The
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lowering of the K/S indicates that the treatment could not completely remove the previous dye
components. While the increase in the K/S value indicates the effectiveness of stripping
re
treatment. The K/S value more than untreated fabric is because of the impurities are removed
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from the cellulose by the stripping process. The fat layer is present in the cellulose, when the
fabric is dyed, this layer hindered the attachment of dye components to the fabric, but when
stripping is performed this fat layer is dissolved and re-dyeing results in more dye adsorption
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hence, more K/S value. Among all the treatments, microwave-assisted acid hydrolysis
followed by reduction and oxidation resulted in higher color strength.
ur

Conclusion
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An innovative, eco-friendly and energy-conservative methodology of microwave-

assisted sequential stripping of Reactive Red CL4BN dye on the cotton substrate was
successfully investigated as an environment friendly method. Microwave-assisted sequential
stripping resulted in up to 97% stripping efficiency. Microwave-assisted sequential stripping
caused an increase in the tear strength of the fabric. Acid hydrolysed sequentially stripped fabric
dyed with Reactive Red CL4BN resulted in an increased tear strength by 17.7% and 24.1% in
warp and weft directions respectively. Where’s Acid hydrolysed sequentially stripped fabric
dyed with Reactive Black PLS resulted in an increased tear strength by 19.3% and 17.2% in
warp and weft directions respectively while the tear strength of microwave-assisted alkali
hydrolysed sequentially stripped fabric dyed with Reactive Black PLS increased by 14.5% and
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29.3% in warp-wise and weft-wise direction respectively. Microwave-assisted acid and alkali
hydrolysed sequentially stripped fabric dyed with Reactive Red CL4BN resulted in 1% and
0.25% weight loss respectively while their respective conventional treatment resulted in 1.75%
and 2.75% weight loss respectively. Microwave-assisted acid and alkali hydrolysed sequentially
stripped fabric dyed with Reactive Black PLS resulted in 1.25% and 0.1% weight loss
respectively while their respective conventional treatment resulted in 1.75% and 2.5% weight
loss respectively. Moreover, by using Fourier transform infrared spectrometry (FT-IR),
the stripping of Reactive Red CL4BN and Reactive Black PLS dyed cotton cellulose was
successfully characterized. According to the colorimetric data of redyed fabric, it is evident that
the re-dyeing ability of microwave-assisted stripped fabric is more than conventionally treated

of
fabric. Hence microwave-assisted sequential stripping method is found to be superior in terms

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of stripping efficiency, weight loss, tear strength, redyeing ability as well as time and energy
saving methods over the conventional stripping method. Therefore, the microwave-assisted
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sequential stripping method might be employed in the practical field by additional investigation
of the textile features of this approach.
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Author contributions
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Taqdees Zahira; Investigation, Methodology, Writing – original draft, Formal analysis, Data curation.
Sadia Noureen; Data curation, Methodology, Draft preparation. Shaukat Ali; Supervision,
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Conceptualization, Project administration, Resources, Funding acquisition. Hina Haq; Methodology

Mubashar Alam; Writing – original draft preparation Anam Akhtar; Data curation, Muhammad
ur

Abdullah; Formal analysis

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Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal
relationships that could have appeared to influence the work reported in this paper.

Acknowledgment

The authors like to acknowledge the support from Textile and Color Chemistry Laboratory,
University of Agriculture, Faisalabad (UAF). We also thank Dr. Muhammad Tahir Hussain,
National Textile University (NTU) Pakistan for additional resources.

Data availability statement

No data is required
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