polymers

Article
A New Sight of Ozone Usage in Textile: Improving Flame
Retardant Properties
Semiha Eren 1 , İdil Yiğit 2, * , Kadriye Kutlay 3 , Zehra Kaya 3 , Cansu Basrık 3 and Hüseyin Aksel Eren 1

1 Textile Engineering Department, Bursa Uludag University, Bursa 16059, Türkiye;

[email protected] (S.E.); [email protected] (H.A.E.)
2 Textile, Clothing, Footwear and Leather Department, Bursa Uludag University, Bursa 16980, Türkiye
3 Berteks Company, Bursa 16245, Türkiye; [email protected] (K.K.); [email protected] (Z.K.);
[email protected] (C.B.)
* Correspondence: [email protected]

Abstract: Ozone, widely recognized as an environmentally friendly gas, is extensively used in various
textile industry applications. These include pre-treatment processes like bleaching and desizing, as
well as creating pattern and vintage effects, wastewater clarification, and surface modification. This
study focuses on ozone as a novel solution to a specific challenge: addressing the reduction in flame
retardancy properties experienced by flame-retardant (FR) polyester fabrics during post-treatment
processes in the production line. Experimentation involved subjecting the fabrics to ozonation and
exploring different combinations of ozone flow rates and treatment durations. Mechanical and func-
tional properties of the fabrics were examined, with flammability tested according to International
Maritime Organization (IMO) standards. Notably, treatment with a 5 L/min ozone flow rate, a
7.01 g/h ozone concentration ratio, and a duration of 10 min showed significant improvements in
IMO values, ensuring compliance with required standards. Furthermore, treated samples underwent
comprehensive tests for fastness and strength, yielding results within acceptable ranges. Fourier-
transform infrared (FT-IR) and thermogravimetric analysis (TGA) measurements were conducted
to evaluate the impact of ozonation. FT-IR results indicated that the presence of C-H groups asso-
ciated with dyestuff contributed to decreased flame retardancy in the original fabric post-dyeing.
However, these groups were effectively eliminated through ozonation, thereby enhancing the fabric’s
flame retardancy.
Citation: Eren, S.; Yiğit, İ.; Kutlay, K.;
Kaya, Z.; Basrık, C.; Eren, H.A. A New
Keywords: ozone; flame retardant (FR); IMO; flammability; polyester
Sight of Ozone Usage in Textile:
Improving Flame Retardant
Properties. Polymers 2024, 16, 735.
https://doi.org/10.3390/
polym16060735 1. Introduction

Academic Editor: Paul Joseph

Flammability presents a significant risk to both human lives and property, making it a
pressing concern in our daily lives [1,2]. The burning behavior of textile products, widely
Received: 11 January 2024 used across various fields, is characterized by their susceptibility to ignition and sustained
Revised: 28 February 2024 burning [3]. These materials, due to their hydrocarbon chains, tend to emit heat, flames, and
Accepted: 4 March 2024 smoke when exposed to fire [1,4]. To address this issue, flame retardants are incorporated
Published: 7 March 2024
into polymeric materials to prevent fire onset or restrict its propagation [5]. Since the 1950s,
flame retardant chemicals have been developed for fibers and textiles [6]. However, many
of these chemicals have shown toxic effects on humans and the environment. Consequently,
Copyright: © 2024 by the authors.
researchers are actively exploring novel flame retardant finishes and coatings with im-
Licensee MDPI, Basel, Switzerland. proved environmental profiles and reduced toxicity for textile applications [7]. There is a
This article is an open access article growing interest in developing flame retardants derived from renewable and sustainable
distributed under the terms and sources, reflecting a broader shift toward more sustainable and eco-friendly solutions in
conditions of the Creative Commons flame retardancy [8]. Various methods, including ASTM standards, have been developed
Attribution (CC BY) license (https:// to assess fabric flammability [9,10]. For materials lacking inherent flame retardancy, such
creativecommons.org/licenses/by/ as meta/para-aramid, glass fiber, carbon fiber, and fluorocarbon fiber, different approaches
4.0/). are employed to impart flame retardant properties:

Polymers 2024, 16, 735. https://doi.org/10.3390/polym16060735 https://www.mdpi.com/journal/polymers

Polymers 2024, 16, 735 2 of 12

(i) Fiber structures can be modified through copolymerization and chemical modifica-
tion techniques involving the addition of halogen and/or phosphorus-containing
comonomers during copolymerization.
(ii) Flame retardant chemicals can be added to the synthetic polymer during the fiber
spinning process.
(iii) Flame retardancy can be achieved through finishing treatments, wherein fabrics are
treated with flame-retardant chemicals [11–14].
(iv) Nanoparticles with flame-retardant properties can be incorporated into coatings or
applied directly to fibers to enhance their resistance to ignition [15].
(v) Phase change materials (PCM) can be integrated into fabrics to provide additional
flame resistance while maintaining wearer comfort [16,17].
Polyester, a widely used synthetic polymeric material in textiles, poses significant
risks due to its highly flammable nature and tendency to drip. Therefore, flame-retardant
properties are essential for polyester products to meet customer demands and comply with
government regulations [9,10,18–20].
Apart from factors like fiber content, fabric construction, and environmental conditions,
the choice of finishing materials can impact fabric flammability [21]. The hydrophobic
nature of polyester fibers results in relatively low chemical absorption during wet process
treatments, potentially decreasing flame retardancy [22]. For instance, softeners in fabrics
have been found to reduce flame retardancy [2,23].
Even when raw materials exhibit satisfactory flame retardancy, finishing processes can
lead to strength loss or increased flammability due to flammable chemicals present on the
fabric’s surface [21]. Researchers have highlighted the adverse effects of dyes, particularly
disperse azo dyes, on polyester fabric flammability, as these dyes tend to migrate to the
fiber’s surface during heat treatment [23,24].
Disperse dyes, with their limited solubility in water, can aggregate and deposit on
the surface of PET fibers during the dyeing process. If not effectively removed, this
surface contamination can negatively impact various fabric properties, including flame
retardancy [23–27]. The conventional method for clearing these dyes involves reduction
clearing, breaking down residual disperse dye molecules into smaller, colorless, and more
readily water-soluble fragments [26,27].
Oxidative agents like ozone (O3 ) have shown effectiveness in breaking down deposited
disperse dyes on fiber surfaces. Ozone, industrially produced using commercially available
ozone generators, has a high oxidation potential and has successfully decolorized disperse
dyeing effluents through ozone treatment [28–30]. Ozone gas is increasingly favored for
various industrial applications due to its potent oxidative properties, offering a more
environmentally friendly and energy-efficient alternative to traditional processes in the
textile industry [28–31].
As demonstrated by previous studies, the flame retardancy of fabrics can diminish
following dyeing, washing, and fixation. Subsequent finishing processes are often required
to enhance the flame retardant properties. However, reusing chemicals in these processes
increases costs and impacts the environment [32]. Therefore, it is advantageous to coun-
teract the decrease in flame retardancy through ozone treatment without harming the
environment or necessitating the use of additional chemicals. Thus, the primary objective
of this study is to restore the diminished flame retardancy resulting from these processes
through ozone gas treatment. This innovative approach holds significant promise for the
textile industry, offering a more sustainable and environmentally friendly method and
effectively clearing the surface of polyester fabrics.

2. Materials and Methods

In this study, 100% polyester fabrics made of polyethylene terephthalate (PET) were
used. The fabrics were produced using flame retardant polyester yarn containing comonomer
with phosphorus. The polyester yarns (300/288 centered and 75/72 550 Draw Texture Yarn)
were sourced from Toray/Korea company. To achieve the desired coloration, the yarns were
Polymers 2024, 16, x FOR PEER REVIEW 3 of 12

Polymers 2024, 16, 735 Yarn) were sourced from Toray/Korea company. To achieve the desired coloration, the
3 of 12
yarns were dyed using a mixed dyestuff comprising Color Index (CI) Disperse Orange 30
(0.02%) (by DyStar, Tekirdağ, Türkiye), CI Disperse Red 167.1 (0.002%) (by DyStar), and
Terasil Blue LF (0.02%) (by Hunstman, The Woodlands, TX, USA) in a Thies dyeing ma-
dyed using a mixed dyestuff comprising Color Index (CI) Disperse Orange 30 (0.02%) (by
chine.
DyStar, The dyeing
Tekirda recipe included
ğ, Türkiye), 1.5% Red
CI Disperse dispersant (Levanol
167.1 (0.002%) HDL
(by by Genkim,
DyStar), Bursa,
and Terasil Blue Tü-
LF
rkiye), 0.4% leveling agent (Segacar D Liq by Sözal Kimya, Bursa, Türkiye),
(0.02%) (by Hunstman, The Woodlands, TX, USA) in a Thies dyeing machine. The dyeing 0.3 g/L wetting
agent
recipe(Revapol
includedENN 1.5%by Alfa Kimya,
dispersant Bursa,HDL
(Levanol Türkiye), and 0.05
by Genkim, g/L acid
Bursa, buffer0.4%
Türkiye), (Exapon Cn
leveling
Plus by MaiTürk Kimya, Bursa, Türkiye).
agent (Segacar D Liq by Sözal Kimya, Bursa, Türkiye), 0.3 g/L wetting agent (Revapol ENN
AfterKimya,
by Alfa dyeing,Bursa,
the yarns were neutralized
Türkiye), and 0.05 g/L with acid
acid (Exapon
buffer CN Plus).
(Exapon Since
Cn Plus bythe fabric
MaiTürk
required a lightTürkiye).
Kimya, Bursa, color, no reduction-clearing process was performed. The yarns were wo-
ven asAfter
jacquard
dyeing,weaves with
the yarns double
were in the warp
neutralized direction
with acid (Exapon satin
CN5Plus).
(SatinSince
4/1) the
using a
fabric
Stäubli, Horgen, Switzerland weaving machine.
required a light color, no reduction-clearing process was performed. The yarns were woven
The resulting
as jacquard weaves fabric
withsamples
doubleunderwent
in the warpprocessing through
direction satin a Monforts
5 (Satin Montex
4/1) using 5000
a Stäubli,
model Stenter, Mönchengladbach,
Horgen, Switzerland weaving machine. Germany (20 m/min) and a Mathis Brand Laboratory
type mini Stenter, Oberhasli,
The resulting Switzerland
fabric samples (LABDRYER
underwent processing TYPE “LTE”)
through (1 min) according
a Monforts Montex 5000 to
the designated
model Stenter,method.
Mönchengladbach, Germany (20 m/min) and a Mathis Brand Laboratory
typeForminiozonation, a ProOzonSwitzerland
Stenter, Oberhasli, (Ankara, Türkiye)
(LABDRYERgeneratorTYPEwith a capacity
“LTE”) (1 min) ofaccording
25 g/h wasto
utilized. The ozonation
the designated method. process occurred in an aqueous environment, utilizing an ATAC
BB01FFor (Atac Co., Istanbul, Türkiye) model bobbin dyeing machine modified
ozonation, a ProOzon (Ankara, Türkiye) generator with a capacity of 25 g/h to accommo-
date
wasthe gas. The
utilized. The outlet gas of the
ozonation ozone
process generator
occurred in was integrated
an aqueous into the liquor
environment, circula-
utilizing an
tion
ATAC lineBB01F
of a sample Atac Istanbul,
(Atac Co., BB01F sample dyeing
Türkiye) modelmachine
bobbin viadyeing
a venturi injector.
machine The sys-to
modified
tem’s setup canthe
accommodate begas.
referenced in the
The outlet gas works of Yigit
of the ozone and Eren
generator was2017 and Eren
integrated and
into theYetişir
liquor
2018 [33,34].line of a sample Atac BB01F sample dyeing machine via a venturi injector. The
circulation
The methods
system’s setup canemployed in this
be referenced instudy are divided
the works of Yigit into
and twoErenmain
2017 parts.
and ErenTheandfirstYetişir
part
covers fabric production and its associated treatments, while the second part is dedicated
2018 [33,34].
to testThe
methods.
methods employed in this study are divided into two main parts. The first part
covers fabric production and its associated treatments, while the second part is dedicated
2.1. Production
to test methods. and Treatments
2.1.1. Yarn Dyeing
2.1. Production and Treatments
The
2.1.1. flame-retardant
Yarn Dyeing polyester yarns underwent the standard polyester dyeing pro-
cess and were subsequently transferred to the SSM PW1 model winding machine
The flame-retardant polyester yarns underwent the standard polyester dyeing process
(Wädenswil, Switzerland). Figure 1 illustrates the dyeing diagram for flame-retardant
and were subsequently transferred to the SSM PW1 model winding machine (Wädenswil,
polyester yarns.
Switzerland). Figure 1 illustrates the dyeing diagram for flame-retardant polyester yarns.

Figure 1. Dyeing diagram of flame retardant polyester yarns.

Figure 1. Dyeing diagram of flame retardant polyester yarns.
2.1.2. Fabric Production
The yarns were woven into a jacquard weave, resulting in 36 weft/cm and 80 warp/cm
density fabric weighing 660 g/L meters.
 2.1.2. Fabric Production
The yarns were woven into a jacquard weave, resulting in 36 weft/cm and 80
warp/cm density fabric weighing 660 g/L meters.

Polymers 2024, 16, 735 2.1.3. Ozonation 4 of 12

The ozonation process was conducted in an ATAC BB01F sample bobbin dyeing ma-
chine specialized and modified for ozonation (refer to Figure 2) at room temperature con-
ditions (22 ± 2 °C) using water, without the addition of any chemicals. Water (liquor ratio
2.1.3. Ozonation
of 15:1) wasozonation
The maintained, and optimization
process was conductedexperiments
in an ATAC wereBB01F
carriedsample
out to determine the
bobbin dyeing
appropriate ozonationand
machine specialized timemodified
and ozone
forflow. After (refer
ozonation the treatments,
to Figure 2)theatfabrics were fixed
room temperature
atconditions
150 °C. (22 ± 2 ◦ C) using water, without the addition of any chemicals. Water (liquor
ratioThe ozone
of 15:1) wasconcentration wasoptimization
maintained, and measured using the standard
experiments iodometric
were carried method
out to determine
(APHA Standardozonation
the appropriate Methods time
2350 and
E) [35],
ozoneyielding a 7.01the
flow. After g/h value at athe
treatments, 5 L/min
fabricsozone gas
were fixed
flow rate.
at 150 ◦ C.

Figure
Figure2.2.Ozone
Ozonegenerator
generatorand
andintegrated
integratedsample
sampledyeing
dyeingmachine
machine(1.
(1.ozone
ozonegenerator;
generator;2.2.auto-
autoclave;
clave; 3. beam;
3. beam; 4. ozone
4. ozone flow flow
pipe;pipe; 5. venturi
5. venturi injector;
injector; 6. circulation
6. circulation pump;pump; 7. ozone
7. ozone outlet)
outlet) [26]. [26].

2.1.4. Washing
The ozone concentration was measured using the standard iodometric method (APHA
The raw
Standard fabric underwent
Methods 2350 E) [35],two washacycles
yielding in avalue
7.01 g/h BABCOCK washing
at a 5 L/min machine,
ozone using
gas flow rate.
10 g/L caustic (by Ozan Kimya, Bursa, Türkiye), 15 g/L reductant (LAUCOL RX by Erca,
2.1.4. Washing
Grassobbio, Italy), and 10 g/L oil remover (OPTISOL RG-50 by Optima Kimya, Tekirdağ,
Thewith
Türkiye), raw fabric underwent
continuous twoatwash
washing 80 °C.cycles in a BABCOCK washing machine, using
10 g/L caustic (by Ozan Kimya, Bursa, Türkiye), 15 g/L reductant (LAUCOL RX by Erca,
2.1.5. FixationItaly), and 10 g/L oil remover (OPTISOL RG-50 by Optima Kimya, Tekirdağ,
Grassobbio,
Türkiye), with continuous washing at 80 ◦ C.
The fabric was subsequently dried in a Monforts Montex 5000 machine (Mönchen-
gladbach, Germany) at 150 °C at a 15 m/min speed.
2.1.5. Fixation
The fabric was subsequently dried in a Monforts Montex 5000 machine (Mönchenglad-
2.2. Test Methods
bach, Germany) at 150 ◦ C at a 15 m/min speed.
2.2.1. Flame Retardant Test
2.2. The
Test majority
Methods of standardized testing methods employed to assess flammability and
flame resistance
2.2.1. Flame are tailored
Retardant Test for measuring specific flammability characteristics of textile
materialsThe [36].
majorityThe of
International
standardized Maritime Organization
testing methods (IMO)tohas
employed established
assess the Fire
flammability and
Test Procedure
flame resistance Code
are Part 7 (IMO
tailored FTPC P7) [37]
for measuring as a standard
specific for testing
flammability flame retardancy
characteristics of textile
developed
materials by [36].theTheorganization
Internationalitself. This code
Maritime outlines the
Organization methods
(IMO) for evaluating
has established the the
Fire
flame retardant properties
Test Procedure Code Part of various
7 (IMO shipP7)
FTPC components, with Part
[37] as a standard for7 testing
specifically
flameaddressing
retardancy
the testing ofby
developed flame retardancy onitself.
the organization vertical
Thistextile
codesurfaces
outlinesor thefilms.
methods for evaluating the
flameIn retardant
essence, the methodofinvolves
properties various suspending
ship components,sampleswithvertically for testing,addressing
Part 7 specifically with di-
mensions
the testing ofof
220 mmretardancy
flame × 170 mm. on A key criterion
vertical textileissurfaces
assessing orwhether
films. the drips produced
duringInthe test canthe
essence, ignite otherinvolves
method materialssuspending
on the surface. To evaluate
samples verticallythis,for
a piece of cotton,
testing, with di-
dried at 100 °C to eliminate moisture, is positioned 15 cm below the sample. A 40 mm
mensions of 220 mm × 170 mm. A key criterion is assessing whether the drips produced
propane
during the gastest
flamecanisignite
then other
used materials
for ignition, with
on the cotton To
surface. serving
evaluate as athis,
reference
a piecematerial
of cotton,
◦
due to its
dried at well-known flammability
100 C to eliminate characteristics.
moisture, is positioned 15 cm below the sample. A 40 mm
propane gas flame is then used for ignition, with cotton serving as a reference material due
to its well-known flammability characteristics.
To initiate the testing process, four samples are prepared in both width and length
directions. For each direction, two flame orientations, referred to as edge and surface in the
standard, must be applied. In the edge direction, the flame makes contact with the lower
edge of the fabric at a 45-degree angle, while in the surface direction, it contacts the front
 The following observations are recorded during the testing:
Ignition Time: After the flame application period concludes, the flame source is re-
moved. If there is any ignition that persists after the flame source is removed, its duration
is documented, and this duration should not exceed 5 s.
Polymers 2024, 16, 735 Dripping: It is crucial to note if any ignition occurs in the cotton placed beneath5 the of 12
sample. No ignition of the cotton should result from dripping from the fabric.
Hole Size: The length or width of the hole caused by burning or flaming in the sample
after the of
surface test
themust not
fabric at exceed 150 mm.
a 90-degree This
angle. requirement
Figure is aconsistently
3 provides met in all of
visual representation tests
the
covered by this
IMO test method. article and is therefore omitted from the tables [38,39].

Figure
Figure3.3.IMO
IMOtest
testmethod:
method:(a)(a)test
testdevice,
device,(b)
(b)edge
edge(45°)
(45◦ )flame,
flame,(c)
(c)surface
surface(90°)
(90◦ )flame,
flame,(d)
(d)hole
hole
caused by burning or flaming.
caused by burning or flaming.

After conducting
For fabric tests and
directions on fabric
flamesamples, the two
orientations, two samples
differentdisplaying the poorest
flame contact times re-
are
sults in both the weft and warp directions were selected. Additionally, five more samples
tested: 5 and 15 s. Therefore, fabric samples in both directions are assessed in four
were chosen
distinct ways. for testing in each direction, maintaining the same conditions as the initial
samples.
The The testingobservations
following was carriedare outrecorded
using the Jamesthe
during Heal Flexiburn test device in the
testing:
Berteks TextileTime:
Ignition Physics Laboratory.
After the flame application period concludes, the flame source is
This study
removed. If therecalculated the average
is any ignition value of
that persists thethe
after testflame
resultsource
times.isThe primary
removed, itsobjective
duration
was not to achieve exceptional test results but rather to showcase an improvement in
is documented, and this duration should not exceed 5 s.
flameDripping:
retardancyItlevels afterto
is crucial ozonation.
note if any Inignition
the IMOoccurs
Part 7 test standard,
in the the average
cotton placed beneath value
the
for after-flame time is typically not considered; any sample flaming for more than 5 s is
sample. No ignition of the cotton should result from dripping from the fabric.
considered failure.
Hole Size: TheHowever, for this
length or width of study,
the hole a caused
modification was made
by burning to theinevaluation
or flaming the sample
process
after the while applying
test must the test150
not exceed method
mm. without any alterations.
This requirement This adjustment
is consistently met in allaimed
tests
to clearly illustrate the difference between the trials. Therefore, the average value of the
covered by this article and is therefore omitted from the tables [38,39].
After time
after-flame conducting
was taken testsinto
on account,
fabric samples,
providing theatwomore samples displaying
transparent the poorest
demonstration of
results in both the weft and warp directions
the improvement between the samples that failed the test. were selected. Additionally, five more samples
were chosen for testing in each direction, maintaining the same conditions as the initial
samples.
2.2.2. The testing was
Fourier-Transform carriedSpectroscopy
Infrared out using the James Heal Flexiburn test device in the
(FT-IR)
Berteks Textile Physics Laboratory.
FT-IR analysis provides information about the functional groups in molecules and
This study calculated the average value of the test result times. The primary objective
the vibrational frequencies of various bonds. FT-IR analysis was performed on the sam-
was not to achieve exceptional test results but rather to showcase an improvement in
ples to determine the reason for the increased flame retardancy test success after ozona-
flame retardancy levels after ozonation. In the IMO Part 7 test standard, the average value
tion. The FT-IR structure
for after-flame analysisnot
time is typically wasconsidered;
conducted any using the SHIMADZU
sample flaming forTracer
more IR100
than 5(Ja-
s is
pan) brand spectrophotometer test device.
considered failure. However, for this study, a modification was made to the evaluation
process while applying the test method without any alterations. This adjustment aimed
to clearly illustrate the difference between the trials. Therefore, the average value of the
after-flame time was taken into account, providing a more transparent demonstration of
the improvement between the samples that failed the test.

2.2.2. Fourier-Transform Infrared Spectroscopy (FT-IR)

FT-IR analysis provides information about the functional groups in molecules and the
vibrational frequencies of various bonds. FT-IR analysis was performed on the samples to
determine the reason for the increased flame retardancy test success after ozonation. The
FT-IR structure analysis was conducted using the SHIMADZU Tracer IR100 (Japan) brand
spectrophotometer test device.

2.2.3. Thermogravimetric Analysis (TGA)

A thermogravimetric analysis (TGA) test was conducted on the SDTQ600 TA with
ISO 11358-1 [40]. The temperature range of the TGA was 20 ◦ C to 600 ◦ C with a heating
rate of 20 ◦ C/min under a nitrogen atmosphere and then heated from 600 ◦ C to 900 ◦ C
under an oxygen atmosphere.
Polymers 2024, 16, 735 6 of 12

2.2.4. Measurement of Color

Color measurements were conducted to evaluate the potential impact of ozonation on
the color of the samples, alongside the improvement in flame retardancy test success. The
color difference tests were carried out using a Datacolor brand spectrophotometer device
and the Kavolab ColorOffice program. A comprehensive set of eight measurements was
taken on both the front and back sides of the samples to ensure a thorough assessment of
any color variations resulting from the ozonation process.

2.2.5. Fastness Tests

Fastness tests were conducted to examine the effect of ozonation on the fastness values
of the samples. The washing fastness was evaluated using a thermal oil paint machine,
following the ISO 105 C06 standard [41]. The rubbing fastness tests were performed using
the J. Heal Crockmeter, by the ISO 105 X12 standard [42].

2.2.6. Strength Tests

Tensile strength tests were carried out to evaluate the effects of ozonation on the
strength values of the samples. The fabric samples were subjected to strength tests using
the Titan 3 device, following the EN ISO 13934-1 standard [43]. A pre-stress of 2 N was
applied, followed by a load of 100 N.

2.3. Optimization
This collaborative study was conducted in partnership with Berteks Textile Company
(Bursa, Türkiye) to address the challenge of low flame retardancy test success in a fabric
highly favored by their customers. Despite being woven with flame-retardant yarn, the
fabric experienced a decrease in test success due to the presence of impurities such as oil
and dye. These impurities, inadequately removed during yarn dyeing, yarn transfer, and
weaving stages, resulted in incomplete elimination, reducing flame retardancy. Among 50
different lots dyed at various times, 20 failed the flame retardancy test, underscoring the
issue of incomplete impurity removal from the fabric.
In pursuit of optimization, various ozonation times and ozone flow rates were tested
on fabrics acquired from different production stages. Flammability tests (IMO) were
conducted on the resultant samples. The trials revealed that the most favorable results
were achieved with an ozonation time of 10 min and a flow rate of 5 L/min.
The study categorized the investigation into four distinct categories, aiming to identify
which process contributes to the reduction of the flame-retardant effect in fabrics. The flame
retardancy of these fabrics was then assessed using the IMO test, with the results detailed
in Table 1. These categories are:

Table 1. IMO test results after different process steps.

Sample Ignition Time (s) Dripping Number Observation * Result

Category 1
- - - Accept
(FR)
Category 2
8.3 5 EDGE/5 Times Reject
(FR + D)
Category 3
14 6 EDGE/6 Times Reject
(FR + D + W + F)
Category 4
3 0 - Accept
(FR + D + W + F + O)
The table displays data obtained from a 10 min ozonation process at a 5 L/min ozone gas flow. The codes used
correspond to the initial letters of the processes as follows: FR: Flame Retardant; FR + D: Flame Retardant + Dyed;
FR + D + W + F: Flame Retardant, Dyed, Washed, Fixed; FR + D + W + F + O: Flame Retardant, Dyed, Washed,
Fixed, and Ozonated. The data are presented in the format: * (Ignition Direction And Cotton Ignition Times).
Polymers 2024, 16, 735 7 of 12

Category 1: Undyed fabrics with flame-retardant additives (FR). It aimed to assess the
effectiveness of the FR additives in the yarns.
Category 2: Fabrics produced from dyed (D) yarns with flame retardant (FR) additives
(FR+D). The objective was to observe the effects of dyeing processes.
Category 3: Fabrics produced from dyed (D) yarns with flame retardant (FR) additives
that were subsequently washed (W) and fixed (F) (FR + D + W + F). This category aimed to
see the flame retardant effect after all processes.
Category 4: The process in which ozonation (O) is performed after the processes
carried out in Category 3. This category of fabrics was produced from dyed (D) yarns with
flame retardant (FR) additives that were subsequently washed (W), fixed (F), and ozonated
(O) (FR + D + W + F + O).

3. Results
The results of the optimization process involving ozone gas and the corresponding
combustion data are presented in Table 1. Various ozone flow rates and durations were
tested, employing a flow rate of 5 L/min and an ozonation time of 10 min. The flame
retardancy effect, which had reduced after dyeing, washing, and fixing fabric produced
with flame retardant (FR) additives, demonstrated successful improvement after ozonation.
To evaluate the fabrics, the average flame time and the number of burning drips were
measured in a total of 18 tests, considering both surface and edge directions in both weft
and warp orientations. Initially manufactured with dyed yarns and FR additives, the
fabrics underwent a standard washing and fixing procedure upon arrival at the facility.
These optimized conditions aim to enhance flame retardancy while preserving the desired
physical properties of the fabrics.
Practical experience and the literature affirm that the flame retardancy properties of
fabrics often decrease after dyeing, washing, and fixing processes. However, it is imperative
to ensure that while the flame retardancy test results improve, the physical performance
tests of the samples also meet acceptable standards. A comprehensive set of tests, including
color measurement, fastness, and strength tests, were conducted to address this.
Additionally, FTIR measurements were performed to elucidate the factors contributing
to the increase in flame retardancy test success. Category 3 (FR added-dyed Fabric by
Washed and Fixed Unprocessed) is the reference sample used for comparing the results.
This reference sample serves as a baseline for evaluating the impact of different processes
and treatments on flame retardancy and physical performance.

3.1. Flame Retardant Test Results

Upon examining Table 1, the IMO test results for Category 1 were successful as
expected, given that no processes other than the addition of flame retardant (FR) were
applied to the samples. However, in Category 2 and Category 3, subsequent processes
such as dyeing, washing, and fixing led to a loss of flame retardant properties in the fabrics.
The literature supports the idea that washing, mainly due to the presence of softeners and
lubricants on the surface, diminishes flammability. Additionally, as supported by the data
obtained, the thermomigration of dyes at high fixing temperatures contributes to this loss.
Hence, it is affirmed that fabrics with FR additives should undergo washing and fixing
steps, as seen in Category 3.
In Category 4, where ozonation was implemented, the fabrics regained flame retar-
dancy, with 5 s or less ignition times. Notably, Category 2 and Category 3 exhibited cotton
ignition and flaming in the edge direction during combustion tests, while the Category
4 fabric showed no drips, and the average flaming time was 3 s. This data supports the
conclusion that the ozonation process can be applied after washing and fixing procedures
for the fabrics.
FTIR measurements were conducted to elucidate the increase in flame retardancy test
success. The results further supported the efficacy of the ozonation process.
 ignition and flaming in the edge direction during combustion tests, while the Category 4
fabric showed no drips, and the average flaming time was 3 s. This data supports the
conclusion that the ozonation process can be applied after washing and fixing procedures
for the fabrics.
Polymers 2024, 16, 735 FTIR measurements were conducted to elucidate the increase in flame retardancy8 test
of 12
success. The results further supported the efficacy of the ozonation process.

3.2.
3.2.FT-IR
FT-IRTest
Test Results
Results
Figure
Figure 4 illustratesthe
4 illustrates themechanism
mechanismof ofdye
dyeand
andozonation
ozonationwithwiththe
theFT-IR
FT-IRspectra
spectraanal-
anal-
ysis.
ysis.Upon
Uponexamination
examination of of
thethe
results, it was
results, noted
it was that that
noted the peak of theof
the peak C-Hthebond
C-H at 3000–
bond at
2840 cm−1 iscm
3000–2840 absent in the flame
−1 is absent in theretardant undyed
flame retardant (Category
undyed 1) sample,
(Category whereas
1) sample, it is pre-
whereas it is
sent in the
present inflame retardant
the flame dyeddyed
retardant (Category 3–FR 3–FR
(Category added-Dyed FabricFabric
added-Dyed by Washed and Fixed
by Washed and
Unprocessed)
Fixed Unprocessed)sample. These These
sample. C-H bonds are attributed
C-H bonds to the to
are attributed dyestuff groups
the dyestuff used in
groups dye-
used in
ing. Following
dyeing. Following the the
ozonation
ozonationprocess, it was
process, observed
it was observed that
thatthe
thesame
samepeak
peakdisappeared
disappeared
again,
again, similar
similar toto the
theCategory
Category1 1sample.
sample.ThisThis indicates
indicates that
that thethe ozonation
ozonation process
process effec-
effectively
tively
removesremoves the dyestuff
the dyestuff from thefrom the surface.
surface. The disappearance
The disappearance of theseof thesealong
peaks, peaks, along
with the
with the of
absence absence
the C-H of the C-H
peak peak
after theafter the ozonation
ozonation process, process,
providesprovides
supporting supporting
evidenceevi-for
dence for the effectiveness
the effectiveness of ozonation.
of ozonation. Ozone plays Ozone plays arole
a pivotal pivotal
in therole in the degradation
degradation of disperseof
disperse
dyestuffsdyestuffs
[44]. The [44]. The improvement
improvement in test
in test success success post-ozonation
post-ozonation is further sub-
is further substantiated by
stantiated by the elimination of dyestuff groups that may contribute to combustion.
the elimination of dyestuff groups that may contribute to combustion.

Figure
Figure4.4.FTIR
FTIRspectra
spectraanalyses
analysesofofsamples:
samples:(a)(a)
Category 1: 1:
Category FR,FR,
(b)(b)
Category 3: FR
Category + D++D
3: FR W++WF, +(c)F,
Category 4: FR + D + W + F + O, (d) Comparative graph of FTIR samples (C1, Category
(c) Category 4: FR + D + W + F + O, (d) Comparative graph of FTIR samples (C1, Category 1—red 1—red line;
line; C3, Category 3—green line; C4, Category 4—black line). FR, Undyed FR-added Fab-
ric); FR + D + W + F (FR added-Dyed Fabric by Washed and Stenter Fixed Unprocessed);
FR + D + W + F + O (FR added-Dyed Fabric by Washed, Stenter Fixed and Ozonated). Red circles
show C-H groups that present by dyeing and affected by ozone treatment.

3.3. Thermogravimetric Analysis Results

Thermogravimetric analysis (TGA) is a technique used to study the thermal degrada-
tion behavior of polymers by measuring the weight loss of a material against an increase in
temperature. TGA provides crucial information on thermal properties such as the onset of
 the onset of decomposition, decomposition temperature, and decomposition rate. Figure
5 illustrates the TGA curves of the fibers, categorized into three groups. The weight per-
centage (wt %) of the retained mass as the temperature increases is depicted in the graphs.
Remarkably, the ozone-treated samples (Category 4) showed a slightly higher initial deg-
Polymers 2024, 16, 735 radation temperature of the polymer (413.16 °C) compared to the untreated samples in
9 of 12
Category 2 (410.24 °C) and Category 3 (411.58 °C). However, no significant differences
among the categories were observed in the residual samples.
Upon examining
decomposition, the TGA temperature,
decomposition results, no substantial differencesrate.
and decomposition wereFigure
noted5among the
illustrates
samples. This can be attributed to the absence of any additional chemicals added
the TGA curves of the fibers, categorized into three groups. The weight percentage (wt %) to the
structure or surface
of the retained of the
mass as the temperature
material for increases
improvedis flame retardancy.
depicted Therefore,
in the graphs. the ozone
Remarkably, the
treatment
ozone-treated samples (Category 4) showed a slightly higher initial degradation the
performed under the selected parameters did not significantly change poly-
tempera-
mer’s
ture ofstructure.
the polymerOzonation
(413.16 ◦primarily
C) comparedaffects theuntreated
to the material’ssamples
surface without altering
in Category its inter-
2 (410.24 ◦ C)
nal
andstructures.
Category 3Consequently, as no operations
(411.58 ◦ C). However, were conducted
no significant differencestoamong
modifythethecategories
internal struc-
were
tures of the samples, it is expected
observed in the residual samples. that the TGA results do not show significant variations.

Figure 5. TGA curve of samples.

Figure 5. TGA curve of samples.
Upon examining the TGA results, no substantial differences were noted among the
3.4. Physical Test Results
samples. This can be attributed to the absence of any additional chemicals added to
As the flame
the structure retardancy
or surface test’s
of the success
material forimproves,
improvedit flame
is crucial to ensure Therefore,
retardancy. that the phys-
the
ical
ozoneperformance tests of the under
treatment performed samples also
the fall within
selected acceptable
parameters did limits. A comprehensive
not significantly change
set
theof tests, including
polymer’s colorOzonation
structure. measurement, fastness,
primarily and the
affects strength tests, were
material’s conducted
surface without on
al-
the samples to achieve this objective.
tering its internal structures. Consequently, as no operations were conducted to modify
the internal structures of the samples, it is expected that the TGA results do not show
3.4.1. Colorvariations.
significant Measurement Results
Upon analyzing the color measurement results of the samples, as outlined in Table
3.4.
2, it Physical Test Results
was observed that the ozonation process did not induce a notable change in the color
values.As The color measurement
the flame results
retardancy test’s successmetimproves,
the success
it iscriterion
crucial toofensure
ΔE ≤ 1. Nothe
that significant
physical
differences
performance were
testsnoted
of theinsamples
the values
also related to lightness–darkness
fall within acceptable limits. A(ΔL), green–redness
comprehensive set
(Δa), andincluding
of tests, yellowness–blueness (Δb) of the
color measurement, samples
fastness, andfollowing
strength the treatment.
tests, Images in
were conducted onFig-
the
ure 6 supported
samples thethis
to achieve color measurement results of samples.
objective.

3.4.1. Color Measurement Results

Upon analyzing the color measurement results of the samples, as outlined in Table 2,
it was observed that the ozonation process did not induce a notable change in the color
values. The color measurement results met the success criterion of ∆E ≤ 1. No significant
differences were noted in the values related to lightness–darkness (∆L), green–redness (∆a),
and yellowness–blueness (∆b) of the samples following the treatment. Images in Figure 6
supported the color measurement results of samples.

Table 2. Color measurement results of Category 4 (FR added-Dyed Fabric by Washed, Stenter Fixed
and Ozonated) samples.

Sample Name ∆L ∆a ∆b ∆E
Category 4
0.38 0.50 0.38 0.85
(FR + D + W + F + O)
The Reference Sample is Category 3 (FR added-Dyed Fabric by Washed and Stenter Fixed Unprocessed).
 and Ozonated) samples.

Sample Name ΔL Δa Δb ΔE
Category 4
0.38 0.50 0.38 0.85
(FR + D + W + F + O)
Polymers 2024, 16, 735 10 of 12
The Reference Sample is Category 3 (FR added-Dyed Fabric by Washed and Stenter Fixed Unpro-
cessed).

Figure6.6.Image
Figure Imageof
ofsamples
samplesbefore
beforeand
andafter
afterozone
ozonetreatment.
treatment.(a)(a)Category
Category 3 (before),
3 (before), (b)(b) Category
Category 4
4 (after).
(after).

3.4.2. Fastness
3.4.2. Fastness Test
TestResults
Results
When examiningthe
When examining thewashing
washing and
and rubbing
rubbing fastness
fastness values
values as
as presented
presented in
in Table
Table3,
3,itit
became evident
became evident that
that the
the fastness
fastness values
values of
of the
theCategory
Category 44samples
samplesremained
remainedconsistent
consistent
withthe
with thereference
referencesamples,
samples,indicating
indicatingthat
thatthe
theozonation
ozonationprocess
processdid
didnot
nothave
havean animpact
impact
onthe
on thefastness
fastnessvalues.
values.

Table3.3.Washing
Table Washingand
andrubbing
rubbingfastness
fastnessresults
resultsofofCategory
Category4 4samples.
samples.

Rubbing Fastness
Rubbing Fastness Washing Fastness
Washing Fastness
Sample
Sample Name
Name
Dry
Dry WetWet Acetate
Acetate Cotton
Cotton Polyamide
Polyamide Polyester
Polyester Acrylic
Acrylic Wool
Wool
Category
Category 33 55 5 5 5 5 5 5 55 55 55 55
(FR
(FR++D D ++ W
W++ F)
F)
Category
Category 4 4
55 5 5 5 5 5 5 55 55 55 55
(FR
(FR++DD ++ W
W ++ F
F++ O)
O)
TheReference
The ReferenceSample
Sample
is is Category
Category 3 (FR
3 (FR added-Dyed
added-Dyed Fabric
Fabric by Washed
by Washed and Stenter
and Stenter Fixed Fixed Unpro-
Unprocessed).
cessed). 4Category
Category 4 (FR added-Dyed
(FR added-Dyed Fabric
Fabric by Washed, by Washed,
Stenter Fixed andStenter Fixed and Ozonated).
Ozonated).

Afterundergoing
After undergoing 55 wash
wash cycles,
cycles, the
the samples
samples were
were observed
observed to
to maintain
maintain their
their flame-
flame-
retardanteffect.
retardant effect.

3.4.3. Strength
3.4.3. StrengthTest
TestResults
Results
Thestrength
The strengthvalues
valuesofofthe
thesamples
samplesare
are presented
presented in in Table
Table 4. The
4. The tensile
tensile strength
strength val-
values
ues
of of Category
Category 4 exhibited
4 exhibited 3% decrease
3% decrease compared
compared to the to the reference
reference samplesample (Category
(Category 3).
3). These
These results fall within the acceptable tolerance values set by companies.
results fall within the acceptable tolerance values set by companies.

Table4.4.Tensile
Table Tensilestrength
strengthresults
resultsofofCategory
Category4 4samples.
samples.

Sample Sample
Name Name Tensile Tensile
StrengthStrength
Force (N) Force (N) Elongation
Elongation (%) (%)
CategoryCategory 3
1177.33 41.4741.47
3
1177.33
(FR + D (FR
+ W ++ DF) + W + F)
Category
Category 4 4
1140.84 1140.84 38.8338.83
(FR + D (FR
+ W ++ D
F ++ O)
W + F + O)
TheReference
The Reference Sample
Sample is Category
is Category 3 (FR 3 (FR added-Dyed
added-Dyed Fabric byFabric
Washedbyand
Washed
Stenterand
FixedStenter Fixed Unpro-
Unprocessed).
cessed).
4. Conclusions
The flame-retardant polyester fabrics, manufactured using flame-retardant yarns, often
experience a reduction in flame retardancy after undergoing dyeing, washing, and fixation
processes. Previous studies attribute this decline to the influence of dyestuffs, softeners, and
lubricants. In this study, samples with diminished flame retardancy underwent ozonation
treatment. Following a 10 min ozonation process at a rate of 5 L/min, flame retardant
tests (IMO) were conducted again. Significantly, Category 4 samples (FR-added Dyed
Fabric by Washed, Fixed, and Ozonated) showed remarkable improvements in both IMO
Polymers 2024, 16, 735 11 of 12

and physical tests. The breakdown of dyestuffs by ozone, whether present on the surface
or remaining post-processing, facilitated the enhancement of flame-retardant properties.
FT-IR analyses revealed the disappearance of dye groups associated with ignition after
ozonation. Samples yielding optimal test results also demonstrated performance in terms
of minimal color differences (∆E < 1), excellent fastness (5 degrees), and acceptable strength
(3% decrease). The application of ozone gas, known for its environmentally friendly nature,
effectively enhanced the success of flammability tests without necessitating additional
flame retardant finishing on FR-added yarn samples. This method proved effective even
for samples initially experiencing decreased test success after undergoing other processes.
The primary aim of this study is to introduce ozone treatment as an innovative approach to
address the documented loss of flame retardancy in the literature. By utilizing environmen-
tally friendly methods like ozone, manufacturers can mitigate environmental and health
risks associated with using additional chemicals, thereby contributing to creating more
sustainable products.

Author Contributions: Conceptualization, S.E., İ.Y., K.K. and H.A.E.; Data curation, S.E., İ.Y. and
H.A.E.; Formal analysis, Z.K. and C.B.; Investigation, S.E., İ.Y., K.K. and H.A.E.; Methodology,
İ.Y., K.K., Z.K. and C.B.; Project administration, S.E., İ.Y. and K.K.; Resources, K.K., Z.K. and C.B.;
Supervision, H.A.E.; Visualization, S.E. and İ.Y.; Writing–original draft, S.E., İ.Y. and H.A.E. All
authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Data Availability Statement: All data relevant to the study are included in the article. On a reasonable
request, additional data shall be available from the corresponding author.
Conflicts of Interest: Author Kadriye Kutlay, Zehra Kaya and Cansu Basrık were employed by the
Berteks Company. The remaining authors declare that the research was conducted in the absence of
any commercial or financial relationships that could be construed as a potential conflict of interest.

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