Basak 2014
Basak 2014
Basak 2014
To cite this article: S. Basak, Kartick K. Samanta & S.K. Chattopadhyay (2014): Fire retardant property of cotton fabric
treated with herbal extract, The Journal of The Textile Institute, DOI: 10.1080/00405000.2014.995456
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The Journal of The Textile Institute, 2014
http://dx.doi.org/10.1080/00405000.2014.995456
Flame retardant functionality was imparted in cellulosic textile using spinach leaves juice (SJ), an eco-friendly natural
product. The extracted juice was made alkaline and applied in fresh bleached and mercerized cotton fabrics. Flame
retardant properties of the control and treated fabrics were analysed in terms of limiting oxygen index (LOI), horizontal
and vertical flammability and radiant heat testing. The study showed that the treated fabrics had good flame retardant
property compared to control fabrics. The LOI value was found to increase by 1.6 times after application of SJ. As a
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result of this, the fabric does not catch flame. In horizontal flammability, the treated fabric showed burning with
afterglow (without presence of flame) with a propagation rate of 10 mm/min, which is almost nine times lower than the
control fabric. The thermal degradation and pyrolysis was studied using thermogravimetric analysis. The chemical
composition of the control and SJ-treated cellulosic fabric were analysed by FTIR, SEM and EDX. Durability of the
flame retardant functionality to soap washing and weathering had also been studied. After application of SJ, cellulosic
fabric sample produced natural green colour. There was no significant change in other physical properties.
Keywords: spinach leaves juice; fire retardant; LOI; cotton; thermogravimetry
retardant property of cellulosic cotton textile using (Model No. 15077968 FB61354 225PE, UK) in non-
vegetable extract i.e. spinach juice (SJ) as it contains contact mode.
sodium, magnesium, silicate, iron, protenious nitrogen
and other metallic constituents (Juicing for health.com). Radiant heat test analysis
Further, spinach is abundantly available in India and it is
Radiant heat test measures the amount of the heat radiated
considered as a value addition of this food material.
through the specimen. Test value of the specimen has been
Extensive study was conducted to assess the effect of SJ
established by ASTMF1939-08 method.
in different concentration on flame retardant properties of
cotton textile in terms of LOI, burning rate and thermo
gravimetry. Wash durability of finish
The fire retardant activity of the finished samples was
evaluated after being subjected to one wash cycle. The
Materials and methods finished fabrics were washed in a laundrometer using
A 200 GSM plain woven bleach cotton fabric of 30 EPI standard detergent 1 g/L at 40°C for 40 min. The fabric
(ends/inch), 40 PPI (picks/inch) with 25 s warp and 30 s was then rinsed in the running water for 5 min, followed
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weft counts procured from the local market was used in by drying at 100°C for 5 min. Then it was placed in a
the study. SJ used for the study was extracted from fresh desiccator for 24 h before conducting the flammability
spinach leaves of local market. Extracted juice was test.
filtered by Whatman No. 1 filter paper and prepared for
application in cotton fabric. Bleach cotton fabrics were Weathering fastness of finish
then impregnated with different composition of SJ and
Treated and untreated cotton fabric samples were
water 1:2, 1:1 and only SJ (1:0) at 90°C with material to
exposed directly under sunlight for measuring the
liquor ratio of 1:15 for 30 min. All the solutions have
weathering fastness as per ISO 105-B03-1978 (E)
been made alkaline at pH 10 with soda ash. Treated
method. However, the samples were protected from rain
fabric was then dried at 110°C for 5 min.
for 6 h each day from July to September and continued
for 300 h. After every 50 h, fire retardant property of the
Testing treated and untreated fabric was measured using LOI
value.
Before testing, treated cotton fabric samples were
conditioned for 48 h at 65% RH and 27°C.
Characterization of treated fabric
Determination of add-on% Thermogravimetry analysis
This property was determined by gravimetric principle Thermogravimetry (TG) measures the gradual weight loss
following oven dry weight method, taking bone dry of a sample with respect to time or temperature. It also
weight of the sample before and after the treatments and indicates the effect of flame retardant on the pyrolysis of
expressing the results as a percentage of the initial bone the polymer substrate (Mostashari & Mostashari, 2009).
dry weight of the material taken. The TG curves of the control and treated fabrics have
been established using thermogravimetric analyser
Add-on% ¼ ½M2 M1 =M1 100: (1) (METTLER TOLEDO TG-50/ MT5, Greifensee,
where M1 and M2 are the oven dry weight of the control Switzerland). The tensile strength, one of the most
and treated fabric samples, respectively. The reported important mechanical properties of both the treated and
results are average of five tests in each case. the untreated fabrics was evaluated on an Instron make
tensile tester as per ASTM D5035-2006 method.
Flammability assessment
Burning behaviour of the control and treated samples FTIR analysis
were evaluated by standard methods. For limiting The FTIR curves of the control and the treated fabrics
oxygen index (LOI) analysis, IS 13501 test method was were evaluated by Shimadzu IR Prestige 21 analyser
used. In horizontal flammability, the flame time and machine.
propagation rate were measured as per the FMVSS302N
standard. In vertical flammability, different parameters
were measured as per the 1871 method A. Maximum SEM and EDX analysis
temperature produced during burning of sample was For surface analysis of the control and the treated
measured using IR thermometer, Fisher Scientific made samples, scanning electron microscope Philips, Model
The Journal of The Textile Institute 3
XL-30 was used. EDX analysis was carried out in field of SJ in bleached cotton samples at different
emission gun scanning electron microscope (FEG-SEM). concentrations, the LOI value increased significantly. In
the bleached cotton fabrics treated with 1:2 SJ solution
(SJ: water ratio), the LOI value was found to increase to
Results and discussion 26, which is almost 1.3 times higher than that of control
Bleached cotton fabric samples have been treated with sample. With application of more concentrated SJ, the
different compositions of spinach juice and water. The add-on percentages increased from 3.5 to 8. As a result
results of the flammability testing of both the control as of this, LOI also increased linearly from 26 to 30. In all
well as the treated samples have been presented in the SJ-treated samples, as LOI value increased
Table 1. significantly, the samples do not catch flame. In vertical
flammability measurement, the control sample catches
flame readily and burnt the entire sample with flame
Flammability testing within 60 s, whereas SJ-treated sample (1:2) showed
LOI values and vertical flammability presence of flame only for 10 s (partial burning)
Bleached cotton fabrics were treated with different followed by combustion with afterglow in 295 s. This
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Table 1. Flammability properties of the control, mordanted and SJ: water-treated cotton fabric.
Figure 1. Comparison of burning behaviour between control and spinach leaves juice (SJ)-treated cotton fabrics at different time
interval.
SJ-treated sample with afterglow (after flame stopped) Radiant heat test analysis
decreased gradually with burning time. Initially, Amount of heat radiated through the fabric was
temperature was 285°C, followed by 250, 200 and measured and is reported in Table 2. As per this process,
finally 120°C with an interval of approximately, 60 s. It 20 kW/m2 heat flux was passed through the control as
will be very useful for the user in real life situation as well as treated fabric. Then the time required to increase
they will be getting much longer escape time (400 s) the temperature of both the fabrics by 12 and 24°C was
from the fire hazards zone or extinguish the flame. In recorded. It was observed that this time increased in case
contrast, the user will be getting hardly time (60 s only) of treated fabric by 14.28 and 12.1%, respectively. In
to escape from fire hazards if the fabric is not flame addition, amount of heat radiated (QC) through the fabric
retardant in the environment of temperature of ~400°C. is also 9% lower in treated fabric compared to the
In flame retardant finishing of any textile material, it will control one. Hence, SJ-treated sample not only radiated
be beneficial if burning with flame time could be less amount of heat but also increases temperature with
reduced and burning with afterglow time could be longer period of time (total burning time). As a result,
increased. This is because afterglow temperature (285– heat transmission factor (TF) of the treated fabric
120°C) is quite less than control sample. In the treated showed almost 20% lower compared to the control
fabrics as LOI value increased with the percentage add- fabric. Which again supports the high LOI value and
on of SJ, afterglow time was found to increase thermal stability of the treated fabric.
significantly from 0 s (control) to 295 s, 345 s and 400 s
for the 1:2, 1:1 and 1:0 SJ-treated samples, respectively.
The SJ-treated sample mostly burnt with afterglow and Table 2. Flammability parameters of the fabrics treated with
burning rate reduced significantly from 250 to 37.5 mm/ different methods.
min. Similar trends were also observed in horizontal
flammability measurement, where the burning rate Radiant heat test (heat flux Control SJ treated (1:0)
density 20 kW/m2) fabric fabric
reduced from 90 mm/min to 10 mm/min in 1:0 SJ-
treated sample, which is 10 times lower than the control T12 (s) 7.7 8.8
sample. In the control as well SJ-treated samples, char T24 (s) 14.9 16.7
length was not observed as the samples completely QC (kW/m2) 9.240 8.421
TF 0.471 0.430
burnt.
The Journal of The Textile Institute 5
observed. Third stage of weight loss occurred over the pyrolysis stage, only 54% mass loss was observed.
600°C temperature due to dehydration and char Amount of this mass loss is intermediate between A
formation. The TG curves of the control (B) cotton (30% loss) and B (78% loss). Hence, it can be deduced
fabric evidenced three stages, in the initial stage at the that spinach juice treatment widens (50°C wider) the
temperature below 100°C. Here, the mass loss occurred pyrolysis region and also reduces the amount of mass
mostly due to the loss of absorbed moisture from the loss in the pyrolysis range. In addition, it reduces the
polymer (Mostashari & Mostashari, 2009). However, the combustion temperature of the cellulosic substrate with
main pyrolysis stage occurred over the 280–380°C the dilution of flammable volatiles by the generation of
temperature range with the peak in the main loss non-oxidizable CO2, H2O at comparatively low
occurred at 300°C. In this stage with rapid mass loss temperature. It can also be observed from the TG curve
(78%), cellulose pyrolysis products might be formed that in the third stage, the treated fabric started char
(Xing, Liu, Li, & Chen, 2012). Above 380°C, formation at a lower temperature and the quantity of
Figure 2. TGA curves of the dried spinach powder (A), control cotton fabric (B) and spinach juice-treated (1:0) (C) cotton fabrics.
6 S. Basak et al.
char residue remained higher compared to the control of inorganic salts have also been detected in EDX
fabric at higher temperature. It started char formation at analysis (discussed below). The curve A pertaining to
around 330°C which is 20–30°C earlier than the control the control cotton fabric showed peak at 3445 cm−1
cotton fabric. Therefore, as compared to the control corresponding to intramolecular –OH stretching,
cotton fabric, char residue remains at 500°C increases including hydrogen bonds. Peak observed at 1161 cm−1
from 13 to 30%. It shows that Spinach juice also had a might be assigned to the C–O–C assymetric stretching of
positive effect on earlier dehydration and char formation. B-glucosydic linkage of cellulose. CH and CH2
This is true that there was less degradation of spinach stretching was indicated by 2898 cm−1 the (Cilurzo,
juice (A) over the range of temperature; hence, the Selmin, Minghetti, & Montanari, 2005). As far the curve
spinach juice-treated sample could retain more masses at C is concerned, it shows large and more intense peak of
higher temperature. Similar results were also observed in water at 3300 cm−1. Calculated area of this peak of
vertical flammability test, where the sample does not curve C between 2600 and 3600 cm−1 is the addition of
catch flame. The result indicates the thermal stability of the area shown by the curve A and B in the same
the spinach juice-treated sample over the temperature region. It proved that more amount of bound and
range of 50–600°C. In the treated samples, the reduction unbound water molecules present in the treated fabric
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in flammable gas production and increase in char also assist to exhibit fire retardant property.
formation, both have helped the sample to be flame
retardant. Therefore, it is obvious to conclude that
spinach juice increases the overall resistance of the SEM and EDX analysis
treated cotton fabric to thermal degradation and it also The SEM images of the control and SJ-treated (1:0)
reduced considerably the rate of weight loss of cellulose. cotton fabric are shown in Figure 4. It can be seen from
Figure 4(A), control sample is clean and there is no
coating and deposition. However, after SJ treatment
FTIR analysis (1:0), coating of SJ could be easily visible as shown in
Figure 3 shows the FTIR spectra of the various samples. Figure 4(B). SJ is uniformly distributed over the entire
It can be clearly observed that there is no significant surface. Energy dispersive X-ray analysis of the control
change between curve A and C. The curve B pertaining and the SJ-treated fabric is represented in Figure 5 and
to the dried SJ showed wide band for water from 2600 data are reported in Table 3. As expected, the control
to 3600 cm−1. Peaks observed between 800 and sample showed only the presence of carbon and oxygen
900 cm−1 are indicated mainly due to the presence of atom as the technique cannot detect hydrogen atom.
inorganic salts in SJ (Karastergiou & Philippou, 2000). However, in SJ-treated (1:0) sample, several atomic
Small peaks observed at 800 and 850 cm−1 might be peaks are easily visible as shown in Figure 5. These are
assigned to sodium chloride and magnesium chloride corresponding to sodium, magnesium, silicon and
salt, respectively, (Miller & Wilkins, 1952). These types chlorine. It can be seen that in the SJ-treated cotton
Figure 3. FTIR analysis of control fabric (A), dried spinach juice (B) and SJ-treated (1:0) fabric (C).
The Journal of The Textile Institute 7
Figure 4. SEM images of Control fabric (A), SJ-treated (1:0) fabric (B).
Table 3. Atomic percentage of control (A) and SJ-treated (1:0) cotton fabric measured using EDX.
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Figure 5. EDX images of control (A) and SJ-treated (1:0) (B) cotton fabrics.
fabric, sodium percentage is more followed by protection from flame. First bleaching and mercerization
magnesium compared to other atoms. It is seen that of cotton fabric followed by application of SJ with
compared to control, in the SJ-treated sample carbon different concentration in alkaline condition ensures the
percentage is significantly lower (27.2%). However, good add-on (3.5–8% uptake). This implies that cotton is
oxygen percentage increased by 7.5%. The elements becoming flame retardant mainly because of SJ and its
except sodium are present in the pure SJ as well SJ- chemical composition. The effect of flame retardancy
treated sample in form of either metal chloride or metal imparted by SJ may be attributed to the presence of
phosphate. Sodium is coming mainly due to presence of mineral salts in the SJ. Metals are present in the cotton
partial soda ash and from SJ. Silicon is present in SJ- textile in the form of chloride such as sodium silicate,
treated fabric in form of silicate (SiO2 or Na2SiO3). magnesium chloride, sodium chloride, etc. In the
presence of these peaks, molecules were also observed
in FTIR analysis and peaks of the elements in EDX
Mechanism of flame retardant property analysis. From the various characterizations, it is
It was seen that cotton being pure cellulosic in nature, it presumed that mineral salts presents in SJ might have
has low LOI value of 18 and does not show any retarded the thermal decomposition of cellulose, and
8 S. Basak et al.
contributed to dehydration process by increasing the Table 4. Weathering durability of control and treated fabric.
amount of char formation, as shown in TG curve.
LOI value
Chloride- and silicate-containing molecules are known to
be flame retardant in literature (Sharma, 1986). Besides, Exposure period in sunlight SJ treated (1:0)
presence of water molecules as shown in FTIR curve C, (h) Control sample
in SJ-treated fabric might have contributed in preventing 0 18 30
the rise in temperature of sample by absorbing heat of 50 18 30
evaporation (540 cal/gm). The presence of moisture peak 100 18 30
has been observed in FTIR spectra and TGA curve C. 150 18 30
200 18 29
Therefore, the flame retardancy effect in the SJ-treated 250 18 30
cotton fabric might have possibly attributed to combined 300 18 29
effect due to presence of (i) metals salts, (ii) silicate and
(iii) bound and unbound water molecules. These have
helped in more char and non-flammable gases formation
such as CO2 and H2O. These gases might have also
Table 5. Flammability parameters control, treated and washed
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