Fibers and Polymers 2015, Vol.16, No.

2, 388-396 ISSN 1229-9197 (print version)

DOI 10.1007/s12221-015-0388-z ISSN 1875-0052 (electronic version)

Enhanced Flame Retardancy of Cotton Fabrics with a Novel Intumescent

Flame-Retardant Finishing System
Dawei Jiang1,2, Caiying Sun1*, Yining Zhou1, Hong Wang1, Xingru Yan2, Qingliang He2,
Jiang Guo2, and Zhanhu Guo2*
1
Heilongjiang Key Laboratory of Molecular Design and Preparation of Flame Retarded Materials,
Northeast Forestry University, Harbin 150040, China
2
Integrated Composites Lab, Dan F. Smith Department of Chemical Engineering, Lamar University,
Beaumont 77710, USA
(Received September 16, 2014; Accepted October 3, 2014)

Abstract: Imidazole spirocyclic phosphoramidate (ISPA) has been synthesized through one-step reaction between
spiralphosphodicholor (SPDPC) and imidazole. The optimal flame-retardant finishing for cotton fabrics process was
4
designed by orthogonal experiment L (5 ) and the finished cotton fabrics with different formulas of aqueous solution
25

containing ISPA, phosphoric acid, and cyanuric acid were prepared. The limiting oxygen index (LOI) to characterize the
minimum amount of oxygen needed to sustain a candle like flame revealed that this novel intumescent SPDPC flame system
exhibited an excellent flame retardant efficiency on the cotton fabric finished with the optimal formula possessing a high LOI
value of 36.6 %. The cotton fabric was investigated by vertical flame test revealing a combustion characteristic of the lowest
damaged length (64 mm) without continuing burning and no smoldering. The flame-retardant cotton fabric showed an
acceptable decreased tensile strength by 13.3 % and enhanced excellent thermal stability compared with pure cotton fabric.
Cone calorimeter test revealed a reduced heat release rate by 57 % and a decreased total heat rate by 60 % for the flame-
retardant cotton fabric compared with pure cotton fabric. Scanning electron microscopy (SEM) indicated a solid and tough
residue for the burned flame-retardant cotton fabric as compared with the very loose and brittle residue of the burned pure
cotton fabric.
Keywords: Cotton fabric, Intumescent flame retardant, Flame retarding finishing, Orthogonal experiment, Fire properties

Introduction adopted by the U.S. require all mattresses to meet the

requirements set forth in the U.S. standard for flammability
Textiles are utilized extensively throughout clothing, of mattresses. This regulation requires mattresses to be
firefighter uniform, student uniform, fabric furniture, institutional cigarette resistant and all fabrics used for clothing purposes
upholstery, military garments, professional racer’s garments, must meet an open flame ignition standard. There are many
mattresses, and bedding with an aim to make our lives more approaches such as grafting flame retardant groups in
comfortable [1-3]. Cotton fabric is an important textile polymer materials to improve flame resistance of the
widely used to produce apparel, home furnishings, and various materials or adding fire retardant into polymer materials directly
industrial products due to its characteristics of softness, to retard inflaming in a material. Mechanical incorporation
breathability, and capability to absorb moisture [4-6]. Cotton of flame retardant additives into cotton fabric is mostly low
fabrics have also been used in both military and civilian cost and fast blending technique to reduce the flammability
areas due to their comfortable, natural, renewable, and of fabric [14].
environmentally friendly properties [7,8]. However, a vital There are many researches of flame retardant on cotton
drawback of cotton fabric, i.e., flammability, limits its use. It and the research of intumescent flame retardant on cotton is
ignites easily and is frequently implicated in fire. Cotton one of them [14,15-17]. Intumescent flame retardants (IFR)
cellulose undergoes degradation on ignition, forming highly have attracted increasing attention in the flame retardation of
combustible volatile compounds mainly levoglucosan with materials because they produce low smoke and toxicity
the propagation of fire causing injuries and fatalities in fire without producing corrosive gases [18]. The IFR system is
accidents [9-11]. Low thermal stability, easy ignition, and usually composed of three components: an acid source, a
rapid combustion of cotton fabric represent their weaknesses carbonization agent, and a blowing agent [19,20]. The
and limitations in the production of high performance and spiralphosphodicholor (SPDPC) has attracted great interests
fire-protective textile products so that flame resistance is of due to its unique functions to act as one of the most
importance for cotton textiles to meet various mandatory important reaction intermediates for introducing more
flammability standards [12,13]. For example, regulations functional groups and to improve the thermal stability of
polymers [21]. SPDPC should be cooperated with other
*Corresponding author: [email protected] nitrogenous compounds to form IFR and a lot of researchers
*Corresponding author: [email protected] paid their attentions to synthesize IFR with a combined

388
Flame-retardant Finishing for Cotton Fabrics Fibers and Polymers 2015, Vol.16, No.2 389

highly active functional groups in both ends, which was

white powder and the melting point (M.P) was 234-236 oC
[32,33]. The details of the preparation of SPDPC are in the
literature [34]. Acetonitrile (CH3CN, 1480 ml), pentaerythritol
(PER, 80 g), and phosphorus oxychloride (136 ml) were
slowly added into a 2 l glass flask, stirring for 1 h at 82 oC
Scheme 1. Structure of SPDPC. till the system turned to colorless solution under nitrogen
atmosphere. AlCl3 (0.5 g) powder was added as catalyst into
system 1 h later since the system became colorless. And
SPDPC and nitrogenous compounds in flame retarding of another 0.5 g catalyst was added to the system per half an
polypropylene [22], acrylonitrile-butadiene-styrene copolymer hour for another six times then the reaction was refluxed for
[23], polyethylene [24], ethylene vinyl acetate copolymer 1.5 h. The molecular structure of SPDPC is shown in
[25], polyurethane foam [26], epoxy resin [27], and Scheme 1.
polycarbonate [28]. However, there is no report about
effective IFR with a combined SPDPC and nitrogenous Synthesis of ISPA
compounds in flame retarding of cotton fabrics. The synthesis of ISPA is briefly described as follows. 1.64 g
In this work, imidazole spirocyclic phosphoramidate (ISPA), imidazole and 50 ml dichloromethane were added into a
a novel intumescent flame retardant containing a combined three-necked round-bottomed flask provided with a mechanical
SPDPC and nitrogenous compounds is synthesized through stirrer reflux condensing tube and temperature control system,
one-step reaction of imidazole with SPDPC, which is a kind then the mixture was stirred at room temperature till the
of effective and environment-friendly halogen-free IFR mixture became clear from turbid. Then 3 g SPDPC and 2.8 ml
containing phosphorus-nitrogen elements flame retardant triethylamine were added into the mixture, and the temperature
[29,30]. The molecular structure of SPDPC is shown in was increased to 40 oC and maintained at that temperature
Scheme 1. The flame retardant finishing of cotton fabric is for 6 h with stirring. The mixture was filtered and washed
prepared through the finishing process with ISPA as several times with acetone. The samples and methanol were
intumescent flame retardant system, phosphoric acid as added into a conical flask with an economical allihn condenser
catalyst system, and cyanuric acid as cross-linking agent to reflux for 2 h, and then the liquid phase was filtered
system. The optimum condition of finishing process is immediately. Colorless transparent acicular solid came out
determined by the orthogonal experimental [31]. The flame when the temperature was cooled down, and then filtered.
retardancy of the samples was characterized by the limiting Finally, the samples were dried in a vacuum oven overnight
oxygen index (LOI) and vertical flammability testing. The at 70 oC. The ISPA is white powder and M.P is 178-180 oC.
oxidative thermal degradation was studied by thermogravimetry Analysis calculated for C10H14O6N4P2 is C (34.48 %), H
(TGA). The burning behavior was carried out by cone (4.02 %), N (16.09 %), and P (17.81 %). Values found
calorimeter. The mechanical properties were analyzed by through elemental analysis are C (34.42 %), H (3.99 %), N
unidirectional tensile testing. The evolution of surface (16.05 %), and P (17.76 %), indicating that the calculated
morphologies of pure cotton fabric and fabric finished with element content correspond with the found one and the target
optimal combination before and after cone calorimeter test product is obtained. The reaction process is represented in
were studied by a field emission scanning electron microscope Scheme 2.
(SEM).
Flame Retardant Finishing of Cotton Fabric
Experimental Optimization of Finishing Process
In the present study, an orthogonal array experimental
Materials design was used for selecting the optimum condition of
100 % cotton fabric with a fabric density of 261 g/m2 was experimental factors on the limiting oxygen index (LOI) of
supplied by Jiulong Cloth Industry Co., Ltd. (Suzhou, cotton fabrics and twenty-five groups of experiment plans
China). Phosphoryl chloride, pentaerythritol, and imidazole with five levels and four factors, L25 (54) were adopted
were purchased from Guangfu Fine Chemical Research where the following four variables were analyzed: the
Institution. Dichloromethane, acetone, and triethylamine
were purchased from Tianjin regent chemical company,
China. Cyanuric acid was purchased from Qianruida Chemical
Co., Ltd. (Puyang, China). Phosphoric acid was purchased
from Shuangshuang Chemical Co., Ltd. (Laiyang, China).
The SPDPC was synthesized by pentaerythritol and
phosphorus oxychloride in the laboratory containing two Scheme 2. Reaction process of ISPA.
390 Fibers and Polymers 2015, Vol.16, No.2 Dawei Jiang et al.

Table 1. Factors and levels of the orthogonal design 75 % or to 100 mm for fabrics having an elongation at
Factor maximum force of more than 75 % and the gauge speed was
ISPA Catalyst Cross-linking Cure 100 mm/min [39].
Level The thermal stabilities of the treated samples were evaluated
loading content agent loading temperature
(wt%) A (wt%) B (wt%) C o
( C) D by thermogravimetric analysis (TGA), using a Perkin Elmer
1 10 0 0 140
Pyris1 TG analyzer including 3-5 mg samples from 50 to
800 oC with a heating rate of 10 oC/min, and the atmosphere
2 15 0.5 0.5 150
is continuous N2 flow of 50 ml/min [40].
3 20 1.0 1.0 160 Thermal combustion behaviors of the cotton fabrics before
4 25 1.5 1.5 170 and after flame retardant treated were examined using an
5 30 2.0 2.0 180 oxygen consumption calorimeter (cone calorimeter, Fire
Testing Technology, East Grinstead, UK) at an incident heat
flux of 35 kW/m2 according to ISO 5660 [41,42]. The
loading of ISPA wt% (factor A), the content of catalyst wt% specimens were wrapped in an aluminium foil and were
(factor B), the loading of cross-linking wt% (factor C), and fixed by a non-combustible mineral fiber mat. All samples
cure temperature oC (factor D). (100×100 mm) were measured in the horizontal position
Flame-Retardant Finishing Process using the retainer frame. The device consisted of a radiant
First the cotton fabric (10 g) was boiled in boiling water electric heater in a trunk-conic shape, an exhaust gas system
(500 ml) for 30 min to remove the impurity from the cotton with oxygen monitoring and instrument to measure the gas
fabric and put them at room temperature till the moisture flux, an electric spark for ignition, and a load cell to measure
volatilize out completely. Then pure cotton fabrics were the weight loss.
immersed in 300 ml aqueous solution containing some The surface morphology of the cotton fabric before and
formulas shown in Table 1, where ISPA was used as after burning was studied using a FEI Quanta 200 scanning
intumescent flame retardant system, phosphoric acid as electron microscope. The fabric pieces (10×10 mm) were
catalyst system, and cyanuric acid as cross-linking agent cut and fixed to conductive adhesive tape. All the samples
system with stirring for 30 min at room temperature. were sputter-coated with a gold layer before test for better
Afterward they were padded in a laboratory padding frame imaging.
with an approximately 100 % wet pick-up, dried at 80 oC in
an oven for 5 min and cured at a series of temperature that Results and Discussion
were also shown in Table 1 for 3 min [35].
Orthogonal Experiment for Determining LOI
Characterization Table 2 shows the result and analysis of the orthogonal
The LOI values of some samples were carried out on a JF- experiment L25 (54). According to the L25 (54) matrix, 25
3 oxygen index instrument (Jiangning, China) according to experiments were carried out. This table also illustrates the
ASTM D2863-09 standard method with sheet dimensions of range of the LOI on various factors and levels. LOI values
130×60 mm, and a mixture of oxygen and nitrogen is passed indicate the minimum amount of oxygen needed to sustain a
up through a cylinder containing the fabric specimen supported candle like flame when the sample was burned in an
vertically [36]. The minimum fraction of oxygen in a atmosphere of oxygen and nitrogen.
mixture of oxygen and nitrogen in which one specimen was It can be clearly seen from the results of orthogonal
just sustained burning was determined and reported as the experiment that the higher the ISPA loading is, the higher the
LOI value. Vertical flame test was performed on strips of LOI value is not always. The maximum loading of ISPA is
cotton fabric (300×76 mm) according to ASTM D-6413-08 30 % (level 5) and the minimum loading of ISPA is 10 %
on a CZF-3 vertical flame test instrument (Jiangning, China), (level 1). In terms of level 5, there are five different values of
five pieces of the longitudinal (vertical) cotton fabrics and LOI. The highest value of LOI of these five different values
five pieces of latitudinal (horizontal) cotton fabrics were is for the cotton fabric treated with trial 21 and the other four
chosen for vertical flame test, respectively. The ignition time values are lower than for trial 21. Even some of LOI values
for the test is 12 s and the height of fire was approximately in level 1 are higher than that of other four values in level 5,
40±2 mm [37,38]. indicating that the loading of ISPA synergistically plays an
Tensile properties of the cotton fabric before and after important role on flame retardancy of the cotton fabric with
flame retardant treatment were carried out on a RGT-20 with other factors. The best level for each factor is level 5 of ISPA
microcomputer control electronic universal testing machine loading, level 4 of catalyst content, level 5 of cross-linking
(Shenzhen, China) according to ISO 13934-1:1994. The agent loading, and level 4 of cure temperature, respectively,
gauge length of the tensile-testing machine was set to that is, the optimal combination is A5B4C5D4 from Table 2.
200 mm for fabrics with elongation at maximum force up to The LOI value of the cotton fabric finished with the optimal
Flame-retardant Finishing for Cotton Fabrics Fibers and Polymers 2015, Vol.16, No.2 391

Table 2. Result and analysis of the orthogonal experiment of L 25 combination (using the level 5 of ISPA loading, level 4 of
4
(5 ) catalyst content, level 5 of cross-linking agent loading, and
Trial Factor Factor Factor Factor LOI level 4 of cure temperature) is 36.6 % from Table 3.
number A B C D (%) Compared with pure cotton fabric, the LOI with treatment of
Pure cotton 18.7 an optimal combination is increased by 95.7 %. Any materials
fabric with a LOI of less than 21 % will burn easily in air, and in
the range of 21 to 27.9 % the materials are known as slow
1 1 1 1 1 24.9
burning [43]. There are eight trials which the LOI values are
2 1 2 2 2 27.8 over 28 % among all orthogonal experiments and they are
3 1 3 3 3 29.8 trial (3rd, 4th, 5th, 9th, 10th, 17th, 21st, and 24th). For
4 1 4 4 4 30.1 further research, these eight groups were used and the
5 1 5 5 5 29.5 sample finished with the optimal combination of cotton
fabric was used for vertical burning test and tensile test.
6 2 1 2 3 26.2
7 2 2 3 4 26.6 Vertical Flame Test
8 2 3 4 5 26.8 Vertical flame test results in Table 3 show that the cotton
9 2 4 5 1 28.7 fabric finished with an optimal combination demonstrates
10 2 5 1 2 28.2
the highest LOI compared with pure cotton fabric and trial
3rd, 4th, 5th, 9th, 10th, 17th, 21st, and 24th samples. The
11 3 1 3 5 26.9 pure cotton fabric is damaged completely (300 mm), after
12 3 2 4 1 26.6 ignition the cotton fabric with a continued burning along
13 3 3 5 2 27.4 with black smoke. The ignition and smolder process
14 3 4 1 3 27.7 continued for 33.6 and 103.0 s, respectively. Peoples often
died from the smoke in the real fire rather than from burning.
15 3 5 2 4 27.1
For samples of trial 3rd, 4th, 5th, 9th, 10th, 17th, 21st, 24th,
16 4 1 4 2 26.6 and cotton fabric finished with an optimal combination, no
17 4 2 5 3 28.2 additional combustion and smoke were observed after the
18 4 3 1 4 27.4 fire was removed from the samples. Figure 1 shows the
19 4 4 2 5 26.9 images of cotton fabric after vertical flame test. The
damaged lengths of 17th, 24th, and cotton fabric finished
20 4 5 3 1 27.7
with optimal combination are between 64-68 mm, the cotton
21 5 1 5 4 34.2 fabric finished with optimal combination sample has the
22 5 2 1 5 27.3 lowest damaged length (64 mm), 3th has the longest
23 5 3 2 1 27.1 damaged length (104 mm). The 21th has a higher value of
LOI (34.2 %) than that of other samples except the sample
24 5 4 3 2 34.0
finished with an optimal combination treatment, though it
25 5 5 4 3 27.7 has a high damaged length (85 mm), indicating that LOI is
K1 141.99 138.72 135.39 132.93 not necessary to be related with the vertical flame test.
K2 136.47 136.42 134.93 143.93
K3 135.67 138.46 144.91 139.45 Tensile Property
Breaking strength and breaking elongation data of trial
K4 136.67 145.28 137.83 145.35
3rd, 4th, 5th, 9th, 10th, 17th, 21st, 24th, and cotton fabric
K5 150.19 140.14 145.96 137.36 finished with optimal combination are listed in Table 3.
k1 28.40 27.74 27.08 26.59 The pure cotton fabric has the highest breaking strength
k2 27.29 27.28 26.99 28.79 and the breaking elongation (386.6 N and 87.5 %). The
breaking strength of finished cotton fabric decreases a little
k3 27.13 27.69 28.98 27.89
from 338.3 to 308.1 N. The breaking elongation also declines
k4 27.33 29.06 27.57 29.07 after the finishing treatment. There is no apparent connection
k5 30.04 28.03 29.19 27.47 between the amount of ISPA and the value of tensile test and
Range (R) 2.91 1.78 2.20 2.48 there is also no relationship between the value of LOI and
Best level A B C D the value of tensile test. After finishing treatment, however,
5 4 5 4

the value of tensile test decreases. This is due to the

Optimal A B C D
5 4 5 4
introduction of ISPA and cross-link agent, which could
combination
make the cotton fabric hard and brittle. The hard and brittle
392 Fibers and Polymers 2015, Vol.16, No.2 Dawei Jiang et al.

Table 3. Vertical flame test and tensile strength of the chosen flame-retardant cotton fabric
No. in LOI Vertical burning test Tensile performance
No.
OE (%) T (s)
c
T (s)
S
DL (mm) ΔDL (%) BS (N) ΔBS (%) BE (%) ΔBE (%)
1 Pure cotton 18.7 33.6 103 300 100 386.8±1.4 0 87.5 0
2 3 29.8 0 0 104 34.7 338.3±2.0 12.5 78.5 10.3
3 4 30.1 0 0 79 26.3 314.8±1.8 18.6 67.7 22.6
4 5 29.5 0 0 81 27 309.1±2.3 20.1 71.3 18.5
5 9 28.7 0 0 72 24 338.5±2.3 12.5 64.3 26.6
6 10 28.2 0 0 74 24.7 338.7±1.9 12.4 65 25.8
7 17 28.2 0 0 67 22.3 344.0±1.6 11 61.5 29.7
8 21 34.2 0 0 85 28.3 308.1±1.3 20.3 66.4 24.1
9 24 34.0 0 0 68 22.7 312.5±1.7 19.2 58.7 33
10 Optimal 36.6 0 0 64 21.3 335.4±1.3 13.3 64.1 26.7
OE: orthogonal experiment, T : time of continue burning, T : smouldering time, ∆L: damaged length, ΔDL: the percentage of the total dam-
c S

age length, BS: breaking strength, ΔBS: breaking strength declined percentage, BE: breaking elongation, ΔBE: breaking elongation
decreased percentage.

Figure 1. The damaged length after vertical flame test of (A) pure
cotton fabric, (B) the 3th treatment, (C) the 24th treatment, and (D)
the cotton fabric finished with an optimal combination treatment.

cotton fabric makes the tensile strength decrease but there is

no significant decrease of the finished cotton fabric. The
cotton fabric finished with an optimal combination treatment
has the highest LOI value (36.6 %) and its breaking strength
is decreased a little (335.4 N) compared with pure cotton
fabric (386.8 N). It is just decreased by 13.3 % compared
with pure cotton fabric. The cotton fabric finished with
optimal combination has the highest value of LOI, the
lowest damaged length and an acceptable decrease of tensile
strength. So the optimal combination treatment was chosen
to do TGA and cone calorimeter test.
Figure 2. (A) TGA and (B) DTG curves of cotton fabric with and
Thermal Stability without finished treatment, (a) pure cotton fabric and (b) cotton
The pyrolysis properties of pure cotton fabric and the fabric treated with optimal combination.
Flame-retardant Finishing for Cotton Fabrics Fibers and Polymers 2015, Vol.16, No.2 393

cotton fabric finished with optimal treatment in orthogonal different in the TGA and DTG curves after finished. There is
experiments were investigated by TG/DTG (Figure 2). The only one main degradation step of cotton fabric after
pyrolysis process is a complex reaction containing various finished. In case of finished cotton fabric, the temperature of
reactions, including endothermic bond rupture, volatilization, degradation begins at a relatively lower temperature of
and exothermic bond formation [44]. Figure 2 shows that 168 oC compared with that of pure cotton fabric (300 oC).
there are two main thermal degradation steps for pure cotton After 168 oC, the fabric is degraded rapidly and reaches a
fabric, where the temperature range is below 300 oC, there is maximum degradation rate of 10 %/min at 300 oC. Large
nearly no thermal degradation and only a very slightly amounts of char were formed after 316 oC and even though
weight loss (below 3.0 %) due to the physical properties that at 600 oC, it also left vast chars of 30 %. All of these could
is the amorphous region of polymer damages occurred be ascribed to the addition of IFR system. The IFR has a
during this temperature [45]. The first main thermal degradation barrier effect of intumescent carbonaceous char created by
is in the temperature range of 300 to 380 oC. In this stage, the the combined actions of three components of IFR [47].
weight loss is very fast and significant due to the decomposition During the heating, the IFR is decomposed at a lower
of cellulose [46]. The first maximum decomposition tem- temperature (168 oC) before that of cotton fabric (300 oC)
perature of pure cotton fabric is at 350 oC with a maximum and the IFR forms the char quickly which can prevent the
decomposition rate of 20 %/min. During this step, the degradation of cotton so that the flame properties of cotton
aliphatic char was yielded delay the decomposition of cellulose fabric were increased.
so there is a slow decomposition in the second main thermal
degradation step and the second maximum decomposition Cone Calorimeter
temperature of pure cotton fabric is at 525 oC with a Figure 3 shows the curves of heat release rate (HRR) and
maximum decomposition rate of only 1.6 %/min. There is total heat release (THR) of the cotton fabrics before and after
scarcely any char left after 600 oC due to the degradation of flame retardant finishing. It is shown completely different
the cellulose. The cotton fabric can be observed completely curves between pure cotton fabric and finished fabric. The

Figure 3. (A) Heat release rate curves, (B) total heat release curves of (a) pure cotton fabric and (b) cotton fabric finished with optimal
combination, (C), (D) digital photos of the residues after cone calorimeter test for pure cotton fabric and the cotton fabric finished with
optimal combination, respectively.
394 Fibers and Polymers 2015, Vol.16, No.2 Dawei Jiang et al.

Figure 4. Schematic of the char formation.

pure cotton fabric has faster HRR than finished fabric The surface of pure cotton fabric is smoother than that of
(Figure 3(A)). Peak of heat release rate (PHRR) of pure finished one before cone calorimeter test indicating that the
cotton fabric is 154 kW/m2, which is 57 % higher than that finished cotton fabric is coated by flame retardant system
of finished fabric (98 kW/m2). THR of pure cotton fabric successfully. The pure cotton fabric left tiny residue after
(4.0 MJ/m2 in 140 s) is also higher than that of finished cone calorimeter test, however the finished fabric was
fabric (2.5 MJ/m2 in 140 s) with 60 % higher than that of carbonized and maintained its original shape after cone
finished fabric. PHRR and THR are believed by many fire calorimeter (Figure 5(H)). The residue of pure cotton fabric
scientists to be the major determinant of the onset of looks loose and gossamer, however, the finished fabric has
flashover for cotton fabric furniture in the real fire situation no change compared with pure cotton fabric. It can also be
[48]. For our finished cotton fabric, it has an excellent flame observed (Figure 5(G)) that the residue is thin and smooth
property including very low PHRR and THR. It is due to the for the finished cotton fabric, but the residue looks solid and
flame retardant decomposed to release nitrogen-containing full of many blocks on it. This is due to the fact that the
gas which was diffused to the surface of cotton fabric and finished cotton formed the char during burning. The carbon
diluted the combustible gas at the same time, the phosphoric layer acts as a physical barrier, which can prevent heat to
acid was formed coated on the surface of the fabric to transfer into the surface of cotton fabric. It can also prevent
promote cellulose fiber dehydration and carbonization. The the release of combustible gases and the contact of oxygen
carbonizing layer plays an important role in the isolation of with the combustible gas at the same preventing the spread
heat radiation and oxygen transfer. Pure cotton fabric has no of fire [50,51].
carbon layer during combustion, heat and oxygen could
spread into the inner of cotton rapidly and promote the Conclusion
decomposition of cellulose, furthermore the decomposition
of cellulose promotes the combustion [49]. A novel intumescent flame retardant, ISPA has been
The digital photos of residues of pure cotton fabric and the synthesized using SPDPC and imidazole. The flame retardant
treated one after cone calorimeter test were shown completely finishing of cotton fabric was prepared with finishing liquid
different (Figure 3(C) and (D)). Pure cotton was observed to formula containing ISPA, phosphoric acid, and cyanuric
be almost burned out and the finished cotton formed acid. The optimal formula was chosen through the orthogonal
coherent and dense char and maintained its original shape experiment L25 (54). LOI test demonstrated the cotton fabric
with little shrinking. The mechanism of the char formation is finished with the optimal formula has a highest value of 36.6 %
shown in Figure 4. and vertical flame test shows that the cotton fabric finished
with optimal formula has the lowest damaged length (64 mm)
Evolution of Surface Morphology with no continuing burning and no smoldering. The cotton
SEM has been performed to assess the morphology of the fabric finished with optimal formula has an acceptable
cotton fabric before and after flame retardant finishing. tensile of 335.5 N, which is just decreased by 13.3 %. The
Surface morphologies of pure cotton fabric and fabric finished finished cotton fabric with optimal formula with an excellent
with optimal combination before and after cone calorimeter flame retardant left vast chars of 30 % even at 600 oC. Cone
test are shown in Figure 5(A) to (H). There is distinct calorimeter indicates that the cotton fabric finished with
difference between the pure cotton fabric and finished one. optimal formula has good combustible properties.
Flame-retardant Finishing for Cotton Fabrics Fibers and Polymers 2015, Vol.16, No.2 395

Figure 5. SEM microstructures of cotton fabric; (A) The pure cotton fabric×100, (B) the finished cotton fabric with optimal
combination×100, (C) the pure cotton fabric×1000, (D) the finished cotton fabric with optimal combination×1000, (E) the residue of the
pure cotton fabric after cone calorimeter×100, (F) the residue of finished cotton fabric with optimal combination after cone calorimeter×100,
(G) the residue of the pure cotton fabric after cone calorimeter×1000, and (H) the residue of finished cotton fabric with optimal combination
after cone calorimeter×1000.
396 Fibers and Polymers 2015, Vol.16, No.2 Dawei Jiang et al.

Acknowledgement Degrad. Stabil., 92, 720 (2007).

24. G. Huang, Y. Li, L. Han, J. Gao, and X. Wang, Appl. Clay
The authors would like to thank the Key Project in the Sci., 51, 360 (2011).
National Science & Technology Pillar Program during the 25. G. Huang, S. Chen, S. Tang, and J. Gao, Mater. Chem.
Twelfth Five-year Plan Period (No. 2011BAD08B01) for Phys., 135, 938 (2012).
financial support. Z. Guo acknowledges the National Science 26. D. Wu, P. Zhao, M. Zhang, and Y. Liu, High. Perform.
Foundation (NSF, CMMI 10-30755) USA. Polym., 25, 868 (2013).
27. X. Wang, L. Song, W. Xing, H. Lu, and Y. Hu, Mater.
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