82
W. Xing et al. / Thermochimica Acta 513 (2011) 75–82
1466 cm−1, assigned to the vibration of C O group, start to decrease
from about 200 ◦C and almost disappear around 450 ◦C.
the surface of cotton fabric. The MCC results showed that the flame
retardant effect correlated with the concentration of the monomer.
Hence, Cotton 3 had the lowest PHRR (119.7 W/g), THC (3.6 kJ/g)
and higher LOI value. Surface morphology of chars indicated that
treated cotton fabric maintained fiber integrity after burning and
revealed the formation of a layer of nonflammable coating on sur-
faces of the burned cotton fibers, which might insulate the inner
layers more efficiently during combustion. TGA results reflected
that with increase of concentration for flame retardant monomer,
the thermal stability for cotton textiles could enhance. Cotton 3
gave the highest char yield, 7.7% in air and 31.1% in nitrogen. TGA-
IR results showed that Cotton 3 had the lower temperature for the
peak release rate of water vapor, CO2 and carbonyl compounds,
higher intensity of absorption for water, and lower intensity of
absorption for CO2 and carbonyl compounds as compared with
Cotton 0.
The appearance of new peak at 1280 cm−1 in the FTIR spectra
[25] indicates that the phosphate group deviates from the aliphatic
structure and then forms PPA or re-links to the aromatic structures
at the temperatures over 300 ◦C. The appearance of new peak at
759 cm−1 implies aromatic structures are formed [26].
In this work, TGA-FTIR was used to analyze the gas products
during the thermal degradation process of Cotton 0 and Cotton 3.
Fig. 10 shows 3D TGA-IR spectra of gas phase in thermal degra-
dation of Cotton 0 (a) and Cotton 3 (b). In Fig. 10, peaks in
the regions of around 3400–4000 cm−1, around 2250–2400 cm−1
,
around 2100–2200 cm−1, and around 1600–1900 cm−1 are noted.
such as H2O (3400–4000 cm−1), CO2 (2250–2400 cm−1), carbonyl
compounds (representing aldehydes, ketones, carboxylic acids,
1633–1839 cm−1). As this figure shown, the process of thermal
degradation for Cotton 0 is different from Cotton 3.
Acknowledgements
The work was supported by the Program for the joint fund of
NSFC and CAAC (61079015), the Opening Project of State Key Labo-
ratory of Environmental Adaptability for Industrial Product, and the
Program for the graduate innovation fund of USTC and the youth
innovation fund of USTC.
Some FTIR spectra are shown in Fig. 11. It can be drawn that
the pyrolysis products for Cotton 0 (Fig. 11(a)) at the beginning
(from about 15 min) are mainly composed of a small amount of
H2O. With the increase of temperature (above 19 min), lots of water,
the earlier time (from about 13.5 min) compared with Cotton 0. And
it releases the similar gas products with Cotton 0.
The change for the intensity of the total evolved products versus
time is shown in Fig. 12(a). It can be seen that the intensity for
Cotton 3 is lower than that of Cotton 0. It can be interpreted that
flame retardant can catalyze the thermal decomposition of cotton
from further decomposition.
In order to further study the difference between Cotton 0 and
Cotton 3, some IR evolution curves of the identified gaseous species
are shown in Fig. 12(b). For example, H2O, CO2 and carbonyl com-
pounds are easily identified by their characteristic absorption. The
data obtained from Cotton 0 and Cotton 3 can be compared quanti-
tatively as the weight of sample during the testing of each sample
was kept constant (1 mg). As shown in Fig. 12(b), Cotton 3 has the
lower temperature for the peak release rate of water vapor. Cotton
perature of the peak release rates and higher intensity of absorption
for Cotton 3 clearly indicate their superior dehydrating action [6].
Release of CO2 and carbonyl compounds during the thermal
decomposition of treated and untreated fabrics is also shown in
Fig. 12(c) and (d). The rate of release of CO2 and carbonyl com-
pounds is lowered as compared with the untreated fabric.
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4. Conclusions
This paper has shown that tri(acryloyloxyethyl) phosphate
(TAEP) and triglycidyl isocyanurate acrylate (TGICA) monomers
could be easily polymerized on the surface of cotton under UV radi-
ation in the presence of Darocur1173. The results of ATR and SEM
showed that TAEP and TGICA polymer coatings were formed on