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Surface modification of polyester fabric using pol yvi nyl alcohol in alkali ne medium

Article in Indian Journal of Fibre and Textile Research · October 2012

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Indian Journal of Fibre & Textile Research
Vol. 37, September 2012, pp. 287-291

Surface modification of polyester fabric using polyvinyl alcohol

in alkaline medium
a
Swarna Natarajan & J Jeyakodi Moses
Department of Chemistry, PSG College of Technology, Coimbatore 641 004, India

Received 16 June 2011; revised received and accepted 21 September 2011

Chemisorption of polyvinyl alcohol (PVA) onto polyester fabric in alkaline medium has been conducted. The treated
fabric is characterized by scanning electron microscope, ATR-FTIR spectroscopy, contact angle, differential scanning
calorimetry and dyeability. The PVA treated polyester fabric shows improved hydrophilic character over intact and sodium
hydroxide treated PET fabrics.

Keywords: Contact angle, Differential scanning calorimetry, Polyester fabric, Polyvinyl alcohol

1 Introduction hydrophilic and to improve its comfort characteristics.

Polyethylene terephthalate (PET), commonly
called as polyester, is the widely used polymer for the
production of synthetic fibres over the past 50 years.
The wide use of PET is the result of its strength
combined with its resistance to chemicals, abrasion,
stretching, shrinking and wrinkling. However, the
disadvantage of PET fibre is its low hydrophilic
character and inactive surface. PET is a hydrophobic
fibre with a moisture regain of only 0.6 - 0.8% even at
100% relative humidity. The basic requirement of
fabric worn next to skin is that it should assist for
1
moisture release to the atmosphere . The conventional
modification of PET fibre properties is through strong
alkaline treatment under high processing temperature.
Alkaline finishing of polyester fabric with sodium
hydroxide changes fabric weight, strength, wettability
2-7
and aesthetics .
Altering the surface characteristics of polyester is
rather difficult due to its inactive chemical structure.
However, modifications of PET surface have been
reported using various techniques, such as chemical
introduction of sugars onto PET fabric using cyanuric
8 9
chloride , protein immobilization on PET film ,
10
application of silk sericin to polyester fabric and
11
cyclodextrin based finishes for polyester fabric .
In the present work, adsorption of PVA onto
polyester fabric has been carried out to modify the
surface properties of base polymer, to make it
——————————
a
To whom all the correspondence should be addressed.
E-mail: nchem2003@yahoo.co.in
12
Polyvinyl alcohol has been used in textile industries ,
13
as a sizing agent since it is a biodegradable polymer .
In this work, efforts have been made to chemically
bind PVA onto PET surface in alkaline medium.
Treating polyester structures with polyethylene
glycol and metal hydroxide has been reported
14
previously . Modification of the fabric surface
without involving hazardous organic solvents and
achieving permanent hydrophilic character is the
advantage of the chosen method.
2 Materials and Methods
2.1 Materials
The materials used in this study were (i) 100%
polyester fabric (plain weave, 55 gsm; epi 92, ppi 80)
and polyvinyl alcohol (C2H4O)n having 1700-1800
degree of polymerization (Loba Chemie Pvt Ltd,
Mumbai, India).
The chemicals used in this study, such as
hydrochloric acid, sodium hydroxide and sodium
sulphate, were of analytical grade. A basic dye
(supplied by Burgoyne & Burbidges & Co, Mumbai)
para-rosaniline hydrochloride (CI Number 42500)
was used for dyeing on polyester fabric.
2.2 Methods
2.2.1 Pretreatment of Polyester Fabric
Polyester fabric was immersed in 10 gpL HCl at
40°C and treated for 1 h at the same temperature
with material-to-liquor ratio 1:50 to get rid of the
11
added impurities .
288 INDIAN J. FIBRE TEXT. RES., SEPTEMBER 2012
2.2.2 Application of PVA onto Polyester Fabric
The pretreated PET fabric was immersed in 1N
NaOH solution containing 1.5% by weight of PVA.
It was kept in the bath at boil for 1 h. Then the
fabric was taken out and immersed in water at
15
boiling temperature for 10 min and soaped to
remove the physically held PVA, washed and dried
at room temperature.
In a separate bath, similar treatment was carried out
on polyester fabric without PVA. This sample was
considered as control fabric.
2.2.3 Test Methods
Moisture Regain
Moisture regain of the polyester fabrics (intact,
control and PVA treated) was determined as per the
AATCC test method 20A-1995, RA 24. The moisture
regain values were calculated using the following
equation:
Moisture regain =
Weight of conditioned fabric – Weight of dried fabric
×100
Weight of dried fabric
Water Retention
Absorptive capacity of polyester fabrics (intact,
control and PVA treated) was measured by standard
AATCC 21-1978 test method.
Identification of PVA in Fabric
The polyester fabrics (intact, control and PVA
treated) were tested for the presence of PVA. All the
samples were spotted with a drop of reagent A (boric
acid) and a drop of reagent B (iodine solution).
Photographs were taken after 5 min. Polyvinyl
alcohol reacts with boric acid and iodine to form a
16
blue colour .
Water Contact Angle
Water contact angle was measured on the polyester
fabrics (intact, control and PVA treated) using contact
angle measuring system (model Phoenix 300 Plus,
M/s Surface Electro Optics Co, Ltd, Korea). Drops
of water (volume 8.0 μL) were placed on the fabric
samples using a microsyringe. The measurements
were taken immediately after placing the water drop
and the variations followed for 10 min.
SEM Analysis
The surface morphology of polyester fabrics
(intact, control and PVA treated) was observed on
17
SEM (JOEL JSM-6360 model microscope, Japan).
FTIR Study
The ATR-FTIR measurements were carried
out on polyester fabrics (intact, control and PVA
treated) using an infrared spectrophotometer
18
(Thermoscientific Nicolet is10) . Attenuated total
reflectance (ATR) spectra were recorded at a
-1
resolution of 4 cm and accumulation of 32 scans.
DSC Study
The differential scanning calorimetry (DSC) for
intact, control and PVA treated PET fabrics was
carried out using Pyris 6 DSC thermal analyzer.
0
The rate of heating was adjusted at 10 C/min. DSC
0 0
traces were recorded from 25 C to 400 C under
19
nitrogen atmosphere .
Dyeing of Fabric
The dyeability of polyester fabrics (intact, control
and PVA treated) was studied using basic dye (para-
rosaniline hydrochloride). Dyeing was carried out at
boil for 2 h with a material- to-liquor ratio of 1:100 at
pH 9 (using sodium hydroxide). Sodium sulphate was
used as an exhausting agent. The dyed samples were
20
washed with hot water, soaped and dried.
Colour Strength
Colour intensities of the dyed PET fabrics were
measured using spectrophotometer (model: Premier
colour scan ss 5000 A) within the range of 400-700
nm. Reflectance values were measured and the
relative colour strength (K/S) was calculated using
Kubelka Monk equation.
3 Results and Discussion
Many trials were carried out on polyester fabric
using sodium hydroxide alone (0.25-2.0 N) and with
PVA at different concentrations (0.25-2.0% by weight
of PVA), time (15 min to 3 h) and temperature
(30-120°C) in different proportions. The weight loss
in the polyester fabric and characteristic changes are
considered. The effect of the PVA application on
polyester fabric in alkaline medium at low
concentration, low temperature and short duration is
found to be negligible, whereas at higher conditions
of concentration, temperature and time, the average
weight loss on the PET fabric is more than 25%.
Based on these, the optimized conditions for
application on the polyester fabric using sodium
hydroxide (1 N) and PVA (1.5%) have been fixed as
mentioned earlier in section 2.2. The data are
presented in Tables 1 and 2 and the effect is shown
in Figs 1-4.
3.1 Wetting Behavior of Polyester Fabric however only PVA treated fabric shows marginal
The water retention values of polyester fabric increase of around 1%.
treated with PVA in alkaline medium, sodium
hydroxide alone, and intact polyester are 99,115 and 3.2 Spot Test Effect of Polyester Fabric
144 % respectively. The PVA treated fabric exhibits The PET fabrics (intact, control and PVA treated)
about 45% and 29% rise in water retention capacity, were tested for the presence of PVA after 10
15
compared to the intact and sodium hydroxide treated washes . Photographs of fabrics subjected to spot
polyester fabric respectively. This may be due to the tests are given in Fig 1. When the PET fabrics are
effect of PVA which is bound to the polyester fabric spotted with reagents, blue colour is developed in the
and enhances the ability of PET fabric to hold more PVA treated sample, and no colour is obtained on the
water molecules. Trials have been carried out for control and intact PET fabrics. The development of
moisture regain of these polyester fabric samples, blue colour in the PVA treated PET fabric confirms
the permanent nature of attachment of PVA to PET in
Table 1—Water contact angle of PET fabric alkaline medium. Intact and control fabrics do not
Time, min
Water contact angle, deg develop colour confirming the absence of PVA as
well as starch which, if present, will develop purple
Untreated Control PVA treated
0 124.24 116.75 67.31 colour with this reagent.
1 119.56 107.52 56.79
3.3 Water Contact Angle in Polyester Fabric
2 113.88 100.99 53.45
3 104.24 97.15 33.86 Water contact angle of intact, control and PVA
4 93.05 94.80 <10 treated PET fabrics is given in Table 1. When a water
6 80.30 83.34 - droplet is placed on these fabrics, it spreads
8 55.56 73.95 - completely within 5 min in PVA treated PET fabric,
10 33.91 59.13 - whereas on the control and intact PET fabrics even
Table 2—DSC measurements of PET fabric after 10 min the water droplet does not spread fully.
PET fabric Temperature peak, °C ΔH, J/g PVA treated PET fabric shows a static water contact
Untreated 254.04 81.327 angle of 67.31° (<90°), indicating that the fabric is
21
Control 253.69 43.592 wetted by water easily . The control and intact PET
PVA treated 247.07 29.617 fabrics show static water contact values > 90°, which

Fig. 1—Spot test on (a) untreated PET fabric, (b) control PET fabric, and (c) PVA treated PET fabric

Fig.2—SEM photograph of (a) intact PET fabric, (b) control PET fabric, and (c) PVA treated PET fabric
 Fig.3—FTIR spectra of (a) untreated fabric, (b) control PET fabric, and (c) PVA treated PET fabric
Fig. 4—DSC of (a) untreated fabric, (b) control PET fabric, and
(c) PVA treated PET fabrics
reveals their hydrophobic character. Thus, this result
shows the enhanced hydrophilic character of PVA
treated fabric.
3.4 Spectral Investigation of Polyester Fabric
3.4.1 SEM Analysis
The surface morphology of intact, control and PVA
treated PET fabrics is shown in Fig. 2. Figure 2c
shows the presence of PVA on the surface of PET
22
fabric, it does not fill up the interstices . SEM
photograph of sodium hydroxide treated control
fabric (Fig. 2b) shows that sodium hydroxide
influences the swelling of PET fabric than that of
intact fabric (Fig. 2a).
3.4.2 FTIR Analysis
The ATR-FTIR spectra of intact, control and PVA
treated PET fabrics are shown in Fig.3. The high
-1 -1
peaks from 1700 cm to 600 cm indicate the original
signals, such as characteristic spectra of stretching
-1
vibration band of C=O at 1730 cm and C-O-C
-1 -1
stretching vibration band at1097 cm and 1240 cm .
All these peaks confirm the existence of ester
23
linkage . Sodium hydroxide treated control fabric
-1
shows an additional peak at 2359 cm . This is
attributed to carboxylic group (–COOH), introduced
on the surface due to hydrolysis of the ester linkage.
The PVA treated PET fabric shows a broad band in
-1
the region 3435 cm which shows the presence of
-1
hydroxyl groups and the peak at 2359 cm is absent in
this fabric. This confirms the adsorption of PVA onto
the PET surface. This can be due to the attachment
of PVA on PET fabric surface by base catalyzed
trans-esterification reaction.
3.5 Thermal Analysis of Polyester Fabric
Thermo-physical properties of the PET fabric
samples are studied using differential scanning
24
calorimeter . Thermal curves of intact, control and
PVA treated PET fabrics are given in Fig.4. The data
are given in Table 2. Melting temperature of PVA
attached PET fabric exhibits a drop of 7°C compared
to intact fabric. The average heat of fusion of PVA
treated fabric is found to be 29.617 J/g, whereas that
of intact fabric is 81.327 J/g. Heat of fusion is the
energy involved in formation and melting of
crystalline regions. It is proportional to %
crystallinity. The heat of fusion decreases after
treatment of fabric with PVA, indicating a loss in the
25
degree of crystallinity of the fabric , and loosening of
compact structure of PET.
3.6 Dyeability of Polyester Fabric
The PET fabric samples (intact, control and PVA
treated) were dyed using basic dye para-rosaniline
hydrochloride, and the K/S values obtained are
1.579, 2.218 and 1.956 respectively. The basic dye
binds well with carboxylic group present in the
26
textile fabric . K/S value can be taken as a
indication of the amount of carboxylic groups
present in the PET fabric. Of the three samples, the
NaOH treated polyester fabric (control) shows the
highest K/S value due to the improved dye uptake by
the reaction between basic dye and carboxyl group in
27
control PET fabric . PVA treated PET fabric shows
a lower K/S value as the carboxylic acid group in
PET fabric for the linkage (dye uptake) with basic
dye is negligible.
4 Conclusion
The wetting behavior of PVA treated PET fabric
increases considerably due to the good linkage
between PET and PVA. The presence of PVA in the
treated PET fabric after ten washes is confirmed by
spot test. The water contact angle of PVA treated
PET fabric is found to be much less than the intact
and control PET fabrics, which reveals its
hydrophilic character. The presence of PVA and the
hydroxyl groups is also confirmed by SEM and
FTIR studies. DSC traces of PVA attached PET
fabric exhibit a lower melting temperature and
lesser value of heat of fusion compared to intact
PET fabric. PVA treated PET fabric exhibits lesser
basic dye uptake compared to the control fabric due
to lack of carboxylic groups which is also
confirmed by FTIR interpretation.
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