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To cite this article: Rakesh M. Musale & Sanjeev R. Shukla (2016): Weight reduction of
polyester fabric using sodium hydroxide solutions with additives cetyltrimethylammonium
bromide and [BMIM]Cl, The Journal of The Textile Institute
Download by: [Institute of Chemical Technology] Date: 05 April 2016, At: 21:35
The Journal of The Textile Institute, 2016
http://dx.doi.org/10.1080/00405000.2016.1171029
Weight reduction of polyester fabric using sodium hydroxide solutions with additives
cetyltrimethylammonium bromide and [BMIM]Cl
Rakesh M. Musale and Sanjeev R. Shukla*
Department of Fibres and Textile Processing Technology, Institute of Chemical Technology, Mumbai, India
(Received 3 November 2015; accepted 22 March 2016)
Polyethylene terephthalate (PET) fibre is largely used in the textile apparel industry. Treatment of PET fibres by sodium
hydroxide solution is a well-known process giving smooth surface with decrease in the fibre diameter. Hydrolytic
scission of ester linkages of the polyester chains on the fibre surface takes place. Appropriate effects are achieved
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through monitoring of alkali concentration, time and temperature of the process without any significant deterioration of
important fibre characteristics. Addition of various chemicals enhances the hydrolytic action of alkali. PET fabric was
treated with aqueous as well as methanolic solutions of sodium hydroxide in the presence of additives namely, a
quaternary ammonium compound, cetyltrimethylammonium bromide (CTAB) and an ionic liquid, 1-butyl-3-
methylimidazolium chloride ([BMIM]Cl). The process parameters were optimized for desired level of treatment and the
effect evaluated in terms of reduction in fabric weight and SEM images of the samples. Weak methanolic NaOH showed
greater effect than aqueous NaOH solution. Also, the addition of [BMIM]Cl enhanced the effect better than CTAB.
Results of ANOVA analysis showed that temperature played very significant role and time was of less significance for
treatment using [BMIM]Cl. Both the parameters were insignificant for the conventional and CTAB treatments. Thus, the
use of novel eco-friendly additive [BMIM]Cl can cause conservation in terms of time and temperature in this
commercially important process.
Keywords: polyester fabric; weight reduction; sodium hydroxide; ionic liquid; quaternary ammonium salt; SEM
and pilling tendency of the fabric. Treatments under The present paper reports the treatment of PET fabric
relatively drastic conditions involving weight loss of using the novel chemicals, a quaternary ammonium salt
15–25% have been suggested with the objective CTAB and an ionic liquid ([BMIM]Cl) as catalytic
of imparting a silk-like feel. The combined action of additives to the aqueous as well as methanolic NaOH
hydrolysis and aminolysis on PET fibres has been solutions. The results were evaluated in terms of weight
explored by including small quantities of loss of fabric and SEM samples. ANOVA test was
ethylenediamine in aqueous NaOH solution in terms of carried out to observe statistical significance of the
weight loss, tenacity and moisture regain (Shukla & results obtained.
Mathur, 2000). The use of alcoholic solutions of alkali
as well as the use of additives like amine to the aqueous
alkaline bath has been suggested to accelerate the Materials and methods
hydrolytic action of polyester (Shukla, Hedaoo, & Substrate
Saligram, 1995). Surface hydrolysis of PET using lipase Polyester fabric 142 × 47 yarns/cm, twisted ply yarn in
enzymes has also been explored (Kardas, Lipp- warp direction with GSM of 105 g/m2 was used in the
Symonowics, & Sztajnowski, 2001; Kim & Song, 2008) present work. It was cleaned by boiling in a 2 g/L non-
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but the treatment possesses the major drawback of high ionic detergent solution for about 1 h to remove any dirt
cost and limited availability of enzymes for large scale present followed by thorough washing with water and
application (Houde, Kademi, & Leblanc, 2004). drying in an oven at 70 °C.
Collins, Zeronian, and Semmelmeyer (1991) reported
that cetyltrimethylammonium bromide (CTAB)
accelerates the rate of hydrolysis of PET fibres by NaOH Chemicals
solution without affecting its physical properties. The All the chemicals including sodium hydroxide, methanol,
other applications of CTAB include quantification and butyl chloride, 1-methyl imidazole and CTAB were of
extraction procedures of heavy metals (dos Santos et al., laboratory reagent grade procured form S.D. Fine
2007; Venditti, Ceglie, Palazzo, Colafemmina, & Lopez, Chemicals, India.
2007), biotechnological and biomedical applications
(Liu, Li, Tao, Zhu, & Yao, 2007), and improvement of
the analytical sensitivity in spectrophotometric Synthesis of ionic liquid [BMIM]Cl
determinations (Carvalho, Costa, Ferreira, & Teixeira, A 100-ml round bottom flask was charged with
2004). Cetrimonium bromide is a quaternary ammonium 1-methylimidazole (1 mmo1) and butyl chloride
salt used for variety of purposes in cosmetics up to 10% (1.2 mmo1) and refluxed at 120 °C for 12 h under
concentration. It is nontoxic as it has been shown that up nitrogen atmosphere. The progress of reaction was
to 20 mg/kg/day doses in drinking water for one year monitored by TLC. After completion, the reaction
did not have any toxic symptoms on rats. At the higher mixture was cooled to room temperature and excess
dose, the rats began experiencing weight loss (Andersen, buty1 chloride was removed under reduced pressure to
1997). give 1-buty1–3-imidazolium chloride [BMIM]Cl. It is a
Ionic liquids (ILs), also known as molten salts, dark brown viscous liquid stable at higher temperature. It
consist of organic cations and organic/inorganic anions. was stored in a vacuum desiccator (Scheme 1).
These are the class for salts, which are liquid below
100 °C. They are environmental friendly solvents and
catalysts (Kosmulski, Gustafsson, & Rosenholm, 2004). Treatment of PET with aqueous and methanolic NaOH
Because of their adjustable physical and chemical solutions with and without additives
properties, ILs got broad attention of scholars from The treatment solutions were prepared as 10% (w/v)
various fields such as synthesis, catalysis, separation and aqueous NaOH and 5% (w/v) methanolic NaOH. The
electrochemistry (Parvulescu & Hardacre, 2007). concentration of the additives CTAB or [BMIM]Cl was
However, ILs exhibit good hydrophilic properties and 5% on the basis of weight of PET fabric. About .5 g of
surface wetting ability; therefore, they could serve as
antistatic agents for modification of hydrophobic
polymers (Tavanaie, 2013). IL as catalyst is used in the
degradation of PET by various chemical processes (Liu,
Cui, Yu, Li, & Ge, 2009; Palekar, Shah, & Shukla,
2012; Wang, Li, Liu, Zhang, & Zhang, 2009; Yue,
Wang, Zhang, Ni, & Jin, 2011). There is no literature on
weight reduction process of polyester fibres using ionic
liquid as an additive in NaOH solution. Scheme 1. Synthesis of ionic liquid [BMIM]Cl.
The Journal of The Textile Institute 3
Table 1. Effect of 10% aqueous sodium hydroxide on weight loss of polyester fabric by various catalysts.
accurately weighed PET fabric samples were treated with Results and discussion
these solutions in an open beaker dyeing machine with The process of alkaline weight reduction of PET, mainly
agitation, maintaining liquor ratio at 50. The time of in the form of fabric, has gained considerable
treatment was varied in each case along with commercial importance because of a number of
temperature. The treated samples were immediately and advantages associated with the process. Our earlier
thoroughly washed with water for complete removal of studies on PET fibres involved the use of aqueous as
alkali. The final washings were checked with a pH paper well as alcoholic solutions of caustic soda for this
until neutral and the samples were air dried. purpose wherein the degree of weight loss was found to
be much greater for methanolic NaOH (10%) than for
aqueous NaOH at higher concentration (40%) under
Measurement of weight loss identical conditions of time and temperature (Shukla &
The control and treated PET samples were dried in an Mathur, 2000). The addition of an organic amine like
oven at 110 °C for 2 h followed by cooling in P2O5 ethylenediamine in catalytic amount was also shown to
desiccator at room temperature. The dried sample was enhance the action under milder conditions of treatment
weighed accurately. The percentage weight loss of sample (Shukla et al., 1995). There is only one report about
was determined according to the following formula: addition of CTAB to aqueous NaOH solution to enhance
the hydrolysis of PET (Collins et al., 1991).
W1 W2 Depolymerization of PET bottle waste using ionic liquid
Weight loss, % ¼ 100: has been reported in the literature (Palekar et al., 2012;
W2
Wang et al., 2009). The IL acts as solvent as well as
where, W1 and W2 are the weights of control and treated catalyst in this case.
samples, respectively. Table 1 gives the data on the effect of 10% (w/v)
aqueous sodium hydroxide solution with 5% addition of
catalyst CTAB or [BMIM]Cl on the weight loss of the
SEM characterization PET fabric samples. The time and temperature were
The morphology of treated PET fibre samples was enhanced till a weight loss of about 20% was observed
studied with Philips XL 30 Scanning Electron by any of the treatments. It may be observed that under
Microscope (SEM) at 12 kV of acceleration voltage. identical conditions of alkali treatment, the effect of
Before placing the samples in the SEM chamber, the catalysts on weight reduction was much higher than that
samples were mounted onto an aluminium stud and by the conventional method. Thus, at 60 °C and for
sputter-coated with gold/palladium for 180 s (E-1010 30 min treatment time, a weight loss of 2.68% was
ION SPUTTER) to prevent charging. observed for the conventional method as compared to
4 R.M. Musale and S.R. Shukla
Table 2. Effect of 5% methanolic sodium hydroxide on weight loss of polyester fabric by various catalysts.
Figure 1. SEM images of (a) control PET (b) PET fibre treated with aqueous NaOH for 60 min at 60 °C (c) aqueous NaOH with
5% CTAB for 45 min at 60 °C and (d) aqueous NaOH with 5% [BMIM]Cl for 45 min at 60 °C.
6 R.M. Musale and S.R. Shukla
another and by p values to test the null hypothesis Carvalho, L., Costa, A., Ferreira, S., & Teixeira, L. (2004).
against an alternative hypothesis. The F values for the Spectrophotometric determination of chromium in steel
with 4-(2- thiazolylazo)-resorcinol (TAR) using microwave
temperature response were nearly same to Fcrit for the
radiation. Journal of the Brazilian Chemical Society, 15,
conventional treatment, insignificantly higher for CTAB 153–157.
treatment and highly significant in case of [BMIM]Cl Collins, M., Zeronian, S., & Semmelmeyer, M. (1991). The use
treatment indicating that the results on surface of aqueous alkaline hydrolysis to reveal the fine structure
modification of PET fibre using the IL are greatly of poly(ethylene terephthalate) fibers. Journal of Applied
Polymer Science, 42, 2149–2162.
significant. With respect to time, the conventional and
El Messiry, M., El Ouffy, A., & Issa, M. (2015).
CTAB treatment did not have much significance, Microcellulose particles for surface modification to enhance
whereas [BMIM]Cl showed some significance. The p moisture management properties of polyester, and
values for the ionic liquid technique are the lowest as polyester/cotton blend fabrics. Alexandria Engineering
compared to those by conventional and CTAB Journal, 54, 127–140.
Houde, A., Kademi, A., & Leblanc, D. (2004). Lipases and
techniques proving thereby that the ionic liquid as an
their industrial applications: An overview. Applied
additive gives superior results. Biochemistry and Biotechnology, 118, 155–170.
The surface morphology PET fibres after conventional, International rayon and synthetic fibres committee. (2013).
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CTAB and [BMIM]Cl treatment was analysed using Retrieved from http://www.cirfs.org.
scanning electron microscopy (SEM). Figure 1 (a) and (b) Kardas, I., Lipp-Symonowics, B., & Sztajnowski, S. (2001).
The influence of enzymatic treatment on the surface of
show similar effect of little etching on surface of fibres,
modification of PET fibres. Journal of Applied Polymer
whereas Figure 1 (c) of chemical treatment using aqueous Science, 119, 3117–3126.
NaOH with 5% [BMIM]Cl shows increase in roughness or Kim, H., & Song, W. (2008). Optimization of enzymatic
pits on the surface of the fibres. treatment of polyester fabrics by lipase from porcine
pancreas. Fibers and Polymers, 9, 423–430.
Kosmulski, M., Gustafsson, J., & Rosenholm, J. (2004).
Conclusion Thermal stability of low temperature ionic liquids revisited.
Thermochimica Acta, 412, 47–53.
The weight loss of PET fabric in aqueous NaOH is much Liu, F., Cui, X., Yu, S., Li, Z., & Ge, X. (2009). Hydrolysis
less as compared to methanolic NaOH due to higher reaction of poly(ethylene terephthalate) using ionic liquids
polarity of the former solution. Less polar solutions of as solvent and catalyst. Journal of Applied Polymer
alkali are more effective in hydrolysing polyester fibres Science, 114, 3261–3565.
topochemically. [BMIM]Cl is more effective in both Liu, Q., Li, J., Tao, W., Zhu, Y., & Yao, S. (2007).
Comparative study on the interaction of DNA with three
solutions than CTAB. Addition of [BMIM]Cl increases different kinds of surfactants and the formation of
the weight loss in methanolic sodium hydroxide than in multilayer films. Bioelectrochemistry, 70, 301–307.
aqueous sodium hydroxide solution. The addition also Palekar, V. S., Shah, R. V., & Shukla, S. R. (2012). Ionic liquid-
allows decrease in the concentration of NaOH, catalyzed aminolysis of poly(ethylene terephthalate) waste.
temperature and time for reaction for similar weight loss Journal of Applied Polymer Science, 126, 1174–1181.
Parvulescu, V., & Hardacre, C. (2007). Catalysis in ionic
of fabric. Further, [BMIM]Cl can be recovered, whereas liquid. Chemical Review, 107, 2615–2665.
CTAB cannot. This makes the process efficient, at the Prorokova, N. P., Vavilova, S. Y., & Prorokov, V. N. (2007).
same time being eco-friendly. Effect of ammonium salts on poly(ethylene terephthalate)
materials. Fibre Chemistry, 39, 20–25.
dos Santos, D., Teixeira, A., Barbosa, J., Ferreira, S., Korn, M.,
Disclosure statement & Teixeira, L. (2007). Use of cetyltrimethylammonium
bromide as surfactant for the determination of copper and
No potential conflict of interest was reported by the authors. chromium in gasoline emulsions by electrothermal atomic
absorption spectrometry. Spectrochimica Acta Part B:
Atomic Spectroscopy, 62, 1072–1077.
ORCID Sarkar, M., Jintu Fan, J., Szeto, Y., & Xiaoming Tao, X.
Sanjeev R. Shukla http://orcid.org/0000-0002-0966-9443 (2009). Biomimetics of plant structure in textile fabrics for
the improvement of water transport properties. Textile
Research Journal, 79, 657–668.
Shukla, S. R., Hedaoo, V. B., & Saligram, A. N. (1995). Alkaline
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