Journal of Cleaner Production 108 (2015) 494e502

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Journal of Cleaner Production

journal homepage: www.elsevier.com/locate/jclepro

Sustainable and economical one-step desizing, scouring and bleaching

method for industrial scale pretreatment of woven fabrics
Muhammad Awais Imran a, *, Tanveer Hussain b, Muhammad Hanif Memon a,
Muhammad Moosa Abdul Rehman a
a
Department of Textile Science, Faculty of Engineering, Science and Technology, Indus University Karachi, Pakistan
b
Faculty of Engineering and Technology, National Textile University, Faisalabad 37610, Pakistan

a r t i c l e i n f o a b s t r a c t

Article history: Combining more than one processes in one-step is an effective approach for economical, ecological and
Received 6 January 2015 efficient processing of textiles. The most commonly used alpha-amylase enzyme, suitable for desizing
Received in revised form woven fabrics, is not compatible for combined desizing-scouring-bleaching process in one step due to
14 August 2015
lack of stability under high temperature and alkaline condition in the combined process. The aim of this
Accepted 16 August 2015
Available online 29 August 2015
study was to use a novel, non-enzymatic desizer, which is stable under high alkalinity and temperature
condition in the combined process. The lab trials showed the effectiveness of non-enzymatic desizer for
one-step pretreatment of polyester/cotton blended fabrics. After successful lab trials, the proposed one-
Keywords:
Sustainable
step process for combined desizing-scouring-bleaching on polyester/cotton blended fabrics was opti-
Economical mized for industrial-scale application. The concentration parameters for hydrogen peroxide, sodium
Combined pretreatment hydroxide and the desizer were optimized with the help of central composite experimental design (CCD)
Woven fabric of response surface methodology. The results obtained in one-step pretreatment method, in terms of the
Novel desizer physical properties of the treated fabrics, were comparable with the results obtained by separate
Response surface methodology desizing, scouring and bleaching processes carried out on the identical fabric. However, the proposed
one-step pretreatment process is much more advantageous with respect to saving in chemicals, water
and energy as well as reduction in the process time.
© 2015 Elsevier Ltd. All rights reserved.

1. Introduction processes. The fabric is cleaned, made absorbent and relatively

whitened through desizing, scouring and bleaching processes
Cotton and its blended fabrics contain some inherent impurities during the pretreatment (Shore, 1998; Ibrahim et al., 2004; Shamey
such as oil, fat, wax and pectin within the fiber structure. The and Hussein, 2005). Each individual pretreatment process sepa-
composition of these impurities depends on the fiber blend, rately consumes water, steam, electricity and chemicals, causing
maturity of cotton fiber, weathering and agriculture conditions etc. chemical oxygen demand (COD) and biological oxygen demand
(Carr, 1995; Brushwood, 2003). The yellowness of cotton fiber is (BOD) loads in the washing effluent (Shafie et al., 2009; Hardin,
due to the presence of protoplasm residue of protein and flavones 2010). In addition, separate time spans are required for each pro-
pigments (Brushwood, 2003). The sizing chemicals (starch, poly- cess, lowering the machine productivity. A one-step combined
vinyl alcohol etc.) are usually applied on warp yarns to avoid pretreatment process cannot only reduce the load of COD and BOD
breakages during weaving process. During fabric formation, woven but also make it suitable for cleaner textile processing by reducing
fabric also acquires some contaminations from machine oil and the consumption of water and effluent discharge and savings in
grease and as a consequence all these impurities create hydro- energy. Combining pretreatment processes has remained an
phobic characteristics in the fabric. Therefore, the pretreatment important research area for cleaner, sustainable and economical
processes for cotton and its blended fabrics are essential to make textile processing. Several studies were made in this regard in the
the textile substrate suitable for subsequent coloration or finishing recent past using novel and biological desizing-scouring-bleaching
€
procedures. Oner and Sahinbaskan (2011) have introduced REST
concept (Rapid enzymatic single bath treatment) which is envi-
* Corresponding author. Tel.: þ92 3232675392. ronmentally friendly and saves enormous amount of water and
E-mail address: [email protected] (M.A. Imran). energy. Although, in this treatment no fresh water was added till

http://dx.doi.org/10.1016/j.jclepro.2015.08.073
0959-6526/© 2015 Elsevier Ltd. All rights reserved.
 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502 495

the end of complete pretreatment and dyeing processes but this The proposed desizer, Auxidesize GLAX, is based on alkylated
treatment is based on separate processes (desizing, scouring and carbonyl butyrate anhydride triglycerides (ACBAT). It converts an
bleaching) with desired enzymes and chemicals which makes it insoluble starch into glucose, which is water soluble, through hy-
somewhat lengthy pretreatment procedure. In some studies, the drolysis mechanism. Its structure can be represented as follows;
cotton fabric was enzymatically desized, scoured and bleached

with an enzyme mixture of starch-degrading enzymes, pectinases R  CH3 ðCH2 Þn CO n O  R
and glucose oxidases (GOx) respectively (Tzanov et al., 2001;
The action mechanism of ACBAT can be seen in Scheme 1, where
Buschle-Diller et al., 2001; Ali et al., 2011; Saravanan et al., 2012).
(C6H10O5)n is the water-insoluble starch, H2O is the aqueous me-
This integrated method is environmentally friendly and offers
dium and C6H12O6 is the water-soluble glucose.
savings for the pretreatment process (Aly et al., 2004), but this is
The one-step desizing-scouring-bleaching process on woven
not practiced because of high cost of GOx enzymes purified by
fabric was optimized using response surface methodology. The
Aspergillus niger (Ali et al., 2014). In another study, the in situ
response surface methodology (RSM) is a combination of mathe-
formation of peracetic acid (PAA), from reaction of tetraacetyle-
matical and statistical techniques used for modeling and analysis of
thylenediamine (TAED) with sodium perborate, was utilized to
problems in which a response of interest is influenced by several
affect simultaneous desizing and bleaching whereas cellulase,
variables and the objective is to optimize this response (Hill and
pectinase and their mixture were used to affect bio-scouring
Hunter, 1966). RSM has been successfully applied in past for
(Huang et al., 2007; Hebeish et al., 2009; Shafie et al., 2009; Shao
several modeling and optimization problems (Montgomery, 2008),
et al., 2010; Li and Hinks, 2012). Many European textile mills are
including the study of decolourization of the azo reactive black 5
using PAA bleaching method (Scarborough and Mathews, 2000).
(RB-5) dye using purified laccase from a white rot fungus Pleurotus
However, the insolubility of TAED is still a problem for industrial
sajor-caju (Murugesan et al., 2007).
pretreatment process thus it has limited use for bleaching of tex-
tiles (Abdel-Halim and Al-Deyab, 2013). The use of ozone-oxygen
gas in combined desizing-scouring-bleaching process of cotton 2. Experimental
has also been suggested with acceptable pretreatment results
(Prabaharan and Rao, 2003). This approach eradicates harsh 2.1. Materials
chemicals, uses less thermal energy and less amount of water for
combined pretreatment process but the inferior whiteness result In this work, polyester/cotton (blend ratio 50:50) blended fabric
and expensive ozone generation process make it impractical at was used, with both warp and weft yarns linear densities Ne 30/1,
industrial level, hence this approach does not attract industrial ends per inch 76, picks per inch 66 and areal density 118 g/m2. The
application. In short, the challenge of a one-step combined pre- warp yarns of the fabric were sized using maize starch 10%, poly-
treatment method for woven fabric at industrial scale is yet to be acrylic 1.5% and softener 0.5% with a total add-on of 12%. A novel
addressed. desizing agent Auxidesize GLAX, based on alkylated carbonyl bu-
The conventional industrial desizing, scouring and bleaching tyrates anhydride triglyceride fluid (ACBAT) was obtained from
processes are completed separately based on enzymatic desizing Rakuto Kasei Industrial Co. Japan. A non-ionic wetting agent,
(Csiszar et al., 1998) alkaline scouring and hydrogen peroxide Auxipal RGN, based on fatty-alcohol Ethoxylate (85% active con-
bleaching methods (Karmakar, 1999; Clark, 2011). Though the tent), and bleaching stabilizer, Biostab AFK, based on modified 2-
conventional method requires separate pretreatment procedures, hydroxy-3-carboxy-6-oxo-7-methylocta-2,4-dieonic, were pro-
the chemicals used are economical making them attractive for large vided by Auxicolors, Pakistan. Industrial grade sodium hydroxide
industrial-scale pretreatment work, using discontinuous or (49.5 Baume) was provided by Sitara Chemicals, Pakistan and
continuous methods of pretreatment (Cardamone and Marmer, hydrogen peroxide bleaching agent (49.5% w/w) was provided by
1995; Rao, 2001). Descon Chemicals, Pakistan. A non-ionic emulsifier, Imerol X, based
In general, desizing is mainly accomplished using eco-friendly on nonyl phenol polyglycol ether was obtained from Archroma,
alpha-amylase enzymes in neutral to acidic pH range (Cavaco- Pakistan. All the chemicals were of industrial/commercial grade
Paulo and Gübitz, 2003; Araújo et al., 2008). Scouring is mostly and all the experiments were performed in a textile processing
done in highly alkaline media using sodium hydroxide and unit, Arabian Textile Mills, Karachi. The mill's process water used in
bleaching is also carried out in alkaline pH range (10.5e11) using this study had total dissolved solids (TDS) and total hardness values
hydrogen peroxide (Trotman, 1984). The task of combining the of 120 ppm and 15 ppm respectively.
above three processes is not possible to be accomplished since
enzymes are quite sensitive to pH and temperature and cannot 2.2. Method
function at high pH and temperature condition (Nierstrasz and
Cavaco-Paulo, 2010). Therefore, it has not been possible to Several lab trials were conducted to assess the effectiveness and
combine enzymatic desizing with alkaline scouring and hydrogen compatibility of the novel desizer, ACBAT, for use in one-step
peroxide bleaching. However, combination of scouring and desizing-scouring-bleaching process. The details of recipe and
bleaching produces acceptable results (Gulrajani et al., 1987). The process conditions are given in supplementary document.
acceptable degree of desizing along with good absorbency and In the present study, response surface methodology (RSM) was
whiteness has remained a challenge in a one-step process. The used to investigate the effect of simultaneous variation in the three
attempt to use oxidative desizing process based on sodium per- key ingredients of the one-step desizing/scouring/bleaching recipe,
sulfate combined with scouring and bleaching was made but it i.e. concentration of alkylated carbonyl butyrates anhydride tri-
leads to a high risk of loss in fabric strength due to oxidative glyceride fluid (ACBAT), concentration of sodium hydroxide (NaOH)
damage of cellulose (Baldwinson, 1990; Iqbal et al., 2007; Wasif and and concentration of hydrogen peroxide (H2O2). This methodology
Indi, 2010).
The present study was carried out to attempt one-step desizing-
scouring-bleaching process for woven fabric. In this study a novel
non-enzymatic desizer was investigated for its compatibility with
conditions used in conventional scouring and bleaching processes. Scheme 1.
496 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502

is used for accurate modeling of the effect of input process variables Table 2
on the output variables and also for identifying and describing the RSM central composite experiment design.

effect of any interactions among the independent variables on the No. X1, (H2O2), g/l X2, (NaOH), g/l X3, (ACBAT), g/l
responses. Furthermore, RSM also enables the estimation of the 1 1 1 1
optimum levels of the independent variables with high degree of 2 1 1 1
accuracy. The RSM factors and levels used in this study are given in 3 1 1 1
Table 1. The complete RSM central composite design (CCD) of 4 1 1 1
5 1 1 1
experiment is given in Table 2. The first 8 experiments in Table 2
6 1 1 1
comprise 2-level factorial points, the next 6 experiments 7 1 1 1
comprise axial points and the last 6 experiments comprise repli- 8 1 1 1
cates at the centre points. All the process variables other than the 9 2 0 0
10 2 0 0
hydrogen peroxide, sodium hydroxide and ACBAT were kept same
11 0 2 0
for all the 20 experiments: wetting agent 1 g/L, emulsifier 2 g/L, 12 0 2 0
stabilizer 2 g/L, fabric to liquor ratio 1:40, process temperature 13 0 0 2
95  C and process time 60 min. All the experiments were conducted 14 0 0 2
on lab-scale batch-processing equipment. After the treatment 15 0 0 0
16 0 0 0
process, the fabric samples were subjected to hot rinsing at 60  C
17 0 0 0
for 5 min, and then neutralization with acetic acid followed by cold 18 0 0 0
rinsing and drying in ambient conditions. 19 0 0 0
20 0 0 0

2.3. Measurements
WI ¼ Y þ 800ð0:3138  xÞ þ 1700ð0:3310  yÞ (1)
In order to measure the degree of desizing, 4  4 cm speci-
mens from each treated sample were put into an iodine solution
Where, Y, x, y are chromaticity coordinates of the treated fabric.
(0.005 mol/l) for one minute, rinsed with cold water for 2e3 s
Tensile strength of the treated samples was determined ac-
and then dabbed off with a starch-free filter paper and compared
cording to ASTM Test Method D5034 using Instron type tensile
immediately with the TEGEWA-scale for giving a TEGEWA rating.
testing machine. The design of experiments and the analysis of
TEGEWA scale consists of colors ranging from violet to white,
results were done using Design-Expert 7.0 statistical software.
with gradually decreasing depth of violet on a scale of 1e9.
TEGEWA was established in 1951 in Wiesbaden as an association
of the manufacturers of chemicals, the name being an amalgam 3. Results and discussion
of the following key activities: TExtilhilfsmittel” (textile auxil-
iaries), “GErbstoffe” (tanning agents) and “WAschrohstoffe” The experimental results are given in Table 3, which will be
discussed in the following sections.
(detergent raw materials). The association developed a scale for
determining the degree of desizing of textile fabrics using iodine
solution. 1e2 drops of iodine solution are dropped on the 3.1. TEGEWA rating
desized fabric. The color of the fabric at the spotted area is
assessed visually with TEGEWA scale. A deep violet color in the TEGEWA rating is a reflection of the degree of desizing of the
fabric at the place of iodine solution-drop indicates the signifi- fabric, which is represented on scale 1e9. A higher TEGEWA rating
cant presence of starch and extremely poor desizing, and a rating indicates better removal of the starch sizing agent from the fabric.
of 1 on the TEGEWA scale. Extremely light or no color on the The mark 9 on the scale represents complete starch removal,
fabric at the place of iodine solution-drop indicates no presence whereas mark 1 on the scale indicates completely inadequate
of starch and excellent desizing with a TEGEWA rating of 9. In- starch removal. The sizing agent comprising starch is applied on the
termediate ratings between 1 and 9 represent increasing degree warp yarns before fabric weaving in order to strengthen the yarns
of desizing. to withstand stresses and frictional forces during weaving without
The absorbency of each sample was determined according to undergoing breakages, leading to frequent loom stoppages and
DIN 53924 capillary rise test method. Strips of 3  25 cm were disruption of fabric production. After weaving, starch size must be
taken out and hung in water colorized with Patent Blue dye. About removed to allow better penetration of dye or other finishes onto
0.5 cm of the bottom of the strips was immersed in the liquid. The the fabric. In this study, ACBAT was primarily used as a desizing
capillary rise of water in 5 min was determined in cm. agent. Unlike commonly used enzymatic desizing agents, ACBAT is
The CIE Whiteness Index (WI) values for each sample were stable under sodium hydroxide alkaline condition along with
determined using Datacolor Spectraflash SF 600þ spectropho- hydrogen peroxide. Its effect on TEGEWA rating is depicted in Fig. 1,
tometer (Datacolor International) with the following settings: where it is evident that an increase in the concentration of ACBAT
illuminant D65, large area view, specular excluded, UV included results in significant improvement in the TEGEWA rating. The in-
and CIE 1964 Supplemental Standard Observer (10 observer). crease in TEGEWA rating is quite sharp when concentration in-
According to AATCC Test Method 110-2005, WI is given by Eq. (1). creases from 1 g/l to 3 g/l, followed by a steady state and then no
improvement is observed with further increase in the
Table 1 concentration.
RSM experimental factors and their levels. Fig. 2 shows that when at concentration 3 g/l of ACBAT was used
there was no significant effect of sodium hydroxide and hydrogen
No Factors Code Units Factors level
peroxide over the range 1.5e4.5 g/l on TEGEWA rating. This fact was
2 1 0 þ1 þ2
established on the basis of analysis of variance (ANOVA).
1 H2O2 X1 g/L 1 2 3 4 5 The response surface quadratic model for TEGEWA rating is
2 NaOH X2 g/L 1 2 3 4 5 given in eq. (2), which is based on the actual levels of variables,
3 ACBAT X3 g/L 1 2 3 4 5
where X1, X2 and X3 are concentrations of H2O2 (g/l), NaOH (g/l) and
 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502 497

Table 3
Central composite design experiment results.

No. Factors Responses

H2O2, g/l NaOH, g/l ACBAT, g/l TEGEWA rating Absorbency, cm CIE whiteness Warp tensile Strength, N Weft tensile Strength, N

1 2 2 2 6.5 5 65.6 476 359

2 4 2 2 6.5 5 69.1 470 332
3 2 4 2 6.5 5 66.1 475 358
4 4 4 2 6.5 6 70.1 476 336
5 2 2 4 8.0 5 66.8 473 360
6 4 2 4 8.0 5 71.0 483 347
7 2 4 4 8.0 6 67.6 479 351
8 4 4 4 8.0 6 70.4 476 367
9 1 3 3 8.0 6 66.3 477 376
10 5 3 3 8.0 6 69.6 481 369
11 3 1 3 8.0 6 60.0 476 359
12 3 5 3 8.0 6 66.5 477 351
13 3 3 1 5.5 6 68.6 474 355
14 3 3 5 8.0 6 68.0 479 360
15 3 3 3 8.0 6 66.2 476 370
16 3 3 3 8.0 6 66.4 479 342
17 3 3 3 8.0 6 66.0 477 356
18 3 3 3 8.0 6 66.1 476 344
19 3 3 3 8.0 6 66.4 477 350
20 3 3 3 8.0 6 66.8 478 360

ACBAT (g/l), respectively. The equation excludes the interaction

terms because their coefficients were found to be zero. The
regression coefficients of the quadratic expressions were obtained
in accordance with the least square method explained by Mont-
gomery in detail (Montgomery, 2005). In least square method,
values of the regression coefficients are chosen so that sums of
squares of the errors are minimized. In matrix terms, the vector of
coefficients in multiple regression is calculated by the formula:
b ¼ (X′X)1 (X′Y), where X is the design matrix, including the
constant; Y is the response vector; and b is the estimate of the
population regression coefficients b. General form of the second
order response surface regression equation with two factors can be
written as follows: Y ¼ b0 þ b1 x1 þ b2 x2 þ b11 x21 þ b22 x22 þ
b12 x1 x2 þ ε; where b is the regression coefficient and ε is the
estimated error.
The R-sq of Eq. (2) was found to be 0.92, indicating that 92%
change in TEGEWA rating could be explained by the terms included
in the model. The higher value of the coefficient (2.85568) of ACBAT
Fig. 1. Effect of ACBAT and NaOH concentration on Tegewa rating (at H2O2 3 g/l).
(X3) indicates its major role in improving the TEGEWA rating. Eq.
(2) does not contain any coefficients for X1X2, X1X3, X2X3, because
these terms were not found to have statistically significant effect on
TEGEWA rating, according to the analysis of variance (ANOVA).

TEGEWA rating ¼ 1:75795 þ 0:29318X1 þ 0:29318X2

þ 2:855568X3  0:048864X21  0:048864X22
 0:36136X23
(2)

Where, X1, X2 and X3 are concentrations of H2O2 (g/l), NaOH (g/l)

and ACBAT (g/l), respectively.

3.2. Fabric absorbency

Native cotton contains different impurities including oily, fatty

and waxy components which hinder the absorption of water itself
or that containing dyes or finishes. The starch added during warp
sizing further deteriorates the fabric absorbency. It can be observed
from Fig. 3 that the best possible fabric absorbency is obtained
when both desizer and scouring agent were used at their maximum
concentration, which is 5 g/l for both ACBAT and sodium hydroxide,
Fig. 2. Effect of NaOH and H2O2 concentration on Tegewa rating (at ACBAT 3 g/l). where these worked at their best. This is because on one hand,
498 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502

Where, X1, X2 and X3 are concentrations of H2O2 (g/l), NaOH (g/l)

and ACBAT (g/l), respectively.
The R-sq value of Eq. (3) was found to be 0.34, which is rather
low. The coefficient of determination (R-sq) represents the per-
centage of response variable variation that is explained by the
predictor variables included in the regression equation. The higher
the R-sq, the better the regression equation fits a given data. The
value of R-sq may range between 0 and 100%. If R-sq is 100, then all
the variance in the response could be explained by the predictor
terms of the regression equation, and results predicted by the
regression equation would always be equal to the experimental
results, which if usually rare because there are always some errors
associated with experimentation due to noise variables. A low
value of R-sq (0.34) for Eq (3) implies that only 34% of variation in
the fabric absorbency can be explained by the predictor terms
included in Eq (3), viz. concentration of H2O2 (g/l), NaOH (g/l) and
ACBAT (g/l). Other factors that are not included in the Eq (3) but
may have effect on fabric absorbency, may include the wetting
agent and the emulsifier used in the treatment recipe. While wet-
Fig. 3. Effect of ACBAT and NaOH concentration on fabric absorbency (at H2O2 3 g/l). ting agent improves the fabric wettability by lowering water/fabric
interfacial surface tension, emulsifier helps in the removal of oil, fat
ACBAT results in the better removal of starch through its hydrolysis and wax impurities through emulsification. In the presence of an
and on the other hand sodium hydroxide results in better removal effective emulsifier, the role of sodium hydroxide was not found to
of the saponifiable oils, fats and waxes present in cotton. The be very significant in improving the fabric absorbency. Since, a fixed
removal of these impurities from the fabric results in better fabric amount of emulsifier and wetting agent was used in all the recipes;
absorbency. Fig. 4 indicates that the fabric absorbency is at opti- these factors could not be included in the quadratic model.
mum when the concentration of hydrogen peroxide is also higher Although the role of sodium hydroxide in improving the fabric
in combination with the concentration of sodium hydroxide. The absorbency was rather limited in the presence a good emulsifier,
removal of motes and other non-cellulosic contents, with the help the addition of sodium hydroxide is necessary to provide alkaline
of both sodium hydroxide and hydrogen peroxide also contribute pH in order to activate the bleaching action of hydrogen peroxide,
towards the improvement in fabric absorbency. Hydrogen peroxide as discussed in the next section.
also contributes in the starch removal. However, as noticed in the
previous section, its role is rather limited in the presence of ACBAT
3.3. Fabric whiteness
which takes precedence in the removal of starch.
The response surface quadratic model for fabric absorbency is
In addition to good degree of desizing and absorbency, fabric
given in Eq. (3).
whiteness is the third desirable objective of fabric pre-treatment
for finishing the fabric as white or before its dyeing, particularly
Fabric absorbency ¼ 3:89886 þ 0:56705X1  0:057955X2 in light and bright shades. It is clear from Figs. 5 and 6 that ACBAT
þ 0:56705X3 þ 0:125X1 X2  0:125X1 X3 does not significantly contribute in increasing fabric whiteness,
which is influenced more by the concentration of hydrogen
þ 0:125X2 X3  0:084091X21  0:084091X22 peroxide and sodium hydroxide. Hydrogen peroxide is the main
 0:084091X23 bleaching agent and increase in its concentration more evidently
results in increase in fabric whiteness. Sodium hydroxide acts as
(3)
bleaching activator and thus indirectly contributes to increase in

Fig. 4. Effect of NaOH and H2O2 concentration on fabric absorbency (at ACBAT 3 g/l). Fig. 5. Effect of ACBAT and NaOH concentration on fabric whiteness (at H2O2 3 g/l).
 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502 499

Fig. 8. Effect of NaOH and H2O2 concentration on fabric strength (at ACBAT 2 g/l).

Fig. 6. Effect of NaOH and H2O2 concentration on fabric whiteness (at ACBAT 3 g/l).

during desizing, scouring and bleaching. Tensile strength is one of

fabric whiteness (Zeronian and Inglesby, 1995). The addition of the most important indicators of degradation of mechanical prop-
sodium hydroxide enhances the formation of perhydoxyl ions erties of the fabric during pre-treatment. It is clear from Figs. 7 and
(OH-2) which actually acts as nucleophile bleaching agent. 8 that ACBAT does not cause any appreciable loss in fabric strength
during the treatment. This is because the action of ACBAT is
H2 O2 þ OH /H2 O þ OH2  confined only to the starch present in the fabric, without any
The response surface quadratic model for fabric whiteness is deleterious effect on the cotton cellulose or the polyester fibers in
given in eq. (4). the fabric. However, increase in hydrogen peroxide concentration
results in decrease in fabric strength in the presence of higher
Fabric whiteness ¼ 62:6167  1:80682X1 þ 5:19193X2 amount of sodium hydroxide (Badaras et al., 1993; Vigo, 1994).
Fabric tensile strength is highest when the concentrations of both
 3:23682X3  0:115X1 X2  0:065X1 X3
the hydrogen peroxide and sodium hydroxide are low. The loss of
 0:185X2 X3 þ 0:60989X21  0:56386X22 tensile strength at higher hydrogen peroxide and sodium hydroxide
concentrations may be attributed to the removal of non-cellulosic
þ 0:70489X23
component from the fabric as well as some oxidative damage to
(4) cellulose. When the rate of decomposition of hydrogen peroxide in
the presence of sodium hydroxide is greater than that of its con-
Where, X1, X2 and X3 are concentrations of H2O2 (g/l), NaOH (g/l) sumption in the bleaching action, the excess formation of perhy-
and ACBAT (g/l), respectively. droxyl ions can lead to formation of oxycellulose, which is lower in
R-sq value for eq. (4) was found to be 0.72, which is better as strength than the native cellulose (Prabaharan and Almeida, 2004).
compared to that of fabric absorbency but poor as compared to that Too high alkalinity at low hydrogen peroxide concentration leads to
of TEGEWA rating. decreasing trend in fabric tensile strength due to too quick
decomposition of hydrogen peroxide, which may have caused some
3.4. Fabric strength cellulosic damage. The response surface quadratic model for fabric
weft strength is given in eq. (5).
One of the key considerations during fabric pre-treatment is to The R-sq value of eq. (5) was found to be 0.52. A lower value of R-
preserve the fabric mechanical properties as much as possible sq may be attributed to another factor affecting the fabric strength
after the pre-treatment, i.e. fabric shrinkage and change in warp
and weft density. During the aqueous pre-treatment, fabric shrinks
because of the relaxation and release of yarn tensions incorporated
during the spinning and weavings processes. Due to fabric
shrinkage the number of yarns per unit area increases, resulting in
increase in fabric density and the fabric strength.

Tensile strength ¼ 471:13295  53:73182X1  7:78182X2

 15:00682X3  4:175X1 X2 þ 6:5X1 X3
þ 1:1X2 X3 þ 2:97614X21  1:34886X22
 0:78636X23
(5)

Where, X1, X2 and X3 are concentrations of H2O2 (g/l), NaOH (g/l)

and ACBAT (g/l), respectively.
It is observed from the above results and discussion that ACBAT
Fig. 7. Effect of ACBAT and NaOH concentration on Fabric strength (at H2O2 3 g/l). worked as an efficient desizing agent and hydrogen peroxide as an
500 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502

Table 4
Search parameters used in response optimization.  1=ðI1 þI2 þ…þIn Þ
D ¼ dI11 *dI22 *…*dInn (8)
TEGEWA Absorbency CIE whiteness Tensile strength,
(cm) weft (N)
Where di is the desirability of individual response i, and Ii is the
Target Minimum Target Minimum Target Minimum Target Minimum
importance of the response i. For the optimization of one-step pre-
8 7 6 5 71 70 375 350
treatment, models for all the four response variables (i.e. TEGEWA,
absorbency, whiteness and tensile strength) were combined into
efficient bleaching agent, denoted by their good R-sq values. single multi-response optimization. Search parameters of the
However the role of sodium hydroxide as scouring agent to increase multiple response optimization approach described above are
fabric absorbency, having an R-sq value of 0.34, was not found summarized in Table 4. These parameters were selected so as to
sufficient therefore wetting agent and emulsifying agent were also meet most of the end-use requirements of the pre-treated woven
used in combination. fabric.
The optimum process conditions determined by the multiple
response optimization were found to be as follow: Hydrogen
peroxide 5 g/l, Sodium hydroxide 3.75 g/l and ACBAT 3.6 g/l. The
results of the optimized recipe were validated and compared with
3.5. Recipe optimization and bulk trials the traditional three-step pre-treatment process. Table 5 gives a
comparison of the recipes and the results of the optimized one-step
In the present study, a multiple response optimization tech- process and the traditional three-step process that was already
nique proposed by Derringer and Suich was used to maximize being used in the textile processing unit, where all the experi-
TEGEWA rating, fabric absorbency, whiteness and tensile strength. mental work was carried out. It is clear from the results that an
It is established from response surface methodology and helps to optimum combination of relative amounts of chemicals used in
use of desirability functions (Derringer, 1980). By using this tech- one-step method gives comparable results to those obtained in
nique, each response variable was expressed in terms of an indi- three-step method.
vidual desirability function di, which could take its value between The one-step recipe optimized at the lab scale was then tried at
0 and 1. When the response variable was at its target or goal, di bulk scale on jig machine with a fabric batch of 3000 m. The bulk-
would become 1, and if the response variable was outside the scale results, as given in Table 6, show lower TEGEWA rating, fabric
acceptance range, di would become zero. In general the objective absorbency and whiteness as compared to the lab results. However,
was to set the process variables to such levels that the overall the results were still acceptable for those cases when the fabric was
desirability function (D) was maximized. By assigning a weight (r) not to be finished white and was to be dyed or printed in medium
to a response variable, relative importance of being close to the to dark shades. Lower results at the bulk scale could be attributed to
target could also be assigned. Selecting r > 1 placed greater shorter liquor to fabric ratio (0.5:1) at the jig machine as compared
importance on being close to the target value, while choosing to that in the lab machine (40:1). Higher liquor to fabric ratio (L:R)
0 < r < 1 made the target less important. The individual desirability in the lab scale trials results in better removal of impurities as
was calculated using the eq. (6) (Derringer, 1980). compared to lower L:R in the jig machine. At bulk scales, shorter
liquor ratios are often preferred to reduce total consumption of
di ¼ fi ðyÞWi (6) water, chemicals and energy required for heating up the liquor.
Nevertheless, in bulk trials of both one-step process and three-
Where Wi is the weight for response and the function fi(y) depends step process, the amounts of chemicals used in one-step process
on whether one desires to hit a target, minimize the response, or were lower than in three-step process. The amounts of hydrogen
maximize the response. To maximize the response, fi(y) was peroxide, emulsifier, wetting agent, sodium hydroxide and acetic
calculated using eq. (7). acid were 38%, 60%, 60%, 46% and 33% lower respectively, in one-
step process as compared to the three-step process.
8 A comparison has been made for the chemical cost, water and
> 0 y<L
>
>  energy consumption and the process time involved in the con-
< yL
fi ðyÞ ¼ LyT (7) ventional three-step and the present one-step process, for which
>
> T L the results are given in Table 7. It can be seen in Table 6, significant
>
:
1 y>T savings in chemical cost (39%), water (60%), electricity (52%), steam
(54%) and the involved process time (52%) were observed for one-
Where y is the response value, and U and L are the upper and lower step process compare to three-step process. For example, as shown
boundaries (i.e. minimum and maximum acceptable values for the in Table 7, total chemical cost in three-step process was 1770
response), respectively, and T is the target. The composite desir- Pakistan Rupees (PKR), and that in one-step process was 1080 PKR,
ability was calculated according to Eq. (8): which is 39% lower as compared to the three-step process. This

Table 5
Results of validation experiments at lab-scale in three-step and one-step processes.

Total chemicals used, g/l Lab scale results

Chemicals Three-step process One-step process Parameters Three-step process One-step process

Wetting agent 1 1 TEGEWA rating 7 8

Emulsifier 3 2 Absorbency, cm 6 6
ACBAT 3 3.6 CIE Whiteness 76 77
Sodium hydroxide 5 3.75 Warp tensile strength, N 471.5 495.6
Hydrogen peroxide 6 5 Weft tensile strength, N 345.11 355.52
Stabilizer 2 2
 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502 501

Table 6
Results of validation experiment at bulk-scale in three-step and one-step processes for a 3000 m batch.

Total chemicals used, g/l Bulk scale results

Chemicals Three-step process One-step process Parameters Three-step process One-step process

Wetting agent 2.5 1 TEGEWA rating 5 5

Emulsifier 5 2 Absorbency, cm 4 4
ACBAT 3.5 3.6 CIE Whiteness 70.55 66
Sodium hydroxide 7 3.75 Warp tensile strength, N 458.3 477
Hydrogen peroxide 8 5 Weft tensile strength, N 355 372.5
Stabilizer 2 2

Table 7
Comparison of chemical cost, water and energy consumption between three-step and one-step processes for a 3000 m batch.

Conventional three-step process

Step 1 2 3
Process Desizing Washing Scouring Washing Bleaching Washing Neutralization Total
Chemical Cost, Rs. 330 0 600 210 420 0 210 1770
Water, L 450 1000 450 1000 450 1000 500 4850
Electricity, kW/hr 20 15 10 10 30 15 5 105
Steam, Kg 210 210 210 105 420 210 0 1365
Time, min. 100 75 50 50 150 75 25 525
Presented one-step process
Step 1
Process One-step treatment Washing Neutralization Total
Chemical Cost, Rs. 870 0 210 1080
Water, L 450 1000 500 1950
Electricity, kW/hr 30 15 5 50
Steam, Kg 420 210 0 630
Time, min. 150 75 25 250

Chemical Cost (PKR/kg): Wetting agent, 180; Emulsifier, 178; Stabilizer, 60; ACBAT, 200; H2O2, 50.5, NaOH, 80; Acetic Acid, 105.

remarkable reduction not only makes the present process highly Ali, S., Khatri, Z., Khatri, A., Tanwari, A., 2014. Integrated desizinge-
bleachingereactive dyeing process for cotton towel using glucose oxidase
advantageous for routine pretreatment in the textile industry but
enzyme. J. Clean. Prod. 66, 562e567.
also contributes to the present sustainable development efforts in Aly, S., Moustafa, B., Hebeish, A., 2004. Bio-technological treatment of cellulosic
the textile industry (Tobler-Rohr, 2011). Based on present study, the textiles. J. Clean. Prod. 12 (7), 697e705.
processing unit, where the bulk trials were conducted, has modi- Araújo, R., Casal, M., Cavaco-Paulo, A., 2008. Application of enzymes for textile fi-
bres processing. Biocatal. Biotransform 26 (5), 332e349.
fied their pretreatment process to one-step process from the con- Badaras, G.W., Madaras, G.W., Shore, J., Parish, G.J., 1993. Technology of fabric
ventional three-step process, which was traditionally used. preparation. In: Batchwise Dyeing of Woven Cellulose Fabrics, first ed. Society
of Dyers and Colourists, Bradford, England, pp. 15e16.
Baldwinson, Terence M., 1990. In: John Shore, Colorants and Auxiliaries, second ed.
Society of Dyers and Colourists, Bradford, England, p. 566.
4. Conclusions Brushwood, D.E., 2003. Noncellulosic constituents on raw cotton and their rela-
tionship to fiber physical properties. Tex. Res. J. 7 (10), 912e916.
One-step combined desizing, scouring and bleaching process Buschle-Diller, G., Yang, X.D., Yamamoto, R., 2001. Enzymatic bleaching of cotton
fabric with glucose oxidase. Tex. Res. J. 71 (5), 388e394. http://dx.doi.org/
has been developed for polyester/cotton sheeting fabrics using a 10.1016/S0141-0229(01)00388-X.
novel desizer which is compatible with sodium hydroxide as a Cardamone, J.M., Marmer, W.N., 1995. 'The whitening of textiles'. In: Carr, C.M. (Ed.),
scouring agent and hydrogen peroxide as a bleaching agent. The Chemistry of the Textiles Industry, first ed. Blackie Academic and Professional,
England, p. 46.
one-step process gives commercially acceptable degree of fabric
Carr, C.M., 1995. In: Chemistry of Textile, first ed. Blackie Academic and Professional,
desizing in terms of TEGEWA rating, fabric absorbency and white- London, England, p. 49.
ness. With one-step process reported in this study, it is possible to Cavaco-Paulo, A., Gübitz, Georg, 2003. Catalysis and processing. In: Cavaco-
Paulo, A., Gübitz, G.M. (Eds.), Textile Processing with Enzymes, first ed.
attain a TEGEWA rating of greater than 7 on a scale of 1e9, fabric
Woodhead Pub. Ltd, England, pp. 90e91.
wicking height greater than 6 cm and whiteness greater than 70 on Clark, M., 2011. Pre-treatment and preparation of textile materials prior to dyeing.
the CIE whiteness scale. As compared to the traditional three-step In: Handbook of Textile and Industrial Dyeing, first ed. Woodhead Pub. Ltd,
process, the one-step alternative offers significant savings in Cambridge, England, p. 69.
Csiszar, E., Szaka cs, G., Rusznak, I., 1998. Combining traditional cotton scouring with
chemical cost (39%), water (60%), electricity (52%), steam (54%) and cellulase enzymatic treatment. Tex. Res. J. 68 (3), 163e167.
the process time (52%). The new one-step process is not only Derringer, G., 1980. Simultaneous optimization of several response variables.
economical but also more efficient and ecological because of much J. Quali. Technol. 12, 214e219.
Gulrajani, M.L., Venkatraj, R., Chandrasekaran, P., 1987. A process for the combined
reduced impact on the environment. The new process has been scouring and bleaching of polyester/cotton fabrics at low temperature. J. Soc.
successfully adopted by the textile industry, in which the bulk trials Dye. Colour. 103 (9), 299e303. http://dx.doi.org/10.1111/j.1478-
were made for this study. The process is now being further opti- 4408.1987.tb01123.x.
Hardin, I.R., 2010. Enzymatic Treatment versus Conventional Chemical Processing of
mized and adapted for fabric qualities other than polyester/cotton Cotton. Advances in Textile Biotechnology. Elsevier, Cambridge, England, p. 132.
sheeting fabric used in this study. Hebeish, A., Hashem, M., Shaker, N., Ramadan, M., El-Sadek, B., Hady, M.A., 2009.
New development for combined bioscouring and bleaching of cotton-based
fabrics. Carbohydr. Polym. 78 (4), 961e972. http://dx.doi.org/10.1016/
j.carbpol.2009.07.019.
References
Hill, W.J., Hunter, W.G., 1966. A review of response surface methodology: a litera-
ture survey. Technometrics 8 (4), 571e590.
Abdel-Halim, E.S., Al-Deyab, S.S., 2013. One-step bleaching process for cotton fabrics Huang, K.S., Jan, E.P., Lu, L.A., 2007. A new process for the desizing, scouring and
using activated hydrogen peroxide. Carbohydr. Polym. 92 (2), 1844e1849. bleaching of cotton/nylon fabrics with tetraacetylethylenediamine. Cellu. Chem.
Ali, S., Khatri, Z., Tanwari, A., 2011. Integrated preparatory method for cotton towel Technol. 41 (1), 43e50.
by using enzymes. Int. J. Chem. Environ. Eng. 2, 295e301.
502 M.A. Imran et al. / Journal of Cleaner Production 108 (2015) 494e502

Ibrahim, N.A., El-Hossamy, M., Morsy, M.S., Eid, B.M., 2004. Development of new Saravanan, D., Sivasaravanan, S., Sudharshan Prabhu, M., Vasanthi, N.S., Senthil
eco-friendly options for cotton wet processing. J. App. Polym. Sci. 93 (4), Raja, K., Das, A., Ramachandran, T., 2012. One-step process for desizing and
1825e1836. bleaching of cotton fabrics using the combination of amylase and glucose oxi-
Iqbal, M., Mughal, J., Aleem, A., Siddiqui, Q., 2007. Effect of textile auxiliaries at dase enzymes. J. App. Polym. Sci. 123 (4), 2445e2450. http://dx.doi.org/10.1002/
various stages of processing and its impact on tensile strength. J. Chem. Soc. Pak app.34838.
29, 195e199. Scarborough, S., Mathews, A., 2000. Text. Chem. Color. Amer. Dyestt. Repo. 32 (3),
Karmakar, S.R., 1999. Chemical Technology in the Pre-treatment Processes of Tex- 33e37.
tiles, first ed., vol. 12. Elsevier, Amsterdam, The Netherlands, p. 171. Shafie, A.E., Fouda, M.M., Hashem, M., 2009. One-step process for bio-scouring and
Li, M., Hinks, D., 2012. An Environmentally Benign Approach to Cotton Preparation: peracetic acid bleaching of cotton fabric. Carbohydr. Polym. 78 (2), 302e308.
One Bath Enzymatic Desizing, Scouring and Activated Bleaching. North Carolina http://dx.doi.org/10.1016/j.carbpol.2009.04.002.
State University, pp. 46e51. Shamey, R., Hussein, T., 2005. Critical solutions in the dyeing of cotton textile ma-
Montgomery, D.C., 2005. Design and Analysis of Experiments: Response Surface terials. Text. Prog. 37 (1e2), 1e84. http://dx.doi.org/10.1533/tepr.2005.0001.
Method and Designs. John Wiley and Sons, Inc, New Jersey. Shao, J., Huang, Y., Wang, Z., Liu, J., 2010. Cold padebatch bleaching of cotton fabrics
Montgomery, D.C., 2008. Design and Analysis of Experiments. John Wiley and Sons, with a TAED/H2O2 activating system. Color. Technol. 126 (2), 103e108.
New Jersey. Shore, J., 1998. Blends Dyeing. Society of dyers and colourists, Bradford, England,
Murugesan, K., Dhamija, A., Nam, I.H., Kim, Y.M., Chang, Y.S., 2007. Decolouri- pp. 170e171.
zation of reactive black 5 by laccase: optimization by response surface Tobler-Rohr, M.I., 2011. Handbook of Sustainable Textile Production. Elsevier,
methodology. Dye Pigment. 75 (1), 176e184. http://dx.doi.org/10.1016/ Cambridge, England, pp. 40e45.
j.dyepig.2006.04.020. Trotman, E.R., 1984. Bleaching, Dyeing and Chemical Technology of Textile Fibres.
Nierstrasz, V., Cavaco-Paulo, A., 2010. Advances in Textile Biotechnology. Elsevier, Griffin, Nottingham, p. 222.
Cambridge, England, p. 31. Tzanov, T., Calafell, M., Guebitz, G.M., Cavaco-Paulo, A., 2001. Bio-preparation of
€
Oner, E., Sahinbaskan, B.Y., 2011. A new process of combined pretreatment and cotton fabrics. Enzyme Microb. Technol. 29 (6), 357e362.
dyeing: REST. J. Clean. Prod. 19 (14), 1668e1675. Vigo, T.L., 1994. Textile Processing and Properties: Preparation, Dyeing, Finishing,
Prabaharan, M., Almeida, L., 2004. Process optimization in tetraacetyl ethylenedi- and Performance. Elsevier Science Publishers BV, Amsterdam, The Netherlands,
amine activated sodium perborate bleaching of cotton. Ind. J. Fib. Tex. Res. 29, p. 25.
343e349. Wasif, A.I., Indi, Y.M., 2010. Combined scouring-bleaching of cotton using potassium
Prabaharan, M., Rao, J.V., 2003. Combined desizing, scouring and bleaching of persulphate. Indian J. Fibre Text. Res. 35 (4), 353e357.
cotton using ozone. Indian J. Fibre Text. Res. 28 (4), 437e443. Zeronian, S.H., Inglesby, M.K., 1995. Bleaching of cellulose by hydrogen peroxide.
Rao, J.V., 2001. Developments in grey preparatory processes of cotton textile ma- Cellulose 2 (4), 265e272. http://dx.doi.org/10.1007/BF00811817.
terials. Indian J. Fibre Text. Res. 26 (1/2), 78e92.