Journal of Cleaner Production xxx (2014) 1e8

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Journal of Cleaner Production

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Review

A review on developments in dyeing cotton fabrics with reactive dyes

for reducing effluent pollution
Awais Khatri a, Mazhar Hussain Peerzada a, Muhammad Mohsin b, *, Max White c
a
Department of Textile Engineering, Mehran University of Engineering and Technology, Jamshoro, Sindh 76060, Pakistan
b
Department of Textile Engineering, UET Lahore, Faisalabad Campus, Lahore, Pakistan
c
School of Fashion and Textiles, RMIT University, Brunswick, VIC 3056, Australia

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

Article history: Most cotton fabrics are dyed with reactive dyes because they produce a full range of bright fashion
Received 23 July 2013 colours with a high degree of wash fastness. Application of these dyes, however, causes high and un-
Received in revised form desirable levels of dissolved solids and oxygen demand in the effluent. This is due to the use of
29 August 2014
considerable quantities of inorganic salt and alkali to ensure efficient utilisation and fixation of the
Accepted 5 September 2014
Available online xxx
reactive dyes. Dye that is unfixed on cotton also contributes to effluent pollution. There are two ap-
proaches to deal with the effluent problem: 1. alternative dyeing techniques and technology, 2. effluent
treatment after dyeing. The effluent treatment requires additional capital investment and high treatment
Keywords:
Cotton
and maintenance costs. Therefore, the first approach is always preferable. There have been a number of
Reactive dyes options developed to overcome the polluted effluent problem of dyeing cotton fabric with reactive dyes.
Environmentally sustainable dyeing This paper reviews the options to improve sustainability of the dyeing process through development of
Effluent pollution and treatment reactive dyes, modification of dyeing machinery and processes, chemical modification of cotton fibre
prior to dyeing, use of biodegradable organic compounds in dyebath formulation, and effluent treatment
processes. The paper highlights the significance and limitations of these ways of improving sustainability
in reactive dyeing, and proposes the areas for further improvements.

© 2014 Elsevier Ltd. All rights reserved.

1. Introduction significant worldwide during 1990s (Schramm and Jantschgi, 1999).

As a result, the practice of determining ‘best available techniques/
Globally, the textile dyeing industry is known to be one of the technologies (BAT)’ and maintaining BAT documents started.
major contributors to environmental pollution (Christie, 2007). Per capita demand for apparel textiles is projected to grow
This is mainly due to heavy discharges of inorganic salts, alkalis, continuously. Therefore, it becomes important to find solutions for
other processing aids such as surfactants and organic matter such reducing water use and the discharge of polluting chemicals. For
as dyes to effluent. Particularly, effluents from dyeing cotton with apparel textiles, the predominant dye-fibre combination is that of
reactive dyes are highly polluted and have high oxygen demand, reactive dyes and cotton (King, 2007). However, of all the dye-fibre
colour, and salt load. The industry also consumes large volumes of combinations, cotton dyed with reactive dyes consumes the high-
clean water. Effluent treatment and water-recycling can play a est volume of water per kg of the fibre. Moreover, this combination
significant role in reducing discharge pollution and providing causes the highest discharge of salts, alkalis and organic matter per
reusable processing water. A brief account of such treatments is unit fibre mass (Smith, 2003). Brief explanation to its reason is
presented at the end of the paper due to their wide practice. given in following paragraphs.
However, these treatments are expensive. The better approach Since 1950s, when ICI introduced the first commercial reactive
would obviously be to modifying the textile processing technolo- dyes for cotton, this dyeclass has become increasingly popular
gies and chemistry to reduce the effluent pollution. Such preven- (Holme, 2004). That is mainly due to high levels of washing fast-
tive approach to environment protection has become more ness, a wide gamut of bright colours, and versatility for different
application methods. The high fastness to washing of reactive dyes
is due to their unique reactive group(s), which form(s) covalent
* Corresponding author. bonds with the hydroxyl groups of the cotton cellulose under
E-mail address: [email protected] (M. Mohsin). alkaline pH conditions.

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Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
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2 A. Khatri et al. / Journal of Cleaner Production xxx (2014) 1e8

The dyes also react with hydroxide ions present in the aqueous 2. Development of reactive dyes
dyebath under alkaline pH conditions. This produces nonreactive
hydrolysed dye which remains in the dyebath as well as in the fibre. A number of improved dye structures and mixtures have been
In order to obtain the required levels of washing fastness, it is developed, since the reactive dye was invented. Most of the major
necessary to remove all unreacted and hydrolysed (unfixed) dye advances for reducing effluent pollution are discussed below.
from the cotton fibre. It is achieved by ‘washing-off’; a series of
thorough rinsing and ‘soaping’ steps. Around 50% of the dyeing cost
is related to the washing-off and effluent treatment (Mohsin et al., 2.1. Bifunctional reactive dyes
2013). The dye remained on the fibre after washing-off is consid-
ered as dye fixed on the fibre. The dye fixation efficiency is typically The first commercial reactive dyes for cotton were based on the
in the range of 50e80% (Smith, 2003); i.e. 20e50% of the dye dichloro-s-triazine reactive group. Since then many other reactive
necessary to achieve the desired depth of colour is discharged to groups have been developed (Ahmed, 1995). The most widely used
the environment. reactive groups, in the order of increasing level of reactivity, are
Reactive dyes are soluble anionic dyes which, in solution, are trichloropyrimidine, aminochloro-s-triazine, sulphatoethylsul-
repelled by the negatively charged surface of the cotton fibre. A salt phone, dichloroquinoxaline, aminofluoro-s-triazine, difluoro-
such as sodium chloride or sodium sulphate is added as an elec- chloropyrimide and dichlorotriazin. The extent of dye-fibre
trolyte to promote the dye transfer (exhaustion) to the fibre reaction and the ultimate discharge of unfixed dye vary widely with
(Gordon and Hsieh, 2007). It also supports dye penetration into the the type of reactive group and the dyeing technology used.
fibre interior (diffusion) which leads to better dye fixation (Khatri The use of two reactive groups in a dye molecule results in
et al., 2014a,b). The amount of the salt can vary up to 2 kg per kg higher fixation efficiencies (Shore, 2002). For exhaust dyeing
of the fibre depending on the dye structure, depth of shade and methods, fixation efficiency typically improves from the range of
dyeing method. Once sufficient dye is on the fibre, either by 50e60% to that of 70e80% (Smith, 2003). Many of the reactive dyes
exhaustion (exhaust dyeing methods) or padding (pad dyeing available today contain two reactive groups. Such dyes are known
methods), alkali such as sodium carbonate, sodium bicarbonate or as bifunctional reactive dyes and are further classified as homo-
sodium hydroxide is added to the dyebath to initiate the dye-fibre bifunctional, containing two identical reactive groups (e.g. the ICI
reaction. The quantities and composition of the alkali depend on Procion HE dyes with two aminochloro-s-triazine groups), and
the pH required for the particular type of reactive group of the dye hetero-bifunctional, containing two different reactive groups (e.g.
and the dyeing method. the Sumitomo Sumifix Supra dyes with aminochloro-s-triazine and
Irrespective of the dyeing method and the type of reactive sulphatoethylsuphone groups) (Taylor, 2000). Technically, the
group(s), almost all of the potentially toxic nonbiodegradable bifunctional dyes have increased probability of reaction with the
inorganic salt (Ahmed, 2005), inorganic alkali and unfixed dye are fibre. Thus, they give higher fixation yields and thus leave less
discharged to dyeing effluent. This leads to the environmental colour in the dye-house effluent. For example, the CI Reactive Black
problem of a highly-coloured effluent with high levels of dissolved 5 (Structure I) is a dye containing two sulphatoethylsulphone
solids (Khatri et al., 2013) and oxygen demand (Ali et al., 2014). precursor groups. This dye has long been successful and known to
produce a high degree of fixation.

Urea, which is often used in pad dyeing methods (Kissa, 1969) and The hetero-bifunctional dyes provide better fixation with more
in reactive printing (Koch, 1992) to increase dye solubility and yield flexibility for the colouration method and the process parameters.
of the dye-fibre reaction, is another environmentally undesirable Some bifunctional dyes are claimed to provide a fixation efficiency
chemical (Hyde et al., 1996). Urea, when used in the pad-dry-bake of up to 95% when applied on cotton by the pad-batch dyeing
dyeing process, decomposes and increases the nitrogen content of method (Luttringer, 1993). Such improvements in dye fixation ef-
the effluent (Chavan, 2001). ficiency result in significant reductions in the amount of unfixed
There have been a number of developments for improving the dye in dyeing effluent. The use of commercially available bi- or
quality of effluent for cotton dyeing systems with reactive dyes. poly-functional reactive dyes have been recommended as the best
This paper presents a review of such developments under following available technique for increasing the dye fixation efficiency
five principal areas. The discussion focuses primarily on how re- (European Commission, 2003).
searchers and industry are addressing the issues of how to reduce
the discharge amounts of inorganic chemicals (salt, alkali and urea)
and unfixed dye, and followed by effluent treatment processes. 2.2. Polyfunctional reactive dyes

 Development of reactive dyes Incorporating more than two reactive groups into the dye
 Developments in dyeing machinery and processes molecule should theoretically increase the fixation efficiency.
 Chemical modification of cotton fibre prior to dyeing However, these additional reactive groups can have an impact on
 Use of biodegradable organic compounds in dyebath formulation important dyeing properties such as substantivity and migration
 Effluent treatment processes because they change the molecular size and alter the extent and
mode of reactivity. Therefore, the idea of additional reactive

Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
pollution, Journal of Cleaner Production (2014), http://dx.doi.org/10.1016/j.jclepro.2014.09.017
 A. Khatri et al. / Journal of Cleaner Production xxx (2014) 1e8 3

group(s) have been more of patenting interest (Taylor, 2000). A such dyes produce lower amounts of unfixed dye and salt in the
careful combination of reactive groups can make polyfunctional dyeing effluent. They are based largely, but not exclusively, upon
dyes superior to traditional dyes. Remazol Red SBB (CI Reactive Red bis(aminofluoro-s-triazine). Use of such low-salt reactive dyes have
181) was the first commercial trifunctional reactive dye by Hoechst been acknowledged as the best available technique for reducing the
(Lewis, 2009). Remazol Red BS and Cibacron Red C-2G are other use of an electrolyte (European Commission, 2003).
commercially successful examples of such dyes. Tertafunctional
and pentafunctional dyes have also been discovered by researchers 2.7. Cationic reactive dyes
and dye manufacturers, but are not yet commercial.
Traditional reactive dyes, being anionic, require high concen-
2.3. Dye mixtures trations of salt to overcome the repulsion effects arising from the
anionic charge on the surface of the cotton fibre in the dyebath.
Commercial mixtures of selected reactive dyes have become Subsequently, development of cationic reactive dyes eliminates the
popular because they provide an economic range of secondary and requirement of an electrolyte (Hinks et al., 2001). Such dyes offer
tertiary colours (Taylor, 2000). At the same time, the commercial the potential for dyeing of cotton using zero-salt but they are yet to
mixtures can have improved dyeing properties and reduced be commercialised.
sensitivity to dyeing variables such as temperature and pH. In turn,
it can improve dye fixation efficiency. 3. Developments in dyeing machinery and processes

2.4. Reactive dye fixable at neutral pH 3.1. Low liquor-to-fibre ratio dyeing

Reactive groups containing a nicotinic acid residue can allow As per industrial dyeing practice, the concentrations of inor-
dye-fibre reaction at a neutral pH of 7e7.5 (Morimura and Ojima, ganic salt and alkali are determined by the mass per unit volume of
1985). A typical aminonicotinotriazine reactive group (Structure II) dyeing liquor. Thus, the total consumption of inorganic chemicals
was introduced by Nippon Kayaku with the name of Kayacelon can be reduced by reducing the total volume of dyeing liquor
React. The Kayacelon React is a homo-bifunctional reactive dye (Kalliala and Talvenmaa, 2000). On the basis of this approach, a
range with the bis(aminonicotinotriazine) reactive system (Renfrew, wide number of forms of low liquor-to-fibre ratio dyeing machines
1999). The requirement of using inorganic alkali for dyeing cotton at have been commercially developed (Phillips, 1996) such as Thies in
pH of 10e12 becomes unnecessary and the amount of the alkali in cooperation with DyStar introduced the Luft-roto Plus as an ultra
dyeing effluent is substantially reduced. These dyes are particularly low liquor ratio dyeing machine (Wilbers and Seiler, 2002). The
suitable for neutral, high temperature exhaust dyeing, and for one- ultra low liquor ratio dyeing machines offer the opportunity to dye
bath one-step dyeing of polyester/cotton blended fabrics. The at ratios as low as 4:1. Industry has been motivated to move from
dyeing starts with the addition of dye, salt and a buffer (pH 7e7.5) 20:1 ratio to lower liquor ratios. The reduction in liquor ratio re-
followed by raising the temperature (Lewis, 1993). This develop- duces the chance of the reactive dye being repelled by cotton fibre
ment was encouraged by the industry. Therefore, more efforts have (Anderson, 1994). Thus, a reduced concentration of salt is needed
been taken in the same direction (Lewis at al., 2008). for dye exhaustion. The use of less volume of water also decreases
the possibility of dyebath hydrolysis. Other advantages of the
development of low liquor-to-fibre ratio dyeing machinery are less
water usage, reduced dye liquor wastage and lower steam con-
sumption to heat the dyebath, thus, minimising air-pollution
generated by steam boilers and reducing the heating costs. Due
to the apparent ecological and economic advantages of this
development, such dyeing machines are highly recommended as
the best available technology for exhaust dyeing (European
Commission, 2003).

3.2. Pad dyeing technology

From a sustainability perspective, padding based dyeing

2.5. Acid fixing reactive dyes methods for cotton fabrics are the most preferred colouration
pathway (Schramm and Jantschgi, 1999). Relative to exhaust
Acid-fixing reactive dyes were developed for reducing the salt dyeing, padding methods offer: Lowest liquor-to-fibre ratio in the
requirement. Burlington Industries (USA) developed reactive dyes dyebath, lower amounts of left-over dyebath solution, faster dye
containing phosphonic acid and carboxylic acid reactive groups for application, easier control on dye levelness on the fabric, and no
dyeing at acidic pH (Renfrew, 1999). However, the use of these dyes electrolyte required for exhaustion (Leube, 2003). However, these
has been reported to cause tendering of cotton (Nkeonye and methods are normally avoided on knitted fabrics and small lots
Olawande, 1994), therefore, they are not commercially successful. due to certain limitations (Smith, 2003) such as dimensional
instability and higher pollution load (European Commission,
2.6. Low-salt reactive dyes 2003).
Pad-batch process, also referred to as cold-pad-batch, of dyeing
The ‘low-salt’ Cibacron LS reactive dyes developed by Ciba have with reactive dyes involves padding the fabric with a dye solution
allowed meaningful improvements to the discharge effluent (Anon, containing a suitable alkali system and then winding the fabric onto
1996). DyStar introduced Remazol EF as its low-salt reactive dye a roller before batching for 6e24 h, followed by washing off
range (Taylor, 2000). The requirement of reduced amount of salt is (Aspland, 1992). Among all pad dyeing processes, pad-batch dyeing
due to the high affinity of such dyes to cotton. Most of these low-salt is the most economical process for the reactive dyeing of cotton. For
dyes are bifunctional and have high fixation efficiencies. Therefore, small lots of around 1000e10,000 m, this process is even more

Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
pollution, Journal of Cleaner Production (2014), http://dx.doi.org/10.1016/j.jclepro.2014.09.017
4 A. Khatri et al. / Journal of Cleaner Production xxx (2014) 1e8

economical than exhaust dyeing, mainly due to lower energy re- 3.5. Modified washing-off techniques
quirements. The cold pad batch dyed fabrics are claimed to have an
improved handle and cleaner surface appearance. Prominent water Washing-off is required to remove unreacted and hydrolysed
and energy savings (Khatri et al., 2014a,b), reduced consumption of dye from the cotton fibre at the end of the dyeing process. The
dyes and chemicals, and less space and labour requirements, of washing-off steps normally recommended by dye manufacturers
pad-batch dyeing process (Stone, 1979), make it economical and are a cold rinse, followed by a warm rinse, soaping at the boil, a
ecologically sustainable (Van Wersch, 1992). warm rinse and finally a cold rinse. An approach of ‘hot-washing’,
i.e. beginning with hot rinses and a final rinse at low temperature,
3.3. Low padding trough volumes has been reported to improve dyeing results and marginally reduce
effluent chemical oxygen demand (Sostar-Turk et al., 2008).
In pad dyeing processes, the dyeing liquor left in the padding Bayer introduced an ‘enzymatic after soaping’ process for
trough, pipes and pumps is drained to the effluent in its concen- exhaust application method, later continued by BASF, for removing
trated form at the end of a dyeing process (European Commission, the unfixed dyes not only from the fibre, but also from the
2003). The volume of the liquor left depends on the padding trough exhausted dyebath (European Commission, 2003). The application
capacity. Reduced trough volumes down to 10e15 L provided of the patented enzymatic compounds, recommended as the best
meaningful reductions in such waste (Phillips, 1996). The new available technique by the Commission, usually takes place in the
padders also benefit in reduced wastage of cotton fabric caused by fourth or fifth rinsing step (see Table 1). No detergent is required
‘tailing’ (Leube, 2003). Tailing is the result of preferential dye up- and one of the hot rinsing steps can be avoided when using enzy-
take of one colour by cotton fibre when dyeing with combination of matic aftertreatment. Therefore, savings in water, energy and
colours. The European Commission (2003) recommended this detergent consumption are the main advantages achievable with
technology, example shown in Fig. 1(A), and also carrying out the this technique.
fabric impregnation step in a nip, Fig. 1(B), as the best available
technologies for reducing the dyeing liquor wastages. Therefore,
3.6. Aftertreatments to fix hydrolysed dye on the fibre
industry is highly motivated to use such padders which lead to cost
savings through reduced liquor waste and reductions in off-
A hydrolysed dye is not able to react with cotton and is removed
specification fabric shades.
through washing-off. A dye fixation efficiency of up to 99% is
sometimes claimed for some reactive dyes with pad-batch dyeing
3.4. Urea- and salt-free continuous dyeing process processes (Phillips, 1996). However, there is still a need for
washing-off to remove any residual hydrolysed and unreacted dyes
Urea is used in continuous pad-dry-bake dyeing process to on the fibre. The use of certain aftertreatment agents to trap small
improve the yield of the dye-fibre reaction. Inorganic salt is used amounts of hydrolysed dye in the fibre has been proposed for
in the continuous pad-steam dyeing process to improve dye reducing the amount of unfixed dye in the discharge and to
levelness into the fibre, and also in the pad-dry-chemical pad- improve colour yields. Cationic aftertreatment agents have been
steam process to avoid dye bleeding during the second chemical studied for immobilising the unfixed dye present on the fibre
padding step. A commercially viable dyeing machine jointly (Cook, 1982). Improvements in colourfastness to washing were
developed by BASF and Monforts, called ‘Econtrol’, eliminates the found (Sampath, 2002). However, such treatments may lead to
need for urea and salt (Hyde, 1998). The machine is designed to slight reduction of the colourfastness to light (Vasileva and Jeleva,
inject humidity into the hot fixation chamber. The typical fixation 2009). Dye manufacturers market such cationic aftertreatment
conditions for a dichloro-s-triazine dyes have been reported as agents (Burkinshaw and Katsarelias, 1995).
120  C temperature and 20e25% relative humidity. Only small
concentrations of alkali (sodium bicarbonate) are required for
these dyes. This development has been highly encouraged as the 3.7. Polymerisation techniques for dye fixation
best available technology for improving ecological and economic
impact of the pad dyeing processes (European Commission, The polymerisation of dye molecules has been explored as a
2003). method for achieving 100% dye fixation (Taylor, 2000). Individual
dye molecules react together in the dyebath forming a polymeric
dye. The polymeric dye is then subjected to covalent fixation to
cellulose through its conventional reactive groups. This approach
offers many potential benefits including the prevention of coloured
effluent and dyeing without using salt. However, the concept has
yet to result as to be commercialized.

Table 1
Comparison of the sequence steps between a conventional and an enzymatic after
soaping treatment (exhaust dyeing).

Typical sequence in the case Sequence in the case of

of conventional washing-off enzymatic after soaping

5 min overflow rinsing 5 min overflow rinsing

10 min 40  C 10 min 40  C; neutralization
10 min 40  C; neutralisation 10 min 60  C
10 min 95  C 10 min 95  C
10 min 95  C 50  C; enzymatic treatment
10 min 50  C 10 min 30  C
10 min 30  C e
Fig. 1. Representation of a U-shaft (A) and nip (B) dye liquor application systems.

Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
pollution, Journal of Cleaner Production (2014), http://dx.doi.org/10.1016/j.jclepro.2014.09.017
 A. Khatri et al. / Journal of Cleaner Production xxx (2014) 1e8 5

3.8. Micelle dyeing stability. Mercerisation is an expensive process in terms of capital,

maintenance, running and the caustic recovery costs. An experi-
Recently, Xie et al. (2011) have reported a micelle dyeing as a mental refinement into the cationisation of cotton fabric has the po-
novel reactive dyeing method for cotton to save large amount of tential of replacing the mercerization process, which can be carried
water and energy. They prepared the dye-surfactant micelles using out on a stenter without any capital and much of the running costs.
dibutyl maleic acid ester sodium sulfate surfactant and applied
them on a cotton fabric at lower liquor-to-fibre ratio of about 5:1 5. Use of biodegradable organic compounds in dyebath
using an IR dyeing machine. Acceptable dyeing results with good formulation
dye-levelness have been shown.
The use of alternative biodegradable non-toxic dyes and
3.9. Emerging technologies chemicals for dyeing is a direct approach of reducing the effluent
pollution. Use of selected organic compounds has been shown to be
The use of certain electromagnetic radiations has been an in- an effective alternative to inorganic salt (Rucker and Guthrie, 1997).
terest to save energy and time consumed on heating and agitating Such compounds reduce effluent load, as most of these tend to be
the dyebath or the padded fabric. However, this approach has not biodegradable. Betaine, an organic compound, has been reported to
been well taken commercially yet. In this context, the use of ul- reduce the amount of inorganic salt (Liu and Yao, 2009). Organic
trasonic energy in dyeing cellulosic fabrics with reactive dyes by cationic surfactants have also been studied as inorganic salt sub-
exhaust (Oner et al., 1995) and pad-batch (Khatri et al., 2011) pro- stitutes (Rucker and Guthrie, 1997). The use of a mixture of
cesses has been studied. The studies have shown that the use of magnesium-based organic compounds in the dyeing of cotton with
ultrasound can result in energy savings, lesser water and chemical direct or reactive dyes has been patented (Moore, 1993). The
consumption, better colour yields and reducing effluent pollution. mixture is claimed to substitute inorganic sodium chloride or so-
As a step towards the application of ultrasonic energy at industrial dium sulphate that prevents the discharge of untreatable toxic
scale, Thakore (Thakore, 2011) constructed a specially mounted effluent. However, this could not be commercialised because
ultrasonic tube resonator and used it for exhaust and pad-batch magnesium ions cause water hardness and create problems with
dyeings of cellulose based fabrics with reactive dyes on a produc- colour matching and dyeing process control (Jain and Mehta, 1991).
tion scale. Improved colour yields, reduced dyeing time and the The sodium salts of organic acids have been explored as alter-
improved washing-off efficiency were the key outcomes of that natives to sodium chloride and sodium sulphate. Prabu and
study. Sundrajan (2002) have demonstrated the use of trisodium citrate
Using microwave heating has been studied for improving as an alternative to traditional inorganic salts for exhaust dyeing of
reactive dye uptake and fixation on cotton fabrics (Lei et al., 2013). cotton with reactive, direct and solubilised vat dyes. Salts of poly-
That is reported to result better colour yield and dye fixation effi- carboxylic acids have also been shown to be the most effective al-
ciency compared to the conventional heating methods. Other ternatives to inorganic salts (Guan et al., 2007). The tetrasodium
emerging technologies such as plasma and supercritical carbon ethylene diamine tetra-acetate, an alkaline polycarboxylic sodium
dioxide have also been reported as alternative ways of eliminating salt, has been reported as an alternative to inorganic salt and alkali
or reducing the use of water and provide acceptable dyeing results in exhaust (Ahmed, 2005) and continuous pad-steam dyeing
(Ahmed and El-Shishtawy, 2010). (Khatri, 2011) of cotton with reactive dyes. The use of other alkaline
polycarboxylic salts (Khatri et al., 2010), such as trisodium nitrilo
4. Chemical modification of cotton fibre prior to dyeing triacetate (Khatri et al., 2013) and tetrasodium N,N-bis(carbox-
ylatomethyl)-L-glutamate (Khatri and Peerzada, 2012), has also
The chemical modification of cotton to improve dyeing with been shown to effectively substitute the inorganic salt and alkali in
direct, reactive, sulphur or vat dyes, is another emerging area. This continuous pad-steam reactive dyeing of cotton. This development
research has focussed mainly on the introduction of cationic groups led to reducing effluent TDS and improve dye fixation efficiency.
to the cotton fibre (Lewis and McIlroy, 1997). Such modifications, In the continuous pad-dry-bake reactive dyeing method, where
usually referred to as cationisation, are achieved by treating cotton urea is used, the process conditions result in some decomposition
with low molecular weight cationic chemicals or with cationic of the urea. That causes an increase in the residual nitrogen content
polymers (resins). Most of the cationic groups are quaternary, ter- and to some extent reduces the yield of dye-fibre reaction. Using
tiary or secondary amino residues. In the reactive dyeing of cat- reduced amount of urea with a dicyandiamide in the dyebath has
ionised cotton, the anionic dyes are attracted by the cationic been proposed to reduce the environmental impact (Phillips, 1996).
charges on the fibre. As a result, higher fixation efficiency and Caprolactum products have been reported as partial or complete
reduced (or no) use of salt can be achieved. Salt and alkali free substitution of urea in reactive dyeing and printing of cotton fabrics
reactive dyeing of modified cotton have also been reported (Sheth and Musale, 2004).
(Blackburn and Burkinshaw, 2003).
In reactive dyeing, cationisation of cotton has been shown to be 6. Effluent treatment processes for cotton dye-houses
capable of eliminating the use of inorganic salt and alkali and
leaving a reduced amount of unfixed dye. This offers significant The effluent components can be classified in four ways of sus-
environmental benefits. However, the technique has yet to be tainability concern, i.e. coloured or colourless, dissolved or not
adopted by industry. That is mainly because cationisation is an dissolved, biodegradable or non-biodegradable, toxic or non-toxic.
additional process step and the treatment itself does not guarantee The majority of the conventional cotton processing effluents are
nontoxic effluent. Natural polymers such as cationic starch (Zhang multi-coloured and composed of non-biodegradable and toxic
et al., 2005) and chitosan (Bhuiyan et al., 2014) have been explored dissolved components. A typical composition of cotton textile mill
as cationising agents. These may make the cationisation process waste is given in Table 2 (Babu et al., 2007). Most of the dyes being
environmentally safer. organic compounds contribute lesser to the toxicity comparing to
Mercerisation of cotton fabric is a usual practice of continuous dye- other inorganic colourless compounds specially salts. However,
houses. It is a pre-dyeing process that ensures the benefits of their colour reduces the depth of penetration of sunlight into the
improved colour yield, tensile strength, lustre and dimensional water environment of drains, channels and rivers, which in turn

Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
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6 A. Khatri et al. / Journal of Cleaner Production xxx (2014) 1e8

Table 2 such as activated carbon and clay, or let the effluent pass through a
Typical composition of the cotton textile mill waste. filter bed composed of granular materials. In this way, pollutants in
Characteristics Values the effluent are adsorbed and removed on the surface of the porous
pH 9.8e11.8
material or filter. Commonly used adsorbents are activated carbon,
Total alkalinity 17e22 mg/l silicon polymers and kaolin. Different adsorbents have selective
BOD 760e900 mg/l adsorption of dyes. The activated carbon has been regarded as the
COD 1400e1700 mg/l best adsorbent for dyeing effluent so far (Christie, 2007). However,
Total dissolved solids 6000e7000 mg/l
the adsorption on activated carbon without pretreatment is
Total chromium 10e13 mg/l
impossible because the suspended solids rapidly clog the filter.
Therefore, this procedure is only feasible in combination with
decreases photosynthetic activity and dissolved oxygen (Cooper, flocculation decantation treatment or a biological treatment. The
1995). That can create an imbalance in the ecosystem and combination permits a reduction of suspended solids and organic
become a threat for aquatic life and organisms. Because they need substances, as well as a slight reduction in the colour. Moreover, the
light in order to develop. Moreover, river water meant for human cost of activated carbon is high.
consumption that is coloured will increase treatment costs.
Therefore, specifying legal limits (although not practiced in all 6.3. Biological treatments
countries) are justified.
The effluent treatment is itself a big processing sector. In the For removal of the bulk of toxic pollutants from complex organic
past several decades, there have a number of techniques and effluent, biological treatment is usually believed to be the most
technologies developed for effluent treatments depending on the effective mean. In such processes, microorganisms usually bacteria
type of industry. The focus of such developments has been to find (natural or regenerated) are used for the biodegradation of syn-
an economic and efficient way to treat the effluent. Today, the thetic dyes and other dissolved substances. The biological process
highly efficient treatment technologies for textile dyeing effluents removes dissolved matter in a way similar to the self-cleaning and
are physicochemical, biochemical, combined treatment processes in a more efficient way than clariflocculation. Biological treatments
and other technologies (Hauser, 2011). They may be further clas- can be classified according to the presence and absence of oxygen,
sified as physical methods (precipitation such as coagulation, respectively known as aerobic and anaerobic treatments (Babu
flocculation and sedimentation; adsorption such as on activated et al., 2007). The aerobic treatments, due to their high efficiency
carbon and biological sludges; and membrane processes, also and wide application, are the most preferable biological treatment.
known as separation techniques, such as reverse osmoses, micro- Aerobic biological treatment can purify the water with the help of
filtration, nano-filtration, ultra-filtration), biological treatments, aerobic and facultative bacteria in the aerobic environment, which
Chemical treatments (oxidative treatments including electro- is divided into two major categories, i.e. activated sludge process
chemical processes and advanced oxidation processes such as and biofilm process. The Activated sludge is more common aerobic
ozone treatment) (Christie, 2007). These treatments are sometimes process in which cleaning efficiency up to 90% can be possible.
designed and carried out in various combinations to have an However, biological treatment of most of the textile dyes and
effective treatment and recycling. A brief description on the most chemicals by the activated sludge process does not always achieve a
effective technologies for the treatment of effluent from cotton dye- great success. Because most of the dyes and chemicals used in the
houses is given below. However, the effluent treatments and textile industry have low or no biodegradability. Therefore, adsor-
recycling methods have been well explained in detail by Hauser bents, such as activated carbon or clay, are added to biological
(2011) and Vandevivere et al. (1998). treatment systems in order to eliminate non-biodegradable sub-
stances produced by the textile industry.
6.1. Coagulation flocculation sedimentation treatments
6.4. Chemical oxidation
Coagulation flocculation sedimentation treatments are gener-
ally used to eliminate organic substances, but the chemicals nor- Chemical oxidation treatments are basically the bleaching pro-
mally used in this process have no effect on the elimination of cesses. In such treatments, the colour components present in the
soluble dyestuffs. Although this process effectively eliminates effluent are oxidized and decomposed to lower molecular weight
insoluble dyes, its value is doubtful because of the cost of treating compounds such as aldehydes, carboxylates, sulphates and nitro-
the sludge and the increasing number of restrictions concerning the gen, and further to degrade them to carbon dioxide and water
disposal of sludge. The electrical charge of colloidal type of very (Christie, 2007). These treatments are the most commonly used
small size suspended mater in the effluent cause repulsion and decolourisation processes as they require low quantities of oxidants
prevent their aggregation. Therefore, electrolytic products such as and short reaction times. They can be applied either as stand-alone
aluminum sulphate, ferric sulphate, ferric chloride are added to technologies or as an integral part of the physical treatments.
eliminate the surface electrical charges of the colloids (Hauser, Various types of oxidant including chlorine, hydrogen peroxide,
2011). This effect is named as coagulation. Normally the colloids ozone and chlorine dioxide are used for colour removal from
bring negative charges, so the coagulants are usually inorganic or effluent. Currently, Fenton oxidation and ozone oxidation are often
organic cationic coagulants (with positive charge in water). The used in the effluent treatment.
metallic hydroxides and the organic polymers can help the particle
aggregation into flocks in addition to coagulation, thereby 6.5. Advanced oxidation processes
increasing the sedimentation. The combined action of coagulation,
flocculation and settling is named as ‘clariflocculation’. Advanced oxidation processes (AOPs) are the processes where
majority of the complex chemicals present in the effluent are oxi-
6.2. Adsorption treatments dised by generating then using activated hydroxyl radicals in suf-
ficient quantities (Hauser, 2011). Hydroxyl radicals have the highest
Adsorption is a physicochemical effluent treatment in which oxidation potential after fluorine radical. The fluorine cannot be
effluent is mixed with the porous material (powder or granules), used for effluent treatment because of its high toxicity. Therefore,

Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
pollution, Journal of Cleaner Production (2014), http://dx.doi.org/10.1016/j.jclepro.2014.09.017
 A. Khatri et al. / Journal of Cleaner Production xxx (2014) 1e8 7

generation of hydroxyl radical and AOPs have gained attention of commercial low-salt reactive dyes and the dyes fixable at neutral
many scientists and technology developers. The activated hydroxyl pH led to reductions into the use of inorganic chemicals. Ultra low
radical are generated by using the UV, UV/O3, UV/H2O2, Feþ2/H2O2, liquor ratio dyeing machines, padders with low trough volume
TiO2/H2O2 and many other combinations. AOPs can be classified in capacity and Econtrol dyeing machine are commercially successful
two groups, i.e. non-photochemical and photochemical. The non- developments for considerably reducing the amount of polluting
photochemical AOPs include cavitation, Fenton and similar pro- chemicals in the effluent. Therefore, their wider use should be
cesses, ozonation at high pH, ozone/hydrogen peroxide, wet air encouraged. Cationisation of cotton is an effective way of reactive
oxidation, etc. The photochemical oxidation processes include ho- dyeing of cotton without inorganic salt and alkali. However, catio-
mogenous (vacuum UV photolysis, UV/hydrogen peroxide, UV/ nisation using natural biodegradable polymers may be a more
ozone, UV/ozone/hydrogen peroxide, photo-Fenton, etc), and het- preferred environmentally sustainable approach. Replacement of
erogeneous (photocatalysis, etc) processes. inorganic chemicals with biodegradable organic compounds is
another way of reducing effluent pollution effectively.
6.6. Electrochemical processes The emerging technologies such as ultrasonic energy and su-
percritical carbon dioxide have been the focus of many researchers.
The base of electrochemical processes is to use electrodes to Commercial developments into these technologies for dyeing cot-
conduct effluent treatment processes such as oxidation, reduction, ton fabrics have environmentally sustainable future. Most of the
coagulation or flocculation by generating electrolytic effect environmentally sustainable options are more costly. Thus, indus-
(Christie, 2007). Such treatments are more efficient than many trial dyers were not encouraged to implement it in past. However,
non-electrochemical treatments. These have the advantages of currently throughout the world, governments and water author-
small devices, small covered area, easily operating and manageable, ities are introducing tougher load based discharge permits, charges
higher rate of removing dissolved solids and oxygen demand and and penalties. The relative higher costs of environmentally sus-
good bleaching effect. However, the precipitation, consumption of tainable options may be offset, in whole or part, by the costs of
electrode material and operating cost are very high. The cost of effluent purification or by penalties on more polluted effluent.
treatment can be effectively decreased with the development of As many industries are motivated to do effluent purification and
electrochemical technologies and availability of a variety of high recycling, a brief account of effluent purification treatments has
efficiency reactors. Electro-catalytic advanced oxidation process also been provided in this review. Membrane separation techniques
(AEOP) is a new advanced oxidation technology developed recently are widely practiced due to their simplicity and recycling advan-
(Hauser, 2011). Because of its high efficiency, easy operation, and tages. Adsorption on activated carbon, biological and electro-
environmental friendliness, it has attracted the attention of re- chemical treatments, AOPs and AEOPs are other emerging
searchers. It can produce hydroxyl radicals directly or indirectly technologies. However, the effluent treatments are expensive.
through the reactions in the catalytic activity electrode under Therefore, the first obvious choice should always be more sus-
normal temperature and pressure. Thus, the degradation of the tainable dyeing techniques and technologies.
difficultly biodegradable pollutants is effective. It is one of the main
directions in future research.
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Please cite this article in press as: Khatri, A., et al., A review on developments in dyeing cotton fabrics with reactive dyes for reducing effluent
pollution, Journal of Cleaner Production (2014), http://dx.doi.org/10.1016/j.jclepro.2014.09.017