Journal of Hazardous Materials B127 (2005) 40–47

Electrochemical coagulation for textile effluent decolorization

Chen-Lu Yang a,∗ , Jared McGarrahan b
a University of Massachusetts-Dartmouth, Advanced Technology and Manufacturing Center, 151 Martine Street, Fall River, MA, USA
b University of Massachusetts-Dartmouth, Department of Textile Sciences, 285 Old Westport Road, North Dartmouth, MA, USA

Received 29 October 2004; received in revised form 15 February 2005; accepted 23 May 2005
Available online 19 August 2005

Abstract

The three most commonly used dyestuffs in textile industry are reactive, acid, and dispersed dyes. One dye from each group, C.I. Reactive
Blue-19, C.I. Acid Red-266, and C.I. Disperse Yellow-218 was chosen to study the feasibility of coagulation for color removal. The dyes used in
these experiments were chosen to represent the two major structural features: anthraquinone and azo dyes. Reactive Blue is an anthraquinone-
based dye, and Acid Red and Disperse Yellow represent azo-based dyes. As there is no standard method to measure the color intensity, a
Hach spectrophotometer was used to measure the absorbance before and after the dye solution was treated. Removal efficiencies on these
dyes were obtained by measuring absorbance of a sample at 592 nm for Reactive Blue, 498 nm for Acid Red, and 428 nm for Disperse Yellow.
Aluminum and ferric coagulants were produced in a parallel-plate electrochemical reactor by anodic dissolution. Removal efficiencies of more
than 98%, in terms of absorbance, were observed in laboratory conditions. Removal was found highly dependent upon NaCl concentration,
applied voltage, current density, and pH. The NaCl in the solution effectively reduced the power consumption and promoted the coagulant
generation by depasivating the Al–water and Fe–water electrochemical systems. The processes were determined to be highly NaCl dependent.
A mechanism was proposed for the corresponding liquid phase chemistry.
© 2005 Elsevier B.V. All rights reserved.

Keywords: Electrochemical coagulation; Decolorization; Textiles dyes; Anodic dissolution

1. Introduction which they can be applied, and the chemical nature of each
dye determines the fibers for which the dye has affinity. Acid
Textile manufacturing begins with the production or har- dyes are water-soluble anionic compounds applied to nylon,
vest of raw fiber. After the raw natural or synthetic fibers wool, silk, and some modified acrylic textiles in an acidic
are shipped from the farm or the chemical plant, they pass medium. They have one or more sulfonic or carboxylic acid
through four main stages of processing: yarn production, groups in their molecular structure. The dye-fiber affinity is
fabric production, finishing, and fabrication. For most uses, the result of ionic bonds between the sulfonic acid part of
these fabrics must undergo further processing, which includes the dye and the basic amino groups in wool, silk, and nylon
bleaching, printing, dyeing, mechanical finishing, preshrink- fibers.
ing, and shaping. Many different textures can also be obtained Reactive dyes are water-soluble, anionic dyes that require
through the application of resins and sizings and the use of relatively simple dyeing methods. They are mainly used for
high temperature and pressure. dyeing cellulosic fibers, such as cotton and rayon, but are
Dyes used by the textile industry are largely synthetic and also used for silk, wool, nylon, and leather. Reactive dyes
are derived from coal tar and petroleum-based intermediates. have largely replaced direct, azoic, and vat dyes and are the
The primary classification of dyes is based on the fibers to largest dye class in the United States. The dyes form covalent
bonds with the fiber and become part of the fiber. To exhaust
the dyes, large amounts of salt are generally essential, and
∗ Corresponding author. Tel.: +1 508 910 9857. significant amounts of dye can remain unfixed at end of the
E-mail address: cyang@umassd.edu (C.-L. Yang). process.

0304-3894/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2005.05.050
 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47 41

Disperse dyes have a very low water solubility, so they adsorption systems for effluent decolorization have yet to be
are applied as a dispersion of finely ground powders in the accepted by the industry. Cucurbituril, a cyclic hexamer with
dyebath. The dyes dissolve at low concentration in the aque- an internal hydrophobic cavity, has been studied for removal
ous dyeing bath but transfer into the synthetic fiber polymer of reactive dyes [7]. An adsorption capacity of 1 g/g makes
because of their higher solubility in the substrate. High tem- this material a candidate for further development. However,
peratures and pressures are consistently used for application. high pH and salt concentrations may have an adverse effect
Disperse dyes are used for oleophylic fibers and polyester on the adsorption.
and other synthetics that do not accept water-soluble dyes. Aerobic treatment of industrial effluents typically
In general, wastewater treatment methodologies in the tex- removes most of the biochemical oxygen demand (BOD)
tile industry are mature and well developed. The industry and 60–80% of COD in wastewater [2,8,9]. However, these
and its regulators have focused on improving the efficiency treatments are ineffective for color removal from textile
of existing treatment processes for some time. The textile industry wastewater because most of the synthetic dyes are
industry is concerned that color residues in dyeing wastewater non-biodegradable. In anaerobic processes, the azo bonds
might not be amendable to treatment with existing treatment can be used as electron acceptors in the electron transport
systems. Technologies to remove color from textile effluents pathways. The products of the azo bond cleavage are lower
continue to be an active area of research and development, molecular weight aromatic amines. Although they are
pursued actively in the United States and abroad. colorless, they cannot be further degraded under anaerobic
conditions. Therefore, various combined processes, such
as anaerobic/aerobic [8], chemical/biological [10], and
2. Literature review electrochemical/biological [11], processes have been under
intensive study to completely mineralize organic dyes.
Decomposition of chromospheres in organic dyes can be All the pretreatments show potential for increasing the
achieved by injecting a strong oxidizing agent, such as ozone biodegradability of textiles effluents for further biological
(O3 ) and hydrogen peroxide (H2 O2 ), to the industrial efflu- treatment. However, the presence of salt, sulfur compounds,
ents [1–3]. Very high color removal and significant amount of heavy metals, and other toxic compounds often inhibits the
chemical oxygen demand (COD) reduction can be achieved anaerobic microbial population and increases chemical and
with ozone application. The process also increases the aero- power consumption in these pretreatment processes.
bic biodegradability of the dyes in the wastewater. However, Among electrochemical treatments, electrochemical oxi-
a large dose of ozone is usually required for decolorization dation and electrochemical coagulation are more effective
due to the significant amount of auxiliary chemicals, such as than others in decolorizing textiles effluents. Although some
acetic acid and silicone oil in the dyebath. Little color removal electrochemical processes involve the direct oxidation of
is achieved by H2 O2 alone or even with ferrous ions as cat- pollutants at anode surfaces, most of the others involve pro-
alyst, known as Fenton’s reagent. Current research has been duction of active species to react with target pollutants. The
focused on combining H2 O2 with UV or ozone to generate rate of electrochemical oxidation depends on the type of elec-
hydroxyl radicals (HO• ) to oxidize various organic chem- trolyte, electrolyte concentration, reaction temperature, and
icals [4,5]. These processes are known in the literature as current density [12]. Another promising electrochemical pro-
the advanced oxidation processes (AOP). The oxidation of cess is by coagulation [13]. Aluminum and iron sheets have
organic dyes with AOP usually produces oxygenated organic been used as consumable anodes to generate coagulants that
compounds and low molecular weight acids that are more adsorb and remove organic dyes. An aluminum coagulant
biodegradable. removes colorant by simple adsorption without involving
Treatment with strong reducing agents, such as sodium chemical reactions while an iron-based coagulant provides
hydrosulfite, sodium borohydride, and sodium dithionite, has ferrous ions (Fe2+ ) to further degrade the dyes [14]. Likewise,
been shown to significantly reduce color in textile effluent [6]. the iron process seems more effective for removal of reactive
These compounds chemically break the nitrogen–nitrogen dyes while the aluminum process is superior for removal of
double bond of azo dyes and produce lower molecular weight disperse dyes [15].
aromatic amines. A small number of aromatic amines are Most of the ongoing development programs address an
classified as being carcinogenic or potentially carcinogenic approach of extending the capacity of existing processes for
to humans. Those azo dyes that can release harmful aromatic dye decomposition or removal. A thorough cost estimation
amines upon reductive cleavage of azo group will soon be has been done on a wastewater treatment system for a flow
banned in European market. rate of 100,000 gallons per day [16]. Table 1 details the result
Adsorption processes have been applied for concentrat- of that study. Operating costs of ozone treatment are higher
ing organic compounds from industrial effluents for years. than that of electrochemical treatment for the same level of
The most widely used adsorbent is granular activated carbon color removal. Chemical reduction is only able to remove a
(GAC). GAC has been proven to be effective for removal of portion of the color but at a competitive cost. A GAC sys-
color from textile and pulp and paper effluents. Due to the tem can remove both color and COD only at an extremely
high capital, regeneration, and disposal costs, full scale GAC high operating cost. The results indicate that electrochemical
42 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47

Table 1
Color and COD removal efficiencies and operating costs of available technologies
Technology Color removal (%) COD removal Operating cost (US$/year) Capital cost (US$/year)
Electrochemical oxidation 97.5 95.1% US$ 1,066,000 ND
Ozone (chemical oxidation) 97.6 55.9% US$ 2,030,000 US$ 700,000
ColorClear (chemical reduction) 76.8 Chemical interference US$ 566,000 US$ 23,700
GAC (activated carbon) 86.1 70.9% US$ 6,813,000 US$ 243,000
Fenton’s reagent (chemical oxidation) 25.4 ND ND ND
Ferric sulfate (chemical coagulation) 0.0 ND ND ND
ND, not determined.

treatment is the most efficient process in terms of operating During the process, an increase in pH is expected. As a
costs for the complete removal of both color and COD. An result of the high pH, precipitates of Fe(OH)2 , Fe(OH)3 ,
electrochemical process that removes color merely by apply- and Al(OH)3 are formed and remain in the solution. The
ing low voltage direct current to a waste effluent could have gelatinous suspension removes colorants by complexation
a significant impact on control strategies. and electrostatic attraction followed by coagulation.

3. Process chemistry 4. Experimental

When wastewater is treated with direct current, a number The study of freshly generated coagulant for color removal
of physicochemical processes take place. These are oxida- was conducted in a bench-scale electrochemical system, as
tion and reduction of impurities in wastewater, dissolution of shown in Fig. 1. The system consists of a dc power supply,
metallic anodes, discharge, and coagulation of colloidal par- a power control and measurement units, an electrochemical
ticles, electrophoresis, electroflotation of particles, precipita- reactor, a reservoir, a feed pump, a flow control valve, a flow
tion of metallic ions on the cathodes, split salts, concentration measuring unit, and a circulation pump. The reactor is made
of acids and alkalis, and water desalination. of PVC plastic with an active volume of 88 cm3 . The anode is
The main pathway for removing colorant from aqueous made of either aluminum or cast iron sheets and the cathode is
solutions is coagulation. At large cathodic potentials, local made of graphite. The electrodes are situated approximately
hydroxyl ions (OH− ) can be generated due to water and oxy- 1 cm apart from each other and submerged in the solution. The
gen reduction: cathode and the anode each have a surface area of 88 cm2 .
The system was operated in a simple batch recirculation mode
2H2 O + 2e− → 2OH− + H2 (1) with a circulation pump to prevent the sedimentation of the
2H2 O + O2 + 4e− → 4OH− (2) coagulant.
Azo and anthraquinone colorants are the two major classes
With cast iron sheets as consumable electrodes, ferrous (Fe2+ ) of synthetic dyes and pigments. Together they represent about
and ferric (Fe3+ ) ions are produced on the anodes. 90% of all organic colorants. Based on their applications,
organic dyes can be subclassified as acid, azoic, basic, direct,
Anode: disperse, reactive, mordant, sulfur, and vat dyes. Reactive
Fe → Fe2+ + 2e− (3) dyes have largely replaced direct, azoic, and vat dyes and are
the largest dye class in the United States. Fig. 2 shows the
Fe → Fe3+ + 3e− (4) anthraquinone structure of Reactive Blue-19 and Fig. 3 shows
the azo structure of Acid Red-266. Disperse Yellow-218 has
Cathode: an unknown azo-based chemical structure. The dyes used in
2H2 O + 2e− → H2 + 2OH− (5) this study were chosen to represent the variety of organic
dyes used in textile industry. A UV–vis range spectropho-
With aluminum sheets as consumable electrodes, Al3+ ions tometer was used to determine the wavelength of maximum
are produced on the anodes. absorbance (λmax ) for each dye. Color intensity was deter-
mined by measuring the absorbance of a sample at 592 nm
Anode:
for Reactive Blue-19, 498 nm for Acid Red-266, and 428 nm
Al → Al3+ + 3e− (6) for Disperse Yellow-218. The data were used to calculate
removal efficiency (x). The percent removal is written as
Cathode (same as Eq. (5)):
A0 − At
− − x (%) = × 100% (7)
2H2 O + 2e → H2 + 2OH (5) A0
 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47 43

Fig. 1. Schematic of the electrochemical coagulation system.

were monitored during the experiment. The results are given

in this section.

5.1. Fe-coagulation process

Due to the generation of OH− on cathode surfaces, the

pH in the system is expected to increase with treatment time.
When the pH increases to a certain level, coagulant will begin
to accumulate in the solution. A portion of the colorant will
Fig. 2. Chemical structure of Reactive Blue-19.
be decomposed by the formation of Fe2+ and/or Fe3+ from
the anode. The majority of color was removed by adsorption
and complexation, however. Fig. 4 shows the characteristics
of the Fe-coagulation process for organic dye removal. Two
grams of Reactive Blue-19 along with 2 g of sodium chlo-
ride were used to prepare 1 L of synthetic dyebath for the
test. A graphite sheet was used as the cathode to pair up with
the iron anode. Initially, the dyebath had an absorbance of
1.6 absorbance units (AU) at 592 nm, which is the λmax of
Reactive Blue-19. The solution was pumped into the electro-
Fig. 3. Chemical structure of Acid Red-266. chemical reactor where 10 V dc was applied across the 1 cm

5. Results and discussion

This study was divided into an Fe-coagulation process and

an Al-coagulation process. For the Fe-coagulation process,
iron sheet was used as consumable anode to generate ferric
and/or ferrous ions. These ions precipitate out as hydroxides
(Fe-coagulant) with OH− anions that are generated on the
cathode through water electrolysis. Aluminum sheet was used
as a consumable anode to generate the Al-coagulant in the
Al-coagulation process. Sodium chloride (NaCl) was added
to provide extra electrical conductivity in the solution and
to promote the production of coagulant. Parameters, such as
voltage and NaCl concentration, were studied for their effect
on color removal. Current, color intensity, and system pH Fig. 4. Characteristics of Fe-coagulation process for color removal.
44 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47

gap. With 2 g/L NaCl in the solution, the applied voltage

resulted in a current of 1.6 A through the reactor. The current
fluctuated a bit and stabilized at around 1.6 A throughout the
10-min treatment. During the experiment, the pH of the solu-
tion increased from 4.2 to 11 in 2 min and remained at 11
throughout the treatment. The solution turned dark brown
in the first minute and a significant amount of coagulant was
observed after 4 min. Samples were withdrawn from the reac-
tor every 2 min. After a 5-min centrifugation, a measure of
color intensity was taken from the spectrophotometer. The
freshly generated Fe-coagulant removed 50% of the color in
2 min and more than 95% by 6 min. The sludge on the bottom
of test tubes turned from dark blue-brown to light brown in
1 week of storage. It is believed that the dye molecules were Fig. 6. Effect of salt concentration on color removal in Fe-coagulation pro-
first adsorbed on the surface of the Fe-coagulant and were cess.
broken down through time.
Fig. 5 shows the effect of applied voltage on color removal. reactor. Fig. 7 shows the current carried through the reac-
With 10 V dc and 1 g/L NaCl, it took 2 min to accumulate tor under different combinations of NaCl concentration and
enough coagulant to start reducing the color intensity. Ulti- applied voltage. At a concentration of 2 g/L, 10 V dc was able
mately, the system was able to remove the color to below the to draw a steady current of 1.6 A across the reactor through-
detection limit of the spectrophotometer. With 5 V applied to out the 10-min treatment time. Under the same concentration,
the reactor, the system was unable to generate coagulant for only 0.5 A was carried through the reactor with a voltage of
color reduction. It was found that a minimum current was car- 5 V. With 1 g/L NaCl in the solution 10 V dc will initially
ried through the reactor at that voltage. In order to increase the drew a current of 1.6 A through the reactor. The reaction
current density in the reactor, NaCl concentration in the syn- was vigorous and a significant amount of coagulant was gen-
thetic dyebath was increased to 2 g/L. Fig. 6 shows the color erated. During the operation chloride (Cl− ) was consumed
removal with the extra NaCl in the solution. A vigorous reac- to produce chlorine gas (Cl2 ) on the surface of the anode.
tion was observed in the reactor when 10 V dc was applied to Some Cl2 evolved from the surface as tiny bobbles while the
the solution containing 2 g/L of NaCl. Color removal started majority of Cl2 dissolved and equilibrated with hypochlor-
immediately and continued until all the color was removed. ous acid (HClO), trichloride ions (Cl3 − ), and hypochlorite
However, the excessive amount of coagulant generated by the (ClO− ) in the solution. After 2 min of operation, the solu-
process ended up with the sludge deposited on the bottom of tion began to lose its electrical conductivity and showed a
the reactor. Centrifugation is an effective method to separate reduction of current through the reactor. Fig. 8 shows the cor-
the sludge from the solution. For the process to be applied to responding color removal under these conditions. With high
an industrial scale, a sludge separation mechanism needs to salt (NaCl) concentration and high voltage, the system started
be considered and examined thoroughly. to remove color at the moment power was applied and com-
An electrochemical reactor can be operated under con- pletely removed the color in 6 min. It took 2 min to initiate
stant voltage or constant current. Theoretically, reaction rate the low salt process. By the end of the treatment, the low salt
is proportional to current density. Applied voltage and NaCl process reached the same level of color removal in the same
concentration both contribute to the current density in the

Fig. 7. Current as a function of salt concentration and applied voltage in

Fig. 5. Effect of applied voltage on color removal in Fe-coagulation process. Fe-coagulation process.
 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47 45

Fig. 8. Effect of current on color removal in Fe-coagulation process. Fig. 9. Application of Fe-coagulation process on reactive, acid, and disperse
dyes.

treatment time. As can be expected, the process efficiency, in cedure from the previous section was followed to yield the
terms of color removal and treatment time, is closely related results for comparison. Again, Reactive Blue-19 was chosen
to the current through the reactor. At a low salt concentration for a thorough evaluation. Fig. 10 shows the effect of applied
and low voltage, low current was carried through the reactor voltage on color removal. Five-volt dc caused minimum cur-
and no color removed in a 10-min treatment. rent through the reactor, which resulted in no color removal.
In viewing the success of the electrochemical coagula- With 1 g/L NaCl in the solution 10 V dc created significant
tion for reactive dye removal, it must be determined how current, resulting in enough Al-coagulant for color removal.
widely this technology is applicable to other textile dyes. Color removal reached a maximum of 75% but the color was
Acid Red-266 and Disperse Yellow-218 were chosen to test restored at the end of the 6-min treatment time. Fig. 11 shows
the process. Different from Reactive Blue, both Acid Red- the same trend with 10 V dc applied to the reactor. At a NaCl
266 and Disperse Yellow-218 are azo dyes. Usually azo dyes concentration of 2 g/L, the applied voltage caused a vigor-
are more accessible to chemical reduction and reactive dyes ous reaction in the reactor thus a significant color reduction.
are more easily broken down by chemical oxidation. Due The color was completely removed in 6 min but the solution
to low solubility, disperse dyes rarely participate in aqueous regained its color at the end of the 10-min treatment. The syn-
phase chemical reactions. Because electrochemical treatment thetic dyebath was prepared with an initial pH of 4.2. During
provides oxidation, reduction, adsorption, coagulation, and the treatment, the pH quickly passed through 7 and increased
flotation in one reactor, one would expect that the treatment to 11. Due to amphorism, aluminum hydroxide dissolves at
might offer an universal process for decolorizing a matrix of high and low pH and has a lowest solubility at pH 6.2. When
textile dyes. Solutions of all three dyes were prepared at a the pH reaches 6, most of the aluminum hydroxide precipi-
concentration of 2 g/L with a same concentration of NaCl to tate out as Al-coagulant and adsorb the colorant. When the
provide the needed conductivity. Initial absorbance of these pH reaches 9, some of the Al-coagulant will dissolve and
solutions was between 1.5 and 1.8 AU at each λmax . These restore a portion of the adsorbed colorant into the solution.
solutions were treated in the electrochemical reactor under The restored color had an observable turbidity that did not
10 V dc for 10 min. Fig. 9 shows the removal efficiencies of
the electrochemical coagulation on the three dyes. It took
6 min to complete the treatment for all three dyes. Residual
color was always observed in the Disperse Yellow dyebath.
Still, 90% removal is achievable. It is believed that the mech-
anism for disperse dye removal is adsorption/complexation
followed by flotation. The reactor is designed to optimize the
generation of coagulant. Therefore, a modification is needed
to improve flotation thus disperse dye removal.

5.2. Al-coagulation process

In terms of chemical coagulation, aluminum ions are in

most cases more effective than ferric or ferrous ions. It
became apparent that freshly generated Al-coagulant must
be evaluated for color removal. An aluminum sheet was used Fig. 10. Effect of applied voltage on color removal in Al-coagulation pro-
to replace cast iron as the consumable anode. The same pro- cess.
46 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47

shows the corresponding color removal for each treatment. It

can be seen from Fig. 13 that high salt content and low applied
voltage produces optimum conditions for color removal.
High salt content favors the color removal and the low cur-
rent density delays the system from color restoration through
Al-coagulant dissolution. After treatment, acids can be added
to the effluent to bring the pH from 11 down to around 6 or
7. This will stabilize the Al-coagulant and thus prevent the
treated solution from color restoration. NaCl is commonly
used in dyebath to promote dye exhaustion. The residual NaCl
can be used in electrochemical treatment of spent dyebath for
color removal as well. During the operation, NaCl is oxidized
to chlorine gas on the anode surfaces. The chlorine will dis-
solve in water to form HClO and ClO− . These are strong
Fig. 11. Effect of salt concentration on color removal in Al-coagulation
oxidizing agents and can be used to further oxidize the dye
process.
molecules that are adsorbed on the coagulant. These species
are widely used disinfectants. Discharge of these chemicals
into a wastewater treatment plant may disrupt its biological
processes.
A set of experiments was conducted to explore the applica-
bility of Al-coagulant for decolorization of different dyebath.
Solutions of Reactive Blue-19, Acid Red-266, and Disperse
Yellow-218 were prepared with the procedure stated in the
previous section. Two grams of NaCl were added to 1 L of
the solution to provide the essential electrical conductivity.
At 5 V dc, a significant amount of Al-coagulant quickly accu-
mulated in the reactor followed by color reduction. Fig. 14
shows the removal of each dye under this treatment. Due to
low water solubility, disperse dyes are difficult to break down
by chemical oxidation or reduction. Al-coagulation removed
color to a level that was beyond the detection limit of the spec-
Fig. 12. Current as a function of salt concentration and applied voltage in
Al-coagulation process.
trophotometer. Because of the low solubility of the disperse
dyes, carriers are used to stabilize the dispersing system and
keep the dye powders in an emulsified solution. The addi-
settle after 5 min of centrifugation. It is believed that the tur- tion of polyvalent aluminum ions will neutralize the colloids
bidity is caused by the gelatin-like aluminum hydroxide that and destabilize the dispersing system thus allowing the col-
dissolves in the high pH aqueous solution. orant to attach to the Al-coagulant and be removed from the
Fig. 12 shows the stable currents in the reactor at different solution.
combinations of salt content and applied voltage, and Fig. 13

Fig. 14. Application of Al-coagulation process on reactive, acid, and dis-

Fig. 13. Effect of current on color removal in Al-coagulation process. perse dyes.
 C.-L. Yang, J. McGarrahan / Journal of Hazardous Materials B127 (2005) 40–47 47

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